Rozprawy doktorskie na temat „Olfactometry”

Большинство методов оценки обонятельных расстройств имеют широкий спектр применения для диагностики различных заболеваний, в том числе психических расстройств, повреждения головного мозга и нервной системы. Однако , необходимо рассмотреть обонятельную дисфункцию в связи с проблемой блокирования воздушного канала в обонятельной системе человека. Поэтому необходимо разработать узкоспециализированный метод оценки обонятельно-респираторных заболеваний, которые имели бы высокую степень объективности для использования в клинической практике оториноларингологов.

Thesis (Ph. D.)--University of Sydney, 2009.
Includes graphs and tables. Includes list of publications and three published articles co-authored with others. Title from title screen (viewed June 9, 2009) Submitted in fulfilment of the requirements for the degree of Doctor of Philosophy to the School of Psychology. Degree awarded 2009; thesis submitted 2008. Includes bibliographical references. Also available in print form.

Odour recognition memory was studied in 49 patients with unilateral temporal lobe excision, and 20 control subjects. Odours were presented monorhinally to explore any asymmetry in performance between nostrils, and to test for hemispheric differences between patients with excision from the right versus the left temporal lobe. Testing was by a 2-alternative, forced-choice procedure, immediately after presentation and 24 hours later. A discrimination test was carried out at the conclusion of the memory test, and nondiscriminated odours were excluded from the final memory scores. The contribution of the hippocampus to odour memory was investigated by dividing patient groups according to the size of hippocampal excision. The memory test showed that only patients with excision from the left temporal lobe that included a large hippocampal removal were impaired after 24 hours. The discrimination test revealed deficits only for patients with right temporal lobectomy, and only in the right nostril.

The aroma quality of cigarette smoke is an important characteristic for smokers. It is therefore critical to understand the nature of the key aroma compounds in tobacco smoke and to identify them. Also, knowing how flavour compounds in tobacco smoke are released and how they persist in the nose of smokers would help in designing cigarettes with optimised flavour release for the consumer. One approach is to use Gas Chromatography with Olfactometry detector (GC-0). The GC-Olfactometry technique and the Nasal Impact Frequency (NIF) method were proven to be applicable in analysing the aroma of complex matrices such as tobacco smoke.

The sense of smell is a primal sense for humans as well as animals.In everyday life the smells encountered are composed of dozens, even hundreds of odors; few arise from a single odorant. Enormous numbers of odors occur due to the vast variation in the concentration, size and structure of odorant molecules that makes olfaction differ from simpler visual or auditory dimensions. Accordingly, little is known about the ways in which changes in molecular structure and concentration of individual odorants change odor quality. Also, currently not much is understood about synergism/antagonism, how one odorant masks or suppresses another in mixtures and there is no method for predicting which odor will be suppressed. The two main objectives of this thesis were to determine whether a part of a molecular structure rather than the whole structure plays a key role in odor quality and whether a key part of a molecule can be used to choose antagonists for that odorant. For this study three classes of musks and two potential antagonists were used. The results of the study are discussed in some detail. It is concluded that future studies of the importance of molecular structure in mixture interactions require substantially more information on the relation between structure and odor quality to allow systematic studies to be developed. In summary the two hypotheses investigated were not supported by the results. Importantly, however, they do support the view that it is likely that odor quality is dependent on the whole structure of an odorant not a single feature.
Master of Science (Hons)

Thesis (Ph.D.)--Tufts University, 2003.
Adviser: David R. Walt. Submitted to the Dept. of Chemistry. Includes bibliographical references. Access restricted to members of the Tufts University community. Also available via the World Wide Web;

Note:
The aim of this dissertation was 10 investigate if and how emotional arousalinfluences odor memory. I conducted three studies , one of which invo lved pat ients withresect ion from the medial tcmporal lobc including the amygd ala (MTLR). In the first experiment of Study 1, participants showed better memory for odo rs rated as being more emotionally arousing than tor odors rated as less arousing.
Cette dissertation avail pour objectif d'etudier si, de quelle maniere. L'eveil emotionnel influence la memoire olfactive. J'ai effectue trois etudes, dont une impliquant des patients ayant subi une resection du lobe temporal median inc1uant l'amygdalc (MTLR). Dans la premiere experience de l'etude 1, la reconnaissance des odeurs plus emotionnellement eveillantes a ete superieure a celle des odeurs moins eveillantes.

Jackfruit seeds are an under-utilized waste in many tropical countries. In this work, we demonstrated the potential of roasted jackfruit seeds to generate chocolate aroma for use as a cocoa substitute in foodstuffs. Twenty-seven different flours were produced from a hard pulp variety of jackfruit by drying (DJS), acidifying (AJS), or fermenting (FJS) the seeds prior to roasting under different time/temperature combinations. The chocolate aroma of groups of four flours were ranked by a sensory panel (n=162) and response surface methodology was used to identify optimum conditions for producing chocolate aroma. Pyrazines were analyzed instrumentally as markers of chocolate aroma, while moisture, pH, and color were also monitored. The best chocolate aroma was produced in three jackfruit seed flours: DJS, AJS, and FJS. Volatile and semi-volatile compound contents were evaluated by GC-MS, GC-O, and SPE-GC in these three jackfruit seed flours and their profiles were compared with the profile of cocoa powder. These flours were also evaluated for their solubility, swelling power, wettability, apparent density, viscosity, sensory preference, and intensity of chocolate aroma. The central composite design was used to optimize the solubility and swelling power. Water temperature and time to flour exposition were the response variables. Owing to their differing volatile compositions, two different flours (DJS and FJS) were applied in six cappuccino formulations with 50%, 75%, and 100% substitution of cocoa powder with jackfruit seed flours. The consumers acceptance of cappuccinos (n=126) and the quantitative descriptive analysis (QDA) were used to describe the preparations. Physicochemical properties in cappuccino formulations were also evaluated. The greatest relative concentration of pyrazines (p<=0.05) was formed in dry, acidified, and fermented flour when we used 156, 165, and 154°C, respectively. Clearly, fermentation is necessary to improve the chocolate aroma of jackfruit seeds, and it is possible to select the best roasting conditions for each treatment to optimize the sensory perception of chocolate aroma. These optimal treatment conditions were found to be 171°C for 47 min in DJS, 180°C for 40 min in AJS, and 154°C for 35 min in FJS. FJS had higher solubility and wettability than other flours. The viscosities of jackfruit seed flours were low with high solubility, properties that are desirable in cocoa powder (CP). Chocolate aroma was most intense for FJS. Therefore, jackfruit seed flours have technological properties and chocolate aroma similar to or better than CP and commercial chocolate (CC). For cappuccino formulations, 50% and 75% cocoa powder was replaced with dry jackfruit seed flour, and there was no change in sensory acceptability or technological properties. The principal component analysis of QDA explained 90% of variance. The primary characteristics of cappuccinos made with dry jackfruit seeds were cappuccino, chocolate, cinnamon, and coffee aromas, and cappuccino and chocolate tastes. Indeed, dry jackfruit seed flour is an innovative cocoa powder substitute; it could be used in food preparations, consequently utilizing this tropical fruit waste by incorporating it as an ingredient in a common product of the human diet.
As sementes de jaca são subaproveitadas em muitos países tropicais. Neste estudo, foi possível demonstrar que as sementes de jaca torrada possuem potencial para produzir aroma de chocolate e podem ser utilizada como um substituto do cacau em alimentos processados. Vinte e sete farinhas foram produzidas com a semente de jaca da variedade dura através de secagem (DJS), acidificação (AJS), ou fermentação (FJS) as sementes foram submetidas sob diferentes combinações de tempo e temperatura de torra. O aroma de chocolate quanto aos grupos de farinha foram avaliados sensorialmente por painel (n=162) e a metodologia superfície de resposta foi utilizada para identificar a melhor condição para produzir aroma de chocolate. As pirazinas foram instrumentalmente analisadas como marcadores do aroma de chocolate. Assim como, umidade, pH e cor também foram monitorados. O melhor aroma de chocolate foi produzido para as três farinhas de semente de jaca: DJS, AJS e FJS. Compostos voláteis e semi-volateis foram avaliados utilizando GC-MS; GC-O e SPE-GC nesses três tratamentos as farinhas de sementes de jaca seus perfis foram comparados com o perfil do cacau em pó. Essas farinhas foram também avaliadas quanto sua solubilidade, molhabilidade, densidade aparente, viscosidade, preferência sensorial e intensidade do aroma de chocolate. O delineamento com ponto central foi utilizado para otimizar a solubilidade e o poder de absorção. As variáveis respostas foram temperatura da água e tempo de exposição da farinha. Devido a sua composição diferenciada quanto aos compostos voláteis, duas diferentes farinhas (DJS e FJS) foram aplicadas em seis formulações de cappuccino com 50, 75 e 100% de substituição do pó de cacau por farinha de semente de jaca. A aceitação dos cappuccinos pelos consumidores (n=126) e a análise quantitativa descritiva (ADQ) foram utilizadas para descrever as preparações. Propriedades físico-químicas das formulações de cappuccino também foram avaliadas. A maior concentração relativa de pirazinas foi formada em farinhas seca, acidificada e fermentada quando utilizado 156, 165 e 154°C, respectivamente. Claramente a fermentação é necessária para melhorar o aroma de chocolate da farinha de semente de jaca, foi possível selecionar a melhor condição de torração para cada tratamento quanto à percepção sensorial do aroma de chocolate. Essas condições ótimas foram encontradas como 171°C para 47 minutos para farinha seca; 180°C durante 40 minutos para as sementes acidificadas e 154°C durante 35 minutos para as farinhas fermentadas com alta solubilidade e molhabilidade em comparação com as demais farinhas. A viscosidade da farinha de semente de jaca foi baixa com alta solubilidade o que é desejável para o cacau em pó (CP). O aroma de chocolate foi mais intenso para FJS. Assim, as farinhas de semente de jaca tiveram propriedades tecnológicas e aroma de chocolate similar ou melhor que CP e de chocolate comercial (CC). Para as formulações de cappuccino 50 e 75% de pó de cacau foram substituídas por farinha de semente de jaca seca, e não houve mudança na aceitabilidade sensorial e nas propriedades tecnológicas A análise de componentes principais para ADQ explicou 90% da variância. A principal característica dos cappuccinos feitos com semente de jaca seca quanto ao aroma foram cappuccino, chocolate, canela e café e cappuccino e chocolate para o sabor. Assim, a farinha de semente de jaca seca é um substituto inovador do pó de cacau, este pode ser utilizado em preparações alimentícias, consequentemente este resíduo agroindustrial pode ser incorporado como ingrediente comum na dieta humana.

In this article an attempt is made to standardize the results of diagnosis of olfactory analyzer disorders. For the development of the integral indicator of olfactory sensitivity in order to formalize the diagnostic data on the basis of the method of increasing the objectivity of alfakometric studies, weighting coefficients were determined based on the method of attribution of points. A questionnaire was prepared for our study.

The sense of smell is a primal sense for humans as well as animals.In everyday life the smells encountered are composed of dozens, even hundreds of odors; few arise from a single odorant. Enormous numbers of odors occur due to the vast variation in the concentration, size and structure of odorant molecules that makes olfaction differ from simpler visual or auditory dimensions. Accordingly, little is known about the ways in which changes in molecular structure and concentration of individual odorants change odor quality. Also, currently not much is understood about synergism/antagonism, how one odorant masks or suppresses another in mixtures and there is no method for predicting which odor will be suppressed. The two main objectives of this thesis were to determine whether a part of a molecular structure rather than the whole structure plays a key role in odor quality and whether a key part of a molecule can be used to choose antagonists for that odorant. For this study three classes of musks and two potential antagonists were used. The results of the study are discussed in some detail. It is concluded that future studies of the importance of molecular structure in mixture interactions require substantially more information on the relation between structure and odor quality to allow systematic studies to be developed. In summary the two hypotheses investigated were not supported by the results. Importantly, however, they do support the view that it is likely that odor quality is dependent on the whole structure of an odorant not a single feature.

La incidència sobre el suro de defectes sensorials amb descriptors de florit-humitat és un dels principals problemes amb què s'enfronta la indústria surera. Els principals compostos relacionats amb aquest defecte son cloroanisoles, metoxipirazines, geosmina i metilisoborneol. Aquesta recerca s'ha fet amb l'objectiu principal d'aprofundir en els mètodes de determinació de compostos volàtils en suro. S'ha desenvolupat una metodologia basada en la microextracció en fase sòlida i la cromatografia de gasos per a l'anàlisi conjunta d'aquests compostos en macerats de suro. El fet que la majoria dels compostos d'interès tingui un origen microbià ha fet necessari completar les anàlisis químiques amb mètodes de detecció i aïllament dels microorganismes susceptibles de produir-los. S'ha utilitzat un mètode per a l'estudi de la diversitat de fongs i bacteris en mostres de suro basat en l'estudi de marcadors genètics mitjançant l'anàlisi en gradients electroforètics desnaturalitzants. Per últim s'ha avaluat la capacitat de producció de defectes sensorials per microorganismes aïllats de suro utilitzant tècniques olfactomètriques.
The incidence of musty-earthy sensory deviations on cork is one of the main problems that the cork industry faces. The main compounds related to this defect are chloroanisoles, methoxypyrazines, geosmin and methylisoborneol. The aim of this research work was to develop analytical methods to simultaneously determine a large set of volatile compounds in cork samples. A methodology based on solid phase microextraction (SPME) and gas chromatography for the determination of TCA, 3-isopropyl-2-methoxypyrazine, geosmin and methylisoborneol in cork aqueous macerates has been developed and validated. Moreover, the microbial origin of most of these compounds makes necessary to complement the chemical analysis with the detection and isolation of microorganisms that may be involved in the production of off-odours. Regular fingerprinting techniques for the analysis of microbial diversity such as Denaturing Gradient Gel Electrophoresis (DGGE) have been applied to the study of microorganism potentially responsible for off-odour formation in cork, in order to complement the chemical characterization of the volatile fraction. Finally we have evaluated the off-odour production capacity of microorganisms isolated from cork using olfactometry techniques.

Parmi les dimensions sensorielles engagées dans la perception de la flaveur, la composante odorante est déterminante car elle porte le plus souvent l’identité et la typicité d’un aliment. L’analyse chimique de la composante odorante repose sur une stratégie séparative qui permet d’identifier les différents odorants présents dans l’aliment. Cependant, la perception des odorants en mélange induit des interactions au niveau perceptif qui ne sont pas prises en compte dans les techniques séparatives. Les mécanismes sous-jacents aux interactions perceptives sont mal connus, ce qui limite les possibilités de prédiction de l’odeur d’un aliment sur la base de sa composition chimique. En réponse à cette problématique deux approches émergent de la revue de la littérature. La première est basée sur la prédiction d’odeur d’après la structure moléculaire des odorants. Cependant, les études concernent des odorants seuls et non leurs mélanges. La seconde repose sur la recombinaison d’odorants en mélange après l’étape d’analyse séparative, mais le choix des odorants à associer est essentiellement empirique. Ainsi, deux questions se posent : Comment prédire l'odeur de mélanges de molécules d’après la structure moléculaire des odorants? Comment améliorer l'analyse de la flaveur dans le but de prédire l'odeur d’aliments complexes composés de plusieurs dizaine d’odorants en mélanges? Ces deux questions ont été abordées dans cette thèse dont les travaux sont décrits dans ce manuscrit selon deux axes principaux.Le premier axe décrit l'utilisation et le développement d’un modèle basé sur le concept des distances angulaires calculées à partir de la structure moléculaire des odorants avec pour objectif de prédire la similarité perceptive de mélanges plus ou moins complexes d’odorants. Les résultats soulignent l'importance de prendre en compte la dimension d'intensité des odorants afin d’améliorer la qualité de la prédiction. Des perspectives d’amélioration du modèle sont dégagées pour permettre de dépasser la dimension de similarité et prédire des dimensions qualitatives de l’odeur.Le deuxième axe présente une démarche originale d’intégration de connaissances liées à l’expertise dans la procédure d'analyse de la flaveur. Ainsi, trois types de données hétérogènes sont agrégés dans un modèle mathématique global : des données chimiques, des données sensorielles et des connaissances d’experts aromaticiens. L'expertise est intégrée à travers la création d'une ontologie qui est ensuite associée à une approche de logique floue optimisée par algorithme évolutionnaire. Le modèle développé permet de prédire le profil odorant de seize vins rouges sur la base de leur composition en odorants. Au final, l’ensemble des travaux menés dans cette thèse apporte des résultats originaux permettant une meilleure compréhension de la construction des odeurs des aliments et permet d’élaborer des hypothèses quant aux relations sous-jacentes de l'espace perceptif des odeurs en mélanges complexes
Among the sensory dimensions involved in food flavor, the odor component is critical because it often determines the identity and the typicality of the food. Chemical flavor analysis provides a list of the odorants contained in a food product but is not sufficient to predict the odor resulting from their mixture. Indeed, odor perception relies on the processing by the olfactory system of many odorants embedded in complex mixtures and several perceptual interactions can occur. Thus, the prediction of the perceptual outcome of a complex odor mixture remains challenging and two main approaches emerge from the literature review. On the one hand, predictive approaches based on the molecular structure of odorants have been proposed but have been limited to single odorants only. On the other hand, methodologies relying on recombination strategies after the chemical analyses of flavor have been successfully applied to identify those odorants that are key to the food odor. However, the choices of odorants to be recombined are mostly based on empirical approaches. Thus, two questions arise: How can we predict the odor quality of a mixture on the basis of the molecular structure of its odorants? How can we improve food flavor analysis in order to predict the odor of a food containing several tens of odorants? These two questions are at the basis of the thesis and of this manuscript which is divided in two main axes.The first axis describes the development of a model based on the concept of angle distances computed from the molecular structure of odorants in order to predict the odor similarity between mixtures. The results highlight the importance of taking into account the odor intensity dimension to reach a good prediction level. Moreover, several perspectives are proposed to extend the model prediction beyond the similarity dimension and to predict more qualitative dimensions of odors.The second axis presents an innovative strategy which allows integrating experts’ knowledge in the flavor analysis procedure. Three different types of heterogeneous data are embedded in a mathematical model: chemical data, sensory data and knowledge from expert flavorists. Experts’ knowledge is integrated owing to the development of an ontology, which is further used to define fuzzy rules optimized by evolutionary algorithms. The final output of the model is the prediction of red wines’ odor profile on the basis of their odorants’ composition. Overall, the thesis work brings original results allowing a better understanding of food odor construction and gives insights on the underlying relationships within the odor perceptual space for complex mixtures

Thesis (M.Sc. (Hons)) -- University of Western Sydney, 2004.
"This thesis was submitted in fulfilment of the requirements for the degree of Master of Science (Hons) in the Centre for Advanced Food Research, University of Western Sydney, June 2004" Includes bibliography.

Mestrado em Viticultura e Enologia - Instituto Superior de Agronomia / Faculdade de Ciências. Universidade do Porto
In this work, the sulphur varietal compound aromatic potencial of 7 Portuguese Grapes wines was studied in comparision with Sauvignon Blanc. The aroma compounds containing sulphur compounds as 3-mercaptohexyl acetate (A3MH), 3-mercaptohexanol (3MH) and 4-mercapto-4-methylpentan-2-one (4MMP) were searched in particular. GCFPD, GC-MS and GC-Olfactometry analysis were conducted to obtain confirmation of the existence of those compounds. Only GC-olfactometry revealed the presence of two olfactory zones relatives of the 4MMP and 3MH in all Portuguese Grape varieties wines from 2009, and a third intermediary olfactory zone relative of A3MH only revealed in the young 2010 wines from Arinto and Fernão Pires. The 4MMP and the A3MH were not quantified nevertheless the olfactometric measures allow to determine relative differences among wines. The 3MH was semi-quantified in 5 of the Portuguese varieties wines using GC-FPD equipment. Some of the portugueses grape wines presented varietal tiol aromatic intensity comparable in scale with the Portuguese Sauvignon Blanc Win

Preventing flavor fade requires an understanding of the relationship between carbonyl amine and lipid oxidation reactions. The polyunsaturated fatty acid content of lipids in peanuts makes them more susceptible to lipid oxidation. The major by-products of the oxidation reaction are nonanal, hexanal, octanal, and decanal. These chemicals are associated with cardboardy, painty, and oxidized flavors associated with flavor fade. The carbonyl-amine reaction yields a variety of pyrazines with positive flavor attributes. Initial flavor notes were explored through sensory work, Gas Chromatography-Olfactometry, and chemical analysis. The fresh roasted volatiles produced from roasted peanuts and the aldehydes resulting from oxidation were also evaluated using GC-FID to quantify and identify the pyrazines and hexanal over a 21 day storage period. Electronic Nose was used to determine differences between storage periods. Gas chromatography-Olfactometry identified potent pyrazines contributing to fresh roasted peanutty aroma in fresh peanuts. Using GC-FID a significant decrease (p<.05) in 2-ethylpyrazine and 2,3-diethylpyrazine concentration was found over a 21-day period. No significant difference (p>0.05) was noted in the other pyrazines evaluated. A significant increase (p<0.05) was noted in the hexanal concentration over a 21-day period. The peroxide values and sensory analysis correlated directly with the GC-FID results with a significant increase (p<0.05) in peroxide value at Day 14 and Day 21, and a significant decrease (p<0.05) in fresh roasted peanuty flavor from days 0-21 and a significant increase (p<.05) in painty, cardboardy and bitter from days 7-21. The electronic nose successfully separated Day 0 and Day 21 samples from Day 7 and 14, which were also separated, but with minimal overlap.
Ph. D.

Abstract Olfactory tasks are used very often with laboratory animals in studies of the neurobiology of learning and memory. Rats and mice are extremely sensitive in their detection and discrimination of odours, learn olfactory tasks rapidly, and can display higher order cognitive functions in olfactory tasks. This cognitive capacity may rival the ability of primates to learn analogous tasks with visual cues and most likely reflects strong anatomical connections between the olfactory bulbs and higher brain regions such as the piriform cortex, orbitofrontal cortex and hippocampus. The current thesis explored olfactory discrimination learning and performance in rats and had two principal aims. The first part of the thesis was oriented around odour masking phenomena in rats: the ability of one odour in a mixture to suppress detection of a second odour in that mixture. A specialized behavioural paradigm was developed to allow the study of odour masking in the rat. The second part of the thesis was pharmacological and determined whether the acquisition, reversal and performance of olfactory discriminations, and analogous auditory discriminations, are affected by two commonly used classes of drugs (benzodiazepines and cannabinoids). Together, these studies attempt to gain a better understanding of the nature of olfactory discrimination learning in rats, by using both psychophysical and pharmacological approaches, and to develop behavioural paradigms which may be used in future psychophysical and pharmacological studies. Following an introduction and review of olfactory and auditory studies in rat (Chapter 1), odour masking phenomena were studied in Chapter 2. The aliphatic aldehydes butanal (C4) and heptanal (C7) were used in the study. Aldehydes were of interest as this class of odorants abound in nature and may be important for rodents’ species-specific communication. Thirsty rats were initially trained to discriminate C4 and C7 in the olfactometer, using a go/no-go olfactory discrimination task. This involved rats learning to nose poke in an odour port and to lick a tube for a water reward on presentation of the rewarded component S+, while withholding licking at the tube when the other, unrewarded, aldehyde (S-) was presented. Odour mixtures (C4C7 or C7C4) were then introduced into the task as an additional non-rewarded condition (mixture S-). The concentration of the non-rewarded aldehyde in the mixture was then systematically decreased, while the concentration of the rewarded aldehyde was kept constant. When the non-rewarded aldehyde reached a critical low level in the mixture, rats started to make responses to the non-rewarded mixture (false alarms) showing that the S+ odour was suppressing the S- odour in the mixture, so the mixture was being responded to in the same manner as the S+ odour presented alone. Results also showed asymmetric suppression in the mixture condition, such that butanal suppressed detection of heptanal at a much lower concentration than vice versa. A second experiment demonstrated that when both butanal and heptanal were present in a binary mixture at the same concentration (10-6 volume %), rats responded to the mixture as if only butanal was present. Our findings are in agreement with human studies showing component interactions in binary mixtures of aldehydes. The molecular feature of carbon chain length appears to be a critical factor in determining the outcome of interactions between aldehydes at peripheral olfactory receptors, with smaller chain aldehydes better able to compete for receptor occupancy. Subsequent chapters explored the effects of two classes of commonly used drugs - benzodiazepines and cannabinoids - on olfactory and auditory discrimination in rats. Animal models such as the radial arm maze, Morris water maze and object recognition test are routinely used to test adverse and facilitatory effects of drugs on cognition in rodents. However, comparatively few pharmacological studies employ olfactory or auditory go/no-go paradigms. Thus, an important part of the present thesis was to assess the viability of using such paradigms in detecting pharmacological effects, and to identify whether such effects may be modality specific (i.e. whether a drug has a greater effect on olfactory or auditory tasks). In Chapter 3, the effects of benzodiazepines on olfactory discrimination tasks were explored. Rats were injected with the benzodiazepine drugs midazolam or diazepam and tested on discrimination tasks involving either the auditory and olfactory modality. Results showed that midazolam (0.5–2 mg/kg sc) did not affect the performance of a well-learned two-odour olfactory discrimination task, and moderately facilitated the performance of a go/no-go auditory discrimination task. On the contrary, midazolam (1 mg/kg) impaired the acquisition of a novel go/no-go olfactory discrimination task, as well as the reversal of a previously well-learned olfactory discrimination. However, midazolam did not affect the acquisition or reversal of an equivalent auditory discrimination task. The olfactory bulb and the piriform cortex are intimately involved in associative learning and behavioural aspects of olfactory performance, and have high concentrations of benzodiazepine receptors. These may therefore be possible neural substrates for the disruptive effects of benzodiazepines on olfactory learning. Findings from Chapter 4 indicated that the prototypical cannabinoid agonist delta-9-tetrahydrocanabinol (Δ9 THC) (0.3, 1 and 3 mg/kg) impairs auditory discrimination performance, but had no effect on equivalent olfactory discriminations. This is in marked contrast to the effects of benzodiazepines. Residual effects were observed, such that auditory discrimination performance was still impaired on the day following Δ9 THC administration. Delta-9-tetrahydrocanabinol effects were prevented by co-administration of the cannabinoid antagonist rimonabant (3 mg/kg). In addition, the anandamide hydrolysis inhibitor URB597 (0.1 and 0.3 mg/kg), which boosts levels of endogenous cannabinoids in the synapse, also impaired auditory discrimination performance, and this effect was also reversed by rimonabant. This study also assessed the effects of Δ9 THC (0.3, 1 and 3 mg/kg) and URB597 (0.1 and 0.3 mg/kg) on acquisition and reversal of novel olfactory discriminations. Results showed that Δ9 THC impairs olfactory reversal learning without affecting acquisition of the original discrimination. It is argued that this reversal deficit may be part of a wider capacity for cannabinoids to impair cognitive flexibility. The final Chapter (General Discussion) discusses the relevance and implications of the combined findings. The results add significantly to our current understanding of perceptual, learning and memory processes involving the olfactory modality in rats. With respect to olfactory perception, this thesis introduced a new behavioural paradigm, which can be used to assess component suppression in mixtures, and may be of use in future psychophysical studies involving rodents or other species. With respect to learning and memory, the thesis provides novel information on the disruptive effects of benzodiazepines and cannabinoids on olfactory and auditory tasks. It is concluded that go/no-go olfactory and auditory discrimination tasks in rats can provide a useful platform for assessing the disruptive and modality-specific effects of drugs on learning, performance and cognitive flexibility. Future studies might expand the range of drugs tested on these paradigms and might consider chronic as well as acute drug effects.

Thesis (Ph.D.)--Tufts University, 2001.
Adviser: David R. Walt. Submitted to the Dept. of Chemistry. Includes bibliographical references. Access restricted to members of the Tufts University community. Also available via the World Wide Web;

Orientadores: Maria Aparecida Azevedo Pereira da Silva, Maria Regina Bueno Franco
Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos
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Resumo: A aceitação dos consumidores por suco de maracujá deve-se ao seu aroma e sabor exóticos. No entanto, na etapa de concentração do suco, juntamente com a água, são também arrastados compostos voláteis responsáveis pelo aroma e sabor característicos da fruta, o que reduz a qualidade sensorial do produto final. A recuperação desses compostos ocorre quando os voláteis extraídos por arraste de vapor durante a etapa de concentração do suco, são condensados em uma solução aquosa denominada ¿water phase¿. Submetendo-se a water phase a um processo de destilação fracionada, ela pode ser concentrada, originando uma essência natural da fruta GRAS, que ao ser readicionada ao suco, aumenta sua qualidade sensorial. No entanto, a indústria de sucos tropicais no Brasil, embora produza a water phase, carece de conhecimento e tecnologia adequada para a produção de essências naturais GRAS a partir da water phase. A presente pesquisa teve por objetivo caracterizar o perfil de voláteis presentes na water phase de maracujá de empresa brasileira, e avaliar o potencial da mesma para a produção de essência natural GRAS de maracujá. Os compostos voláteis da water phase foram isolados por extração líquido-líquido (diclorometano) e identificados por cromatografia gasosa (CG) e espectrometria de massas (CG-EM). A qualidade e poder odorífero de cada volátil presente no isolado e sua possível contribuição a uma essência de maracujá foram avaliados, utilizando-se a técnica CG-olfatométrica Osme. Quatro julgadores treinados avaliaram sensorialmente o efluente cromatográfico, em três repetições; seus resultados foram integrados pelo software SCDTI, produzindo-se um aromagrama do isolado. Dos 110 picos detectados no cromatograma, 71 foram identificados, perfazendo 72% da área total. Trinta e cinco voláteis foram percebidos no efluente cromatográfico, dos quais, 60% possuíam aromas de impacto positivo para a elaboração de uma essência. Entre esses compostos, os de maior impacto odorífero no efluente cromatográfico foram: butanoato de etila (descrito como frutas vermelhas, tuttifrutti, uva); 3-hexenal (verde, grama); butanoato de metila (doce, frutal); hexanoato de etila (cítrico, frutal); acetato de hexila (verde, fruta verde); óxido de rosa (mamão, doce); hexanal (grama, mato), terpinen-4-ol (frutal, banana); hexanol (desinfetante de limão, mato). Voláteis de impacto odorífero negativo para uma essência foram também percebidos no efluente cromatográfico, tais como: isobutanol e acetato de isobutila, descritos como ¿borracha¿ e ¿fio queimado¿, assim como voláteis de notas ¿torradas¿, tais como benzaldeído e furfural, descritas como café, grão torrado e amendoim torrado. Esses resultados, assim como dados complementares gerados por ensaios exploratórios de destilação fracionada, mostraram grande viabilidade de uso da water phase como matéria-prima para a produção de essência natural de alta qualidade sensorial
Abstract: Consumers are attracted to passion fruit juice due to its exotic smell and flavor. Unfortunately, during the juice concentration, the volatile compounds responsible for the passion fruit smell and flavor are dragged along with the water, reducing the sensory quality of the concentrate. These volatile compounds can be condensed and recovered in an aqueous solution called "water phase". By submitting the water phase to a fractional distillation process, its volatiles can be concentrated, thus producing a GRAS natural fruit essence which can be added to the juice, increasing its sensory quality. In despite of being able to produce water phase, Brazilian tropical juice industries, usually lack the adequate knowledge and technology to produce GRAS natural essences. This study aimed: to characterize the profile of volatiles found in the passion fruit water phase produced by a Brazilian juice factory and, to evaluate the water phase potential for the production of a natural essence. The water phase¿s volatile compounds were isolated using a liquid-liquid extraction (dichloromethane) and identified by gas chromatography (GC) and mass spectrometry (GC-EM). Each volatile¿s aroma quality, power and possible contribution for the production of a passion fruit essence were evaluated through Osme GC-olfactometry technique. Thus, four experienced assessors evaluated the GC effluents in three replicates; their data were integrated by SCDTI software, generating an averaged consensual aromagram. Out of the 110 peaks detected in the chromatogram 71 were identified, totalizing 72% of the chromatogram total area. Thirty five volatiles were perceived in the GC effluents, 60% of which possessed pleasant fruit, floral or sweet like aromas, with predicted positive contribution for the production of a passion fruit essence. Among these compounds, those presenting the greatest aroma impact in the CG effluent were: ethyl butyrate (described as berry-like, tutti-frutti, grape); 3-hexenal (green, grass); methyl butyrate (sweet, fruity); ethyl hexanoate (citric, fruity); hexyl acetate (green, green fruit); rose oxide (sweet papaya); hexanal (grass, weeds), terpinen-4-ol (fruity, banana); hexanol (lemon scented disinfectant, weeds). Negativearoma-impact volatiles were also perceived in the CG effluent, such as: isobutanol and isobutyl acetate, described as "rubber" and "burnt wire"; as well as volatiles classified as "roasted¿ such as benzaldeyde and furfural. Combined with complementary data generated by exploratory assays involving fractional distillation, the results showed great viability of using this water phase as raw material for the production of high quality natural essences
Doutorado
Nutrição Experimental e Aplicada à Tecnologia de Alimentos
Doutor em Alimentos e Nutrição

Orientadores: Maria Aparecida Azevedo Pereira da Silva, Maria Regina Bueno Franco
Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos
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Resumo: Os salames são produtos cárneos fermentados e desidratados/maturados apreciados mundialmente e possuem características sensoriais peculiares, principalmente envolvendo o aroma e sabor. No Brasil este produto tem conquistado sucessivos recordes em faturamento no mercado interno, registrando R$ 265,3 milhões em vendas no ano 2005. Apesar de sua importância econômica, poucos estudos envolveram o perfil de voláteis do produto brasileiro e, nenhum deles avaliou a importância odorífera dos compostos voláteis. Assim, os objetivos do presente estudo foram: otimizar as condições de isolamento dos voláteis de salame para duas técnicas diferentes, headspace dinâmico (HD) e microextração em fase sólida (SPME); a partir destes métodos, caracterizar quantitativamente (CG-DIC) e identificar (CG-EM) os voláteis das amostras de salame brasileiro; determinar o impacto odorífero dos compostos voláteis (CV) presentes na amostra mais aceita pelos consumidores, por duas técnicas de CGO, OSME e Freqüência de detecção dos odores; determinar através da ADQ, o Perfil Sensorial dos salames e verificar a aceitação destes por consumidores potenciais; e por fim, correlacionar as medidas instrumentais com as sensoriais por métodos estatísticos multivariados. Foram analisadas seis amostras de salames brasileiros de dois tipos -Italiano (SI-1, 2 e 3) e Milano (SM-1, 2 e 3)- produzidos por três grandes fabricantes. As condições ótimas de isolamento obtidas com o auxílio da metodologia de superfície de resposta para o método de HD corresponderam à 3h e 26¿ de captura a 40°C, enquanto que para o de SPME, foram 45 minutos de extração a 50°C. A representatividade do aroma original da amostra de salame obtido nas condições otimizadas por SPME (7,2) foi superior à alcançada pelo método de HD (6,4). No entanto, ambos os métodos foram eficientes para discriminar as amostras de salame através da composição de voláteis, apesar dos diferentes perfis cromatográficos. Nos dois casos, os resultados da Análise de Componentes Principais (ACP) revelaram que as amostras dos fabricantes 1 e 2 foram caracterizadas por compostos provindos principalmente da oxidação de lipídeos, da atividade proteolítica e da fermentação de carboidratos (aldeídos, ésteres, álcoois e cetonas alifáticas), enquanto que as amostras do fabricante 3 apresentaram áreas maiores dos compostos com o grupo funcional fenol e de algumas cetonas cíclicas. Adicionalmente, os salames SI-2, SM-2 e SI-3 distinguiram-se das amostras SI-1, SM-1 e SM-3, pela maior quantidade de terpenos, o que sugere um maior grau de condimentação para aquelas amostras. As análises realizadas por CG-O (OSME e Freqüência de detecção dos odores) revelaram elevada correspondência quando aplicada a um mesmo método de isolamento. Além disso, apesar das diferenças entre os métodos de isolamento empregados, foram comumente importantes para o aroma de salame tipo Italiano os compostos metilalilsulfeto, os ésteres acetato de metilpropila, butanoato de etila, 2- e 3-metilbutanoato de etila, 1-octen-3-ona, 2-ciclohexen-1-ona, 1-octen-3-ol, 2-nonanona, (E)2-octenal, linalool, ácido 3-metilbutanóico, p-guaiacol, p-creosol e 1,4-dimetoxi-2-metilbenzeno. No teste de aceitação, realizado com 96 consumidores, a amostra SM-1 apresentou maior escore de aceitação global, e juntamente com as amostras SI-1 e SI-2 formaram um segmento com a maior parte dos consumidores ajustados no Mapa Interno de Preferência. Os resultados da ADQ foram analisados em dois grupos de atributos: aparência/textura e aroma/sabor das amostras. No primeiro grupo, os atributos distribuição da gordura e tamanho dos glóbulos de gordura discriminaram as amostras em função dos tipos dos salames e a cor vermelha diferenciou os fabricantes. Já os atributos de aroma e sabor foram correlacionados com 51 compostos voláteis (SPME), selecionados pelo seu elevado poder de discriminação das amostras e importância odorífera, juntamente com as propriedades físico-químicas, por PLSR-2. Assim, as amostras do fabricante 3 foram caracterizadas por aroma e sabor de defumado, as quais mostraram elevada correlação com os compostos fenólicos e cetonas cíclicas. O salame SM-2 apresentou maior proporção de compostos provenientes da oxidação lipídica e foi fortemente correlacionado com os atributos aroma e sabor de ranço. Já as amostras SI-2 e SM-1 foram descritas com aromas ácido e de gordura e sabor de gordura, e foram correlacionadas com teores elevados de gordura e por CVs originados da oxidação de lipídeos e da degradação de proteínas e carboidratos. A amostra SI-1 apresentou elevada quantidade de ácido acético, metionol e dos compostos recentemente relatados e, ainda foi caracterizada pelo maior teor protéico. Com as mesmas variáveis, os modelos desenvolvidos para prever os escores dos atributos sensoriais mostraram ajustes adequados (r>0,9) e habilidade de previsão (erro padrão médio de 15,3%). Desta forma, este estudo proporcionou informações sobre a qualidade dos salames brasileiros, incluindo os perfis dos constituintes voláteis e sensoriais das amostras, além de determinar a importância odorífera dos voláteis da amostra mais aceita com relação ao aroma
Abstract: Dry-fermented sausages are meaty products resulting from fermentation and dehydration/ripening processes. They are produced and consumed worldwide because of their typical sensory characteristics mainly in relation to the aroma and flavor. In Brazil this product has reached successive record sales in the internal market, with a total sale of R$ 265 million during the year 2005. In spite of its increased commercialization in the country, few studies about the volatile compounds of Brazilian dried sausages were found and their odoriferous importance had not been evaluated. The aims of the present study were: to optimize the conditions for the isolation of the salami volatile compounds by two different techniques, dynamic headspace (HD) and solid phase microextraction (SPME); to characterize the volatile compounds of some Brazilian salami samples by a gas-chromatograph equipped with a flame ionization detector (GC-FID) and by massspectrometry (MS), using the optimized techniques of isolation; to determine the odoriferous impact of the volatile compounds of the most accepted sample by two olfactometric techniques, OSME and Frequency of odor detection; to determine the sensory profile of the samples by Quantitative Descriptive Analysis (QDA), verifying also their acceptability by potential consumers; and finally to correlate the instrumental and sensory data using multivariate statistic techniques. Six different Brazilian dried sausage samples of the Italian (SI-1,2,3) and Milan types (SM-1,2,3) from three important national producers were analyzed. The optimized conditions for the isolation of the volatile compounds determined with the aid of Response Surface Methodology were 3h 26¿ (trapping time) and 40°C (temperature trapping) for the HD technique and 45¿ (extraction time) and 50°C (extraction temperature) for the SPME. Evaluation of the original aroma of the sample extracted by SPME obtained a higher score (7.2) than that of the HD technique (6.4). However, both methods were efficient in discriminating the salami samples by comparison of the volatile compounds in spite of their different chromatographic profiles. The data obtained from the two methods interpreted by Principal Component Analysis revealed that the samples from producers 1 and 2 were characterized mainly by compounds arising from lipid oxidation, proteolytic activity and carbohydrates fermentation (aldehydes, esters, alcohols and aliphatic ketones). The samples from producer 3 were characterized by greater areas of phenolic compounds and by cyclic ketones. Additionally, the samples SI-2, SM-2 and SI-3 could be distinguished from the SI-1, SM-1 and SM-3 by a higher amount of terpenes, suggesting that more condiments were added to these samples. On the other hand, the analyses carried out by GC-O (OSME and Frequency) showed good agreement when applied to volatile compounds isolated by the same procedure. In spite of the different chromatographic profile obtained by the two methods, the compounds methylallylsulfide, methylpropyl acetate, ethyl butanoate, ethyl 2- and 3-methylbutanoate, 1-octen-3-one, 2-cyclohexen-1-one, 1-octen-3-ol, 2-nonanone, (E)2-octenal, linalool, 3-methylbutanoic acid, p-guaiacol, p-creosol and 1-4 dimethoxybenzene were considered important for the Italian type salami aroma by both olfactometry techniques. An acceptability test applied to 96 potential consumers showed that the SM-1 sample obtained the highest score of overall acceptability and together with the SI-1 and SI-2 samples, they formed a segment with the major part of the consumers adjusted in the Internal Preference Mapping. The QDA data were interpreted after division of the samples¿ attributes in two groups: appearance /texture and aroma/flavor. In the first group, the distribution of fat and size of fat globules discriminated the samples in terms of the salami types while the red color differentiated the producers. The attributes of aroma/flavor were correlated to 51 volatile compounds (SPME) which were selected because of their high discriminatory power in relation to the samples and the odoriferous importance, and to the physicchemical properties by PLSR-2. Thus, the samples of producer 3 were characterized by a smoke aroma/flavor and they showed a high correlation to phenolic compounds and cyclic ketones. The SM-2 sample, characterized by a high proportion of compounds arising from lipid oxidation, was strongly correlated to the aroma and flavor attributes of rancidity. The samples SI-2 and SM-1 were described by acidic and fatty aroma attributes and fatty flavor and they were correlated to high amounts of fat and also to the volatile compounds originating from lipid oxidation and from protein / carbohydrate degradation. The SI-1 sample showed high amounts of acetic acid, metionol, the recently reported compounds and total protein. Considering the same variables, the models developed in order to predict the scores of the sensory attributes of the samples showed adequate adjustment (r>0.9) and prediction ability (mean standard error of 15.3%). Thus, this study provided some information concerning the quality of Brazilian salami samples, including the volatile and sensory profiles, in addition to the determination of the odoriferous importance of the volatile compounds present in the most accepted salami aroma
Doutorado
Consumo e Qualidade de Alimentos
Doutor em Ciência de Alimentos

Orientador: Maria Aparecida A. P. da Silva
Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos
Made available in DSpace on 2018-08-05T15:54:43Z (GMT). No. of bitstreams: 1 Almeida_SelmaBergara_D.pdf: 1651470 bytes, checksum: a5ee60dbc52c3dc1aeab330822f4380b (MD5) Previous issue date: 2006
Resumo: Para a recuperação do aroma e sabor de fruta fresca ao suco industrializado, subprodutos do processamento do suco de laranja, como óleo essencial e essências aquosa e oleosa, são normalmente reincorporados ao produto processado. A adição de cada um desses subprodutos confere ao produto final qualidade e estabilidade sensoriais distintas. O presente trabalho teve por objetivo avaliar a qualidade e estabilidade sensoriais do suco de laranja reconstituído, produzido com laranjas de variedades brasileiras e aromatizado com quatro diferentes aromas naturais de laranja, quais sejam: I - óleo essencial; II - frações destiladas de essência oleosa (oil phase); III - aroma formulado contendo frações destiladas de óleo essencial e de essência oleosa; e, IV - aroma formulado contendo frações destiladas de óleo essencial, frações destiladas de essência oleosa e de essência aquosa (water phase). Assim, esta pesquisa consistiu em quatro etapas, a saber: avaliação do impacto dos quatro aromas naturais sobre a aceitação e perfil sensorial do suco de laranja pronto para beber em condições pré-processamento térmico; avaliação da estabilidade sensorial dos aromas naturais ao processamento térmico do suco; avaliação do impacto dos aromas naturais sobre a estabilidade sensorial do suco pronto para beber durante o armazenamento da bebida e, finalmente, a identificação de compostos voláteis odoríferos presentes em um dos aromas mais estáveis - Aroma III. Quatro formulações de suco de laranja reconstituído foram elaboradas, adicionando-se os aromas I, II, III e IV, processadas e envasadas assepticamente em garrafas PET. Os perfis sensoriais, através de Análise Descritiva Quantitativa, e a aceitação das quatro formulações de suco de laranja pronto para beber foram avaliados antes e após o processamento térmico, bem como durante o armazenamento da bebida por 20, 40, 60 e 90 dias. Índices de escurecimento e teores de vitamina C foram determinados durante o armazenamento. Adicionalmente, amostras comerciais de suco de laranja pronto para beber foram avaliadas. Os dados foram analisados por ANOVA, teste de média Tukey ou t-Student, Mapa de Preferência, Análise de Componentes Principais, análise de correlação de Pearson e análise de regressão linear dos parâmetros sensoriais em função do tempo de armazenamento da bebida. O aroma III foi avaliado por cromatografia gasosa (CG), CG-olfatometria (Osme) e espectrometria de massas. Os resultados obtidos na primeira etapa da pesquisa sugeriram que a reincorporação dos compostos voláteis provenientes da essência oleosa contribuem menos para aumentar a aceitação do suco de laranja do que aqueles provenientes do óleo essencial. Em contrapartida, as amostras comerciais tiveram aceitação modesta entre os consumidores indicando que, no Brasil, os sucos de laranja comerciais podem ainda ter sua qualidade sensorial melhorada pela adição de novos aromas naturais. Na segunda etapa, a avaliação da aceitação das amostras pré e pós-processamento indicou boa estabilidade dos aromas naturais estudados ao processamento térmico. Os perfis sensoriais das formulações sugeriram que: i) a reincorporação ao suco de frações destiladas dos três subprodutos do processamento da laranja, resulta em maior estabilidade térmica do que aromas derivados apenas do óleo essencial; e, ii) a presença de voláteis provenientes da essência aquosa no aroma natural de laranja, mesmo que em proporções minoritárias, realça no suco notas de sabor de suco natural e suaviza as notas de aroma e sabor de casca de laranja. Na terceira etapa, durante o armazenamento da bebida, a formulação contendo apenas frações de essência oleosa apresentou, notadamente, menor estabilidade sensorial do que as demais formulações, contendo compostos voláteis provenientes do óleo essencial. Possivelmente essa ocorrência seja devida à presença de agentes antioxidantes naturais nas frações derivadas do óleo essencial. Adicionalmente, os resultados sugeriram que a adição ao suco de laranja de frações destiladas de óleo essencial resulta em melhor estabilidade sensorial à bebida do que a adição ao suco do óleo essencial na sua forma integral. Em todas as amostras, ao longo do período de armazenamento, ocorreu queda dos teores de vitamina C e concomitante escurecimento dos sucos. Finalmente, na última etapa, foram gerados 55 picos de odores, os quais apresentaram, predominantemente, notas de aroma associadas à laranja. Beta-mirceno, butanoato de etila, a-pineno, hexanal, citral e decanol foram os compostos voláteis de maior importância odorífera identificados. Os compostos ß-terpineol, citronelal, undecanal, acetato de a-terpenila, acetato de nerila e a-cariofileno foram identificados como compostos de alto poder odorífero e, limoneno, linalol, a-terpineol e decanal, como compostos de baixo poder odorífero
Abstract: To restore the natural orange aroma and flavor to industrialized juices, processors add natural flavorings obtained from three orange juice by-products: the cold-pressed oil, the oil phase and the water phase. The addition of each of these by-products results in juices with distinct sensory characteristics and acceptability. The present work aimed at evaluating the sensory quality and stability of reconstituted orange juice from Brazilian varieties, flavored with four different orange natural aromas, which are: I ¿ essential oil; II ¿ distilled fractions of the oil phase; III - formulated aroma containing distilled fractions of the essential oil and of the oil phase e, IV ¿ formulated aroma containing distilled fractions of the essential oil, distilled fractions of the oil phase and of the water phase. Thus the present research was divided into four stages: evaluation of the impact of four natural aromas (I, II, III, IV) on the acceptability and sensory profile of ready-todrink orange juice before thermal treatment; evaluation of the sensory stability of the natural aromas to the thermal treatment of the juice; evaluation of the natural aromas impact to the sensory stability of ready-to-drink orange juice during storage; the identification of odor volatiles compounds in one of the most stable aromas ¿ Aroma III. Four reconstituted orange juices formulations were elaborated, by adding the above mentioned flavorings (I, II, III, IV), processed and packed in PET bottles. The sensory profiles, by using Quantitative Descriptive Analysis, and the acceptability of the four ready-to-drink orange juices were evaluated before and after the processing, and also during their 20, 40, 60 and 90 day-storage. In addition, other commercial samples of ready-to-drink orange juice were included in this study. Determinations of the ascorbic acid and the browning index of formulated juices were done as well. Data were analyzed by ANOVA, Tukey or t-Student mean test, Principal Component Analysis, Preference Mapping, Pearson¿s correlation analysis and linear regression analysis of sensory parameters as a function of the storage time. The aroma III was evaluated by gas chromatography (GC), GC-olfactometry (OSME) and by mass spectrometry. The results obtained from the first research stage suggested that reintroduction of the volatiles compounds from oil phase contribute less to increase the acceptability of orange juice than those from the essential oil. On the other hand, all the commercial samples presented moderate acceptability by consumers, indicating that the commercial orange juices in Brazil may have their sensory quality improved by adding new natural aromas. In the second research stage, the evaluation of the pre and post-processing samples acceptability indicated that the studied natural aromas presented good stability to the thermal treatment. The formulations sensory profiles suggested that: i) the reintroduction of the distilled fractions of the three orange processing by-products to the juice results in higher thermal stability than that caused by the aromas derived from the essential oil; ii) the presence of volatiles from distilled fractions of the water phase in the natural orange aroma, although in very small proportions, enhances natural juice flavor and softens orange peel flavor and aroma. In the third research stage, during the drink storage the formulation containing only distilled fractions of the oil phase presented much less sensory stability than the other formulations, containing volatile compounds from the essential oil. A possible explanation for this occurrence is the presence of natural antioxidants in those fractions derived from essential oil. Further, the results suggested that the addition of distilled fractions of essential oil to orange juice provides better sensory stability to the drink than the addition of the integral essential oil. During storage all samples showed decrease in vitamin C and simultaneous browning of juices. Finally, in the last research stage, Fifty-five odor peaks were generated, which presented aroma notes associated mostly to orange. Beta-myrcene, ethyl butanoate, a-pinene, hexanal, citral and decanol were identified as the highest aroma impact compounds. The compounds ß-terpineol, citronellal, undecanal, a-terpinyl acetate, neryl acetate and a-cariophylene were identified as high odor power compounds and, limonene, linalool, a-terpineol and decanal, as low odor power compounds
Doutorado
Doutor em Tecnologia de Alimentos

The roles of Ca2 + and cAMP in olfactory transduction were explored using agents which affect calcium channels and second messenger systems. These agents were applied at certain calculated final concentrations onto olfactory epithelia of urethane-anesthetized frogs (Sana PiPlens) by two-sec aerosol spray. During extracellular recording, saturated vapors of isoamyl acetate were delivered every 100 sec in 0.3 sec pulses to produce an electroolfactogram (EOG). Inorganic cations that block inward calcium currents inhibit EOG responses with the following rank order: (La3+) > (Zn2+, Cd2+) > (Al3+, Ca2+, Sr2+) > (Co2+). Application of 7.5 mM La3+ eradicates £0G's, while Ba2+ (which can carry more current that Ca2+) initially produces significant enhancement (F=43.04, p<0.001, df=19). Magnesium ion has no effect on EOG's at 7.5 mM, while 1.5 X 10"4M Ca2+ is significantly inhibitory (F=5.74; p=0.0355; df=12). Control aerosol sprays of distilled water depress EOG's by an average of 5%. The organic calcium channel antagonists diltiazem and verapamil inhibit EOG's by 17% and 36X, respectively, at a concentration of 1.5 X 10~*M. Verapamil produces significant inhibition (F=17.17; p=0.002; df=ll) at 1.5 X 10" 5 M, while the 1,4-dihydropyridine calcium channel antagonists, nicardipine and nifedipine, do not inhibit beyond 1% DMSO controls. Several calmodulin antagonists decrease EOG's, but without correlation to their anti-calmodulin potency. Application of 1.5 X 10"*M chlorpromazine and N-(6-aminohexyl)-5-chloro-l-naphthalenesulfonamide inhibit EOG's by 31% and 27%, respectively, while trifluoperazine inhibits by 23%. Dibutyryl cAMP, a lipophilic mimic of cAMP, produces 54% inhibition at 1.5 X 10" *M. Dibutyryl cGMP, cGMP, cAMP, and adenosine all decrease EOG's by less than 15% compared to distilled water controls. Forskolin, a reversible activator of adenylate cyclase, inhibits EOG's by 57% at 1.5 X 10"5M, which is significant beyond the 1% DMSO controls (F=17.17; p=0.002; df=ll). These data support the hypothesis that Ca2+ participates in olfactory transduction. Calcium ions could serve as charge carriers, second messengers, or both. Cyclic AMP could be involved with the primary excitatory process or sensory adaptation, or both.

Orientador: Maria Regina Bueno Franco
Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos
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Resumo: Apesar da importância do aroma e sabor para determinar a qualidade dos vinhos, praticamente não existe nenhum estudo sobre a composição de voláteis dos vinhos nacionais. Os poucos que existem utilizam ainda coluna empacotada e outros traçam apenas o perfil sensorial dos vinhos, sem fazer correlações dos dados com qualquer outro parâmetro. No presente trabalho estudou-se 11 vinhos seco varietal Cabernet Sauvignon oriundos das principais regiões produtoras do país: Serra Gaúcha e Campanha, no Rio Grande do Sul; do Vale do Rio do Peixe, em Santa Catarina e do Vale do São Francisco, região de Pernambuco/Bahia. Foram efetuadas análises dos constituintes químicos e minerais presentes, após a homogeneização de três garrafas de vinho. Os parâmetros físico-químicos foram determinados pelos métodos clássicos e os teores dos minerais cálcio, magnésio, ferro, cobre e zinco foram analisados por absorção atômica; potássio, lítio, sódio e rubídio por emissão de chama e o fósforo por colorimetria. As características sensoriais das amostras foram determinadas pelo uso da Análise Descritiva Quantitativa através de nove provadores selecionados e treinados. As amostras foram avaliadas em quintuplicata, em 11 sessões, utilizando blocos incompletos balanceados. O teste de aceitação também foi realizado e os dados avaliados utlizando-se o Mapa Interno de Preferência. Os componentes voláteis foram extraídos em triplicata de cada garrafa de vinho, através de uma técnica de extração em fase sólida utilizando coluna Lichrolut EN e eluíção com diclorometano, conforme metodologia já validada para análise de compostos voláteis em vinho. Os contituinte voláteis foram separados por duas colunas capilares de polaridades diferentes. A identificação dos voláteis foi realizada por espectrometria de massas, além da comparação dos índices de Kovats experimentais com os valores encontrados na literatura e comparação dos espectros dos compostos com os dos padrões disponíveis. O extrato da amostra de maior aceitação foi analisado pela técnica de cromatografia gasosa-olfatometria0 para identificar a contribuição dos diferentes compostos voláteis para o aroma global do vinho. Os resultados das análises físico-químicas mostraram que todos os vinhos estavam dentro dos padrões estabelecidos pela legislação vigente, sendo que os teores encontrados de acidez volátil foram considerados elevados. Os valores de pH também foram elevados, mas tal fato é esperado quando da avaliação de vinhos Cabernet Sauvignon. A análise de minerais mostrou que os teores de potássio estavam bem acima dos encontrados em literatura. A técnica estatística multivariada de Análise de Componentes Principais, aplicada ao teor dos componentes físico-químicos e dos minerais não foi capaz de discriminar as amostras em relação à sua origem geográfica. O emprego do Mapa Interno de Preferência demonstrou que a amostra 245 (Serra Gaúcha) foi a mais aceita pela equipe, sendo caracterizada por uma forte sensação de doçura, apesar do teor de açúcares (2,65±0,05 g/L), aroma frutado e de frutas vermelhas. Os vinhos da região nordeste obtiveram uma aceitação inferior junto aos consumidores, juntamente com a amostra 512 (Serra Gaúcha). Foram identificados pela primeira vez em vinhos nacionais, 39 compostos voláteis, sendo que 13 pertenciam à classe dos álcoois, 13 à dos ésteres, 7 à dos ácidos, 2 à das lactonas, além de 3 compostos carbonílicos e 1 composto fenólico. Apesar da variação da concentração dos compostos entre as amostras, o pico correspondente aos compostos 2-metil-1-butanol e 3-metil-1-butanol foi o mais abundante para todas as amostras, seguido pelo álcool feniletílico, lactato de etila e álcool isobutírico. A amostra 245 (Serra Gaúcha), que obteve a melhor aceitação, distinguiu-se das amostras 326 e 512 (Serra Gaúcha), de menor aceitação, pela alta concentração de acetato de etila, 1-butanol, 2-metil-1-butanol concomitantemente com o 3-metil-1-butanol, hexanoato de etila, 3-metil-1-pentanol, octanoato de etila e ácido hexanóico. Uma análise olfatométrica preliminar permitiu a detecção dos compostos voláteis odoríferos presentes na amostra de maior aceitação, além de estabelecer sua contribuição para o aroma total. Acetato de feniletila, furfural, hexanoato de etila, ácido hexanóico e butírico, além de um composto não identificado foram considerados importantes para o aroma do vinho estudado
Abstract: Despite the importance of flavour in determining the sensorial quality of wines, there are only few studies concerning the volatile composition of Brazilian wines. These few studies reported only major compounds, utilizing packed columns while other researchers described only the sensorial profile of the wines, without establishing any correlation of the data with other parameters. In the present study, 11 Cabernet Sauvignon red wines from main regions of the country were analysed: Rio Grande do Sul (Serra Gaúcha and Campanha); Santa Catarina (Rio do Peixe valley) and Pernambuco/Bahia (Rio São Francisco valley). Physical-chemical parameters were determined by classic analysis and the minerals content was determined by flame absorption and flame emission methods, after homogenization of 3 wine bottles. Nine selected and trained judges, utilizing Quantitative Descriptive Analysis, determined the samples¿ sensorial characteristics. They were evaluated in fiveplicates through 11 sessions. The acceptance test was realized with 87 consumers participation and data were interpreted utilizing Internal Preference Mapping (MDPREF). The volatile compounds were extracted in triplicates from each wine bottle and Total Analysis technique was used. A Lichrolut EN cartridge was utilized and elution with dichloromethane was performed, according to an already recognized in the literature methodology for volatile compounds analysis in wine. The volatile mixture of compounds was separated by high-resolution gas chromatography, utilizing two columns with different polarity phases. The identification of volatile compounds was realized by using mass spectrometer coupled to gas chromatography, besides comparison of Kovats experimental indexes with literature values and beyond that comparison between spectral mass data of the unknowns and those of the standards. A preliminary olfatometric test was realized using two selected and trained judges, who evaluated aroma of the eluted compounds of the highest preferred sample. Results of the physical-chemical and mineral analyses indicated that all samples were within the established legal limits. The amount of volatile acids was considered high, but such a fact is expected when Cabernet Sauvignon wines are evaluated. Potassium content of the samples was higher than already reported values in literature. The use of the MDPREF demonstrated that sample 245 was the highest preferred wine, characterized by a strong perception of the sweet, fruity and red fruit aroma descriptors. The northeast wines and sample 512 obtained the lowest acceptance among consumers. Thirty-nine volatile compounds were identified by GC-MS and Kovats Indexes in Brazilian wines by the first time, of which 13 were alcohols, 13 esters, 7 acids, 2 lactones, 2 terpenes, 3 carbonyl compounds and a phenolic compound. In spite of the great variation observed among the samples, 3-methyl butanol and 2-methyl butanol peaks were the most abundant compounds, followed by phenylethyl alcohol, ethyl lactate and isobutyric acid. The previous olfatometric test applied to the extract of the most preferred wine leaded to the detection of the odoriferous volatile compounds responsible for their acceptance while determining the contribution of those compounds to the global aroma. Hexanoic acid, furfural, butanoic acid and ethyl hexanoate were considered important contributors to the aroma of this preferred sample. ACP applied to physical-chemical and mineral content of the samples was not able to discriminate different samples according to their geographical origin
Doutorado
Doutor em Ciência de Alimentos

Hop cones, the immature inflorescences of the female plant of Humulus lupulus L., have an important role in defining flavour, bitter stability and shelf life of beer. Hop cones are characterised by a wide range of molecules, such as α- and β-acids that contribute to the bitter taste of beer, and essential oils, which are responsible for the aroma. Nowadays hop is mainly cultivated in other countries and imported in Italy as raw material. Despite hop’s cultivation is not widespread in Italy, the number of Italian microbreweries is increasing and most of them are located in Northern-Italy. Taking into accounts this geographical distribution, it is therefore interesting to determine the achievable quality of hops cultivated in the Northern-Italy area. Among factors that limit the crop production, water availability is one of the major constraint since, in Mediterranean areas, the phenological cycle of hops coincides with a climate characterized by high air temperature and drought. For this reason, the selection of hop drought-tolerant varieties is crucial for the introduction of this crop in Italy. Hop physiological, molecular and metabolic responses activated in response to drought are poorly understood. For this reason eleven hop cultivars were subjected to drought and physiological and ionomic parameters were measured throughout water stress development. A total of 8 plants for each cultivar (4 controls and 4 water stressed-plants) were used. 3-L pots were sealed to avoid water evaporation, then control plants were watered every day while stressed plants were left without irrigation till the achievement of permanent wilting (after about 30 days). Physiological and growth parameters (pots weight, leaves axes, shoots length and SPAD chlorophyll meter) were measured. Results highlight that, compared to well-watered plants, most of stressed hop varieties did not reduce their transpiration until the Fraction of Transpirable Soil Water (FTSW) ≈0.7, showing, in general, an anisohydric behaviour. The experiment allowed us to pinpoint the more drought-tolerant/susceptible hop cultivars. Besides the selection of drought-tolerant cultivars, it is important to verify the achievable quality of hops cultivated in Northern-Italy and its variability among different cultivation years. Although the effect of climatological conditions on α and β-acids formation is well-known, no information are available on the variability of hops’ volatile profiles among different growing seasons. For this reason, hop acids and volatile compounds profiles of sixteen hop varieties cultivated in the same field in Parma (Emilia-Romagna, Italy) in two different years were analysed via High Performance Liquid Chromatography (HPLC) and comprehensive two-dimensional gas chromatography (GCXGC) respectively. In general, a strong variability in the dependence of the amount of hop acids and volatile compounds on the climate was found, nevertheless, hop acids and the key compounds of aroma showed a pattern specific for each variety. Moreover, cones of ten hop varieties cultivated in 2013 were subjected to ultrasonic extraction and the extracts were used to flavour a Blond Ale beer. Each beer was then sensory analysed by a trained panel. Finally, the sensory properties of flavoured beers were evaluated in relation to hops’ volatiles profiles and correlations were pinpointed. High and significant (p< 0.05) correlation coefficients were find between specific volatile compounds and aromatic descriptors as ‘hoppy’, ‘grassy’ and ‘spicy’, while few volatiles correlated with the descriptors ‘citrusy’, ‘fruity’ and ‘floral’. A chemical and sensory characterization of volatile compounds in different hop varieties was also performed to identify the odour-active molecules of particularly citrusy hops. Indeed, although different odour impressions such as grassy, floral/fruity or spicy notes have already been described, few attempts were made to clearly correlate the citrus aroma with the chemical profile of hop oil. The essential oil of three hop varieties with a well-known ‘citrus’ character and of three ‘spicy’/’hoppy’ varieties were chemically and sensory analysed. Each essential oil was fractionated by Solid Phase Extraction (SPE) and, according to a descriptive sensory analysis of the different fractions, the 70/30 ethanol/water (v/v) SPE fraction turned out to be the most citrusy one. This fraction was then analysed via Headspace Solid Phase Microextraction (HS-SPME) and Gas Chromatography−Mass Spectrometry/Olfactometry (GC-MS/O). A total of 59 volatiles were identified, 35 of which resulted to be odour-active. In this study the character-impact odorants in the citrusy fraction of hop essential oil were outlined; hierarchical cluster analysis and Principal Component Analysis (PCA) highlighted that hops that expressed a typical citrus aroma are characterized by high levels of specific esters as methyl (E)-4-decenoate, methyl nonanoate and methyl caprate, high levels of esters of geraniol and nerol and low levels of ‘grassy/spicy’ sesquiterpenes as α-humulene and β-caryophyllene. Summarizing, in this work different responses to drought stress were highlighted in different hop cultivars, allowing us to determine the most tolerant and drought-sensitive hop cultivars. The quality of hops cultivated in Northern-Italy (expressed as hop acids content and volatile profile) and its variability were outlined for two cultivation years and some important odour impressions in hops (especially ‘citrusy’ notes) were characterized by a molecular point of view. This project has therefore increased our understanding of hop response to drought stress and of hop aroma, providing initial practical benefits for hop growers and for the hop industry.
I coni di luppolo, le infiorescenze femminili della pianta Humulus lupulus L., hanno un ruolo importante nella definizione dell’aroma, della stabilità dell’amaro e della shelf-life della birra. I coni di luppolo sono caratterizzati dalla presenza di particolari sostanze, ad esempio gli α- e β-acidi che contribuiscono al sapore amaro della birra, e gli oli essenziali, responsabili dell’aroma. Attualmente il luppolo viene coltivato principalmente in altri Paesi e importato in Italia come materia prima. Nonostante la coltivazione di luppolo non sia molto diffusa in Italia, il numero di micro-birrifici è in continua crescita e la maggior parte di essi è localizzata nel Nord-Italia. Considerando questi dati, risulta interessante determinare la qualità ottenibile da luppoli coltivati in quest’area. La disponibilità d’acqua è uno dei maggiori fattori ambientali che limita la produzione e nell’area del Mediterraneo il ciclo fisiologico del luppolo coincide con un clima caratterizzato da alte temperature e periodi siccitosi. Perciò, la selezione di cultivar di luppolo più tolleranti allo stress idrico è di cruciale importanza per l’introduzione di questa coltivazione in Italia. Ciò nonostante, le riposte fisiologiche, molecolari e metaboliche attivate in luppolo in risposta allo stress idrico sono poco conosciute. Per questo motivo dieci cultivar di luppolo sono state sottoposte a stress idrico prolungato e durante la cinetica di stress sono stati misurati alcuni parametri fisiologici e la concentrazione di alcuni ioni. Per l’esperimento è stato utilizzato un totale di 8 piante per ogni cultivar (4 piante controllo e 4 piante stressate). I vasi utilizzati (di un volume di 3 L) sono stati sigillati allo scopo di evitare l’evaporazione e, mentre le piante controllo sono state irrigate ogni giorno, le piante stressate sono state lasciate senza acqua fino al raggiungimento del coefficiente di avvizzimento permanente (dopo circa 30 giorni). Sono stati misurati parametri fisiologici e di crescita (peso dei vasi, assi fogliari, lunghezza degli internodi e valori di clorofilla misurati tramite SPAD). I risultati ottenuti hanno evidenziato come, comparate alle piante controllo, le piante stressate non riducono la loro traspirazione fino al raggiungimento di una frazione di acqua traspirabile nel terreno (FTSW) ≈0.7, mostrando in generale un comportamento anisoidrico. L’esperimento ha permesso di individuare le cultivar più tolleranti/sensibili allo stress idrico. Oltre alla selezione di cultivar di luppolo tolleranti allo stress idrico, è importante verificare la qualità ottenibile da luppoli coltivati in Nord-Italia e la sua variabilità tra diverse annate di coltivazione. Nonostante l’effetto delle condizioni climatiche sulla formazione di α e β-acidi sia ben conosciuto, non ci sono invece informazioni sulla variabilità delle molecole volatili del luppolo fra diverse annate. Per questa ragione, il profilo degli acidi e dei componenti volatili di sedici cultivar di luppolo coltivate nello stesso campo sperimentale a Parma (Emilia-Romagna, Italia) in due diverse annate sono state analizzate via Cromatografia liquida ad alta prestazione (HPLC) e Gas-cromatografia bidimensionale (GCXGC) rispettivamente. È stata evidenziata, in generale, una forte variabilità degli acidi e dei componenti volatili di luppolo in rispetto all’annata. Ciò nonostante, gli acidi del luppolo e i composti volatili chiave mostrano un pattern di base tipico per ogni varietà. In aggiunta, undici varietà di luppolo coltivate nel 2013 sono state sottoposte ad estrazione ad ultrasuoni, e gli estratti ottenuti sono stati utilizzati per aromatizzare una birra stile Blond Ale. Ogni birra aromatizzata è stata successivamente analizzata sensorialmente da un panel addestrato. Infine, le proprietà sensoriali delle birre aromatizzate sono state valutate in relazione al profilo volatile delle varietà ed alcune correlazioni sono state evidenziate. Sono state evidenziate correlazioni significative (p< 0.05) fra specifici componenti volatili e i descrittori aromatici ‘luppolato’, ‘erbaceo’ e ‘speziato’, mentre poche molecole volatili sono risultate essere correlate con i descrittori ‘agrumato’, ‘fruttato’ e ‘floreale’. Una caratterizzazione chimica e sensoriale dei componenti volatili in differenti cultivar di luppolo è stata effettuata anche allo scopo di identificare le molecole odorose di luppoli particolarmente agrumati. Infatti, nonostante differenti caratteristiche odorose come note erbacee, floreali/fruttate e speziate siano già state descritte, pochi tentativi sono stati effettuati per correlare chiaramente l’aroma agrumato con il profilo chimico del luppolo. Gli oli essenziali di tre varietà di luppolo con un noto carattere ‘agrumato’ e tre varietà di luppolo ‘speziate’/’luppolate’ sono stati analizzati chimicamente e sensorialmente. Ciascun olio essenziale è stato frazionato tramite estrazione in fase solida (SPE) e, grazie all’analisi sensoriale descrittiva delle diverse frazioni, la frazione SPE 70/30 etanolo/acqua (v/v) è risultata essere la più agrumata. Questa frazione è stata successivamente analizzata tramite microestrazione in fase folida in spazio di testa (HS-SPME) e Gas Cromatografia−Spettrometria di Massa/Olfattometria (GC-MS/O). Sono state individuate 59 molecole volatili, 35 delle quali sono risultate essere molecole odorose. In questo studio sono state caratterizzate le molecole odorose della frazione agrumata dell’olio essenziale di luppolo e grazie a clusterizzazione e analisi delle componenti principali (PCA) è stato possibile evidenziare che luppoli che esprimono un tipico aroma agrumato sono caratterizzati da alti livelli di particolari esteri come ad esempio metil (E)-4-decenoato, nonanoato di metile e decanoato di metile, alti livelli di esteri del geraniolo e nerolo e bassi livelli di sesquiterpeni ‘erbacei/speziati’ come ad esempio α-umulene e β-cariofillene. Riassumendo, in questo lavoro sono state evidenziate differenti risposte allo stress idrico in diverse cultivar di luppolo, permettendo di individuare cultivar più tolleranti e sensibili. La qualità di luppoli coltivati in Nord-Italia (espressa come concentrazione di acidi e profilo volatile) e la loro variabilità sono state delineate in due annate diverse ed alcune importanti caratteristiche organolettiche (specialmente la nota ‘agrumata’) sono state caratterizzate per la prima volta dal punto di vista molecolare. Questo progetto ha dunque aumentato la nostra conoscenza in merito alla risposta allo stress idrico in luppolo e in merito al suo aroma, fornendo informazioni basilari utili per coltivatori e per l’industria del luppolo.

Orientador: Maria Aparecida Azevedo Pereira da Silva
Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos
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Resumo: O suco concentrado de caju apresenta grande potencial de mercado, mas tem sua receptividade prejudicada em decorrência da perda, por evaporação ou degradação, de compostos voláteis importantes para o aroma e sabor da bebida. Os objetivos desta pesquisa foram: conhecer a dinâmica da perda e formação de voláteis durante a concentração do suco de caju por evaporação, avaliar o impacto dessas alterações sobre o perfil sensorial da bebida ao longo do processo de concentração, e identificar a importância odorífera dos voláteis perdidos e formados. Suco fresco de caju (clone CCP76) foi concentrado de 10,3°Brix a 42,1°Brix em evaporador piloto tipo termo-sifão, operando em sistema fechado, com vácuo de 700mmHg e com vapor a 110oC. Ao longo do processo de concentração cinco amostras de suco foram recolhidas. Seus teores de sólidos solúveis foram de 11,8°Brix, 14,9°Brix, 20,2°Brix, 29,6°Brix e 42,1°Brix. Os voláteis do suco fresco e das cinco amostras de suco concentrado foram extraídos por método de enriquecimento dos vapores do headspace em armadilha contendo polímero poroso (Porapak®), procedendo-se duas horas de captura sob vácuo de 70mmHg, e eluição dos voláteis capturados em acetona. Os voláteis foram identificados por cromatografia gasosa-espectrometria de massas (CG-EM) e quantificados por padronização externa, utilizando-se 12 padrões de diferentes classes químicas. A importância odorífera dos voláteis presentes nos isolados do suco fresco e do suco concentrado a 42,1°Brix foi avaliada pela técnica de cromatografia gasosa-olfatometria (CG-O) Osme. O perfil sensorial do suco fresco e das cinco amostras de suco concentrado foi gerado pela técnica de Análise Descritiva Quantitativa (ADQ®). Os dados sensoriais foram analisados por ANOVA, Tukey (p=0,05) e Análise de Componentes Principais (ACP). Modelos preditivos gerados para avaliar a dinâmica da perda e formação de ésteres, terpenos, álcoois, aldeídos, cetonas e hidrocarbonetos ao longo da concentração do suco de caju, indicaram que logo na primeira etapa de concentração, quando o suco foi concentrado até 11,8°Brix, foram perdidos aproximadamente 95% dos terpenos, 85% dos ácidos e cerca de 50% das cetonas e aldeídos. Já na segunda etapa do processamento, quando a bebida foi concentrada até 14,9°Brix, foram perdidos mais de 90% dos ésteres inicialmente presente no suco fresco, 85% dos álcoois e 90% dos hidrocarbonetos. Quando o suco atingiu 20,2°Brix, o conteúdo de álcoois e principalmente de hidrocarbonetos passou a aumentar, sugerindo uma possível formação de voláteis dessas classes químicas nas etapas finais de concentração do suco. Alterações significativas no perfil sensorial ocorreram a partir da concentração do suco acima de 20,2°Brix, com destaque para o aumento na intensidade de aroma e sabor cozido, aroma e sabor passado, aroma e gosto doce e redução de aroma e sabor de caju fresco. A análise CG-olfatometrica e correlações entre os dados instrumentais e sensoriais identificaram os seguintes voláteis como marcadores potenciais da intensidade de aroma e sabor de caju fresco na bebida: isovalerato de metila, 2-metil-butanoato de etila, butanoato de etila, isovalerato de etila, hexanoato de etila, butanoato de metila, 2-metil-butanoato de metila e 2-metilene-butanoato de etila. Por sua vez, os voláteis pentanal, tolueno, salicilato de homomentila, psi-cumeno e acetato de 1-metil-hexila correlacionaram-se positivamente com intensidade dos aromas e sabores de cozido e passado no suco de caju. De um modo geral, a perda de ésteres e terpenos ao longo da concentração do suco, associada ao aumento dos níveis de hidrocarbonetos promoveu alterações drásticas no perfil sensorial do suco concentrado. Uma adequada recuperação dos terpenos e ésteres evaporados no inicio do processo de concentração, seguida da sua reincorporação ao suco processado seria uma solução para a melhoria da qualidade sensorial do suco concentrado por evaporação
Abstract: Concentrated cashew apple juice shows considerable market potential, but its acceptability is affected by the loss of volatile compounds of importance to the aroma and flavor of the beverage, due to evaporation or degradation. The objectives of this research were: understand the dynamics of the loss and formation of volatiles during the concentration of cashew apple juice by evaporative concentration, evaluate the impact of these alterations on the sensory profile of the beverage throughout the concentration process, and identify the odiferous importance of the lost and formed volatiles. Fresh cashew-apple juice (clone CCP76) at 10.3ºBrix were concentrated to 42.1ºBrix in a pilot thermo-syphon type evaporator operating in a closed system with 700mmHg of vacuum and steam at 110ºC. Five juice samples were taken throughout the concentration process and were found to contain the following soluble solids contents: 11.8°Brix, 14.9°Brix, 20.2°Brix, 29.6°Brix and 42.1°Brix. The volatiles of the fresh juice and of the five concentrated samples were extracted from the headspaces for two hours using a vapor enrichment method with a trap containing the porous polymer Porapak® under a vacuum of 70mmHg, followed by elution of the trapped volatiles into acetone. The volatiles were identified by gas chromatography-mass spectrometry (GC-MS) and quantified by external standardization using 12 standards of different chemical classes. The odoriferous importance of the volatiles present in the isolates from the fresh juice and from that concentrated to 42.1ºBrix were evaluated by the Osme gas chromatography-olfactometry (GC-O) technique. The sensory profiles of the fresh juice and of the five samples of concentrated juice were generated by Quantitative Descriptive Analysis (QDA®). The sensory data were analyzed by ANOVA, Tukey (p=0.05) and by the Principle Component Analysis (PCA). Predictive models generated to evaluate the dynamic of the loss and formation of esters, terpenes, alcohols, aldehydes, ketones and hydrocarbons during concentration of the cashew-apple juice indicated that in the first step of concentration, when the juice was concentrated to 11.8ºBrix, approximately 95% of the terpenes were lost, 85% of the acids, about 50% of the ketones and aldehydes. In the second processing step when the beverage was concentrated to 14.9ºBrix, more than 90% of the esters initially present in the fresh juice were lost, more than 90% of the hydrocarbons and 85% of the alcohols. When the juice reached 20.2ºBrix, the content of alcohols and principally that of hydrocarbons starting increasing again, suggesting the formation of volatiles from these chemical classes in the final juice concentration steps. Significant changes in the sensory profile occurred when the juice was concentrated to 20.2ºBrix or above, highlighting increases in the cooked flavor and aroma, overripe flavor and aroma and sweet flavors and aromas, with reductions in the fresh cashew apple flavor and aroma. The GC-olfactometry analysis plus correlations between the instrumental and sensory data identified the following volatiles as potential markers of the intensity of fresh cashew apple flavor and aroma in the beverage: methyl isovalerate, ethyl 2-methyl butanoate, ethyl butanoate, ethyl isovalerate, ethyl hexanoate, methyl butanoate, methyl 2-methyl butanoate and ethyl 2-methylene- butanoate. On the other hand, the volatiles pentanal, toluene, homomenthyl salicylate, psi-cumene and 1-methyl-hexyl acetate correlated positively with the intensities of the cooked and overripe aromas and flavors of cashew apple juice. In general it can be conclude that the loss of esters and terpenes during concentration of the juice, associated with the increase in hydrocarbons resulted in drastic changes in the sensory profile of the concentrated juice. One possible solution for improvement of the sensory quality of the concentrated juice could be an adequate recovery of the terpenes and esters evaporated off at the start of the concentration process by evaporation, followed by their reincorporation into the processed juice
Doutorado
Consumo e Qualidade de Alimentos
Doutora em Alimentos e Nutrição

Les nuisances causées par les odeurs sont devenues un problème environnemental et de santé publique majeur au cours des dernières décennies, surtout dans les zones densément peuplées. Pour cette raison, les odeurs environnementales sont un sujet de préoccupation mondiale et qui reçoivent une attention de plus en plus importante au Brésil. Cependant, il manque aux autorités brésiliennes les instruments réglementaires pour prévenir ou atténuer ces impacts. Plus précisément, au niveau national, aucune législation n’établit des limites d’exposition aux odeurs (critères d’acceptabilité) basé sur les facteurs FIDOL (i.e., fréquence, intensité, durée, offensivité et localisation) qui déterminent l’ampleur de l’effet expérimenté par le récepteur, qui peut être un individu ou un groupe d’individus dans une communauté exposée à des odeurs environnementales. En outre, à l’exception de l’état du Paraná (au sud) et la ville de Uberlândia (au sud-est du pays), aucune méthodologie basée sur l’olfactométrie (i.e., mesure de la réponse d’un jury à un stimulus olfactif), n’est ni standardisée ni reconnue. Dans ce contexte, ce travail de thèse vise à contribuer au développement de politiques publiques de lutte contre les nuisances olfactives au Brésil. Une approche est présentée pour l’évaluation des émissions odorantes d’un site d’équarrissage (une activité à fort potentiel de pollution environnementale) et mettre en évidence la nécessité d’établir un cadre légal et réglementaire pour les odeurs au Brésil, notamment un système d’agrément environnemental avec des critères de conformité spécifiques à chaque secteur de l’industrie. Conscient du besoin de tenir compte des caractéristiques et attributs de la juridiction, comme l’activité économique et la superficie du territoire, l’applicabilité de l’olfactométrie de terrain (en utilisant des appareils portables) a été évaluée pour le relevé d’un contour de panache d’odeur dans l’environnement. De plus, une recherche bibliographique et documentaire a été menée afin de fournir des éléments qui pourront aider les autorités locales dans le développement de solutions adaptées en référence aux expériences et pratiques utilisées à l’échelle internationale. Différents critères de conformité sont discutés et recommandés, sur la base d’une approche réglementaire qui prévoit l’adoption des Meilleures Techniques Disponibles (MTD) et l’établissement de Normes de Distances Minimales (NDM), Normes Maximales d’Emission (NME), Normes Maximales d’Impact (NMI), Normes Maximales de Nuisance (NMN; VIEIRA, 2013). Il est prévu que cette recherche promeut des discussions sur la gestion et la réglementation des odeurs au Brésil (y compris les citoyens, le gouvernement, l’industrie et le milieu académique) et puisse aider à soutenir le développement des structures juridique et réglementaire en vigueur, afin d’assurer un niveau minimum de confort et de protection à la population exposée à ce type de pollution
Annoying odours have become a major environmental and public health issue in recent decades, especially in densely populated areas. For this reason, environmental odours are a matter of global concern and have received increasing attention in Brazil. However, Brazilian authorities lack the regulatory instruments to prevent or mitigate such impacts. More specifically, at the national level, there is no legislation establishing odour exposure limits (acceptability criteria) based on the FIDOL factors (i.e., frequency, intensity, duration, offensiveness and location) that determine the magnitude of the effect experienced by the receptor, which may be an individual or a group of individuals in a community exposed to environmental odours. Moreover, except for the state of Paraná (in the southern) and the municipality of Uberlândia (in the southeast part of the country), no methodology based on olfactometry (i.e., the measured response of a jury to an olfactory stimulus) is neither standardised nor recognized. In this context, this doctoral thesis aims to contribute to the development of public policies for odour-nuisance control in Brazil. It presents an approach for the evaluation of odour emissions from a rendering plant (an activity with high potential for environmental pollution) and highlights the need to establish a legal and regulatory framework for odours in Brazil, including an environmental permitting system with industry-specific compliance criteria. In light of the necessity of considering jurisdiction-specific characteristics and features such as economy and land area, the applicability of field olfactometry (using portable equipment) was evaluated to outline the contours of an odour plume in the environment. Additionally, bibliographical and documentary research were conducted to provide information that may assist local authorities in developing tailored solutions by reference to experience and practices that have been employed internationally. Different odour compliance criteria are discussed and recommended, based on a regulatory approach that provides for the adoption of the Best Available Techniques (BAT) and the establishment of Minimum Distance Standards (MDS), Maximum Emission Standards (MES), Maximum Impact Standards (MIS) and Maximum Annoyance Standards (MAS; VIEIRA, 2013). It is expected that this research will foster discussions on odour management and regulation in Brazil (involving citizens, government bodies, industry and academia) and may help support the development of the legal and regulatory framework in force, to ensure a minimum level of comfort and protection for the population exposed to this type of pollution

Depuis leur apparition sur Terre, les Hommes utilisent les substances naturelles présentes dans leur environnement afin de répondre à leurs besoins vitaux. Ces matières premières, d'origine minérale, végétale ou animale, sont utilisées quotidiennement par les Hommes pour se nourrir, se protéger et s'abriter. Outre ces fonctions essentielles à notre survie, les matières végétales sont utilisées depuis l'Antiquité pour de nombreuses autres vertus : religieuses, curatives et odorantes. Des préparations à base de matières végétales étaient couramment obtenues à partir de fleurs, de plantes aromatiques mais aussi de gommes-résines d'encens, de myrrhe et de labdanum. Aujourd'hui encore, ces exsudats sont utilisés partout dans le monde pour leurs propriétés odorantes et médicinales. Cependant, leur composition phyto-chimique renferme encore de nombreux secrets, et de nombreux composés restent à découvrir et à caractériser. Récemment seulement, les acides olibaniques qui sont les odorants typiques de l'encens, ont été identifiés dans la résine de Boswellia sacra. D'autres composés d'encens, à intérêt médicinal tels que les acides boswelliques, méritent d'être quantifiés dans d'autres espèces d'encens peu étudiées. De même, dans l'huile essentielle provenant de la gomme résine de l'espèce de myrrhe Commiphora myrrha, des composés à intérêt olfactif restent à caractériser chimiquement afin de compléter les connaissances de ces plantes. Une autre plante à exsudat méritant d'être étudiée au regard de ses vertus odorantes est le Cistus ladanifer, dont la résine «labdanum» entre encore dans la composition de nombreux parfums. Une odeur puissante émane de cette plante typique de notre région méditerranéenne, et une identification exhaustive des odorants la composant est primordiale.Bien que de nombreux travaux aient été menés afin d'élucider la composition complète de ces résines, beaucoup de composés restent à caractériser et quantifier afin de les valoriser au mieux. Par conséquent, l'étude de ces matières premières aromatiques est aujourd'hui essentielle afin de percer les secrets de leurs vertus tant convoitées. Pour ce faire, diverses techniques d'extraction de ces matières premières (macération, extraction Soxhlet, hydro-distillation), et de séparation de ces composés (flash chromatographie, séparation sur colonne de silice en phase normale ou greffée au nitrate d'argent) ont été employées durant ce travail de thèse. De plus, plusieurs outils analytiques puissants pour identifier, caractériser, quantifier (GC-MS, RMN, GC-Olfactométrie, UHPLC-Orbitrap) et isoler (GC-préparative) ces composés ont été adoptés et optimisés, et seront abordés ici. Dans un premier temps, un chapitre permettant de situer le contexte bibliographique des études menées sur ces trois matières premières sera présenté. Un second chapitre présentera notre approche analytique afin de caractériser et valoriser composés lourds et semi-volatils de diverses espèces d'encens pour leur intérêt médicinal. Plusieurs méthodes d'extraction et d'analyse des composés d'intérêt médicinal ont été testées, optimisées et adaptées à la nature des composés à identifier. Des tests d'activité enzymatiques ont également été appliqués à plusieurs extraits d'une espèce d'encens, dans le but de la valoriser. Un troisième chapitre permettra de de caractériser et quantifier les odorants à fort impact de ces matières premières, grâce à une méthode développée et conçue pour l'analyse de composés à l'état de traces (GC-MS-SIDA), ainsi que par l'utilisation de techniques d'extraction efficaces (Kugelrohr distillation, vacuum distillation). Ce travail s'achèvera par un chapitre comportant une discussion et une conclusion générale portant sur les résultats obtenus au cours des travaux menés durant cette thèse, et ouvrira la discussion sur de futurs travaux et perspectives afin de compléter la caractérisation et la valorisation de diverses matières premières aromatiques
Since their origin on Earth, humans have used natural substances present in their environment to meet their vital needs. These raw materials, of mineral, vegetable or animal origin, are used by human beings every days to feed, protect and shelter themselves. In addition to these essential functions for our survival, plant materials have been used since Antiquity for their numerous virtues: religious, curative and odorant. Preparations based on raw plant material, were commonly obtained from flowers, aromatic plants but also gum-resins of incense, myrrh and labdanum. Even today, these exudates are used all over the world for their odorant and medicinal properties. However, their phytochemical composition still holds many secrets, and many compounds remain to be discovered and characterized. Only recently, the typical note of incense (due to olibanic acids), have been identified in the resin of Boswellia sacra. Other constituents of medicinal interest such as boswellic acids, deserve to be quantified in other less known incense species. Similarly, in the essential oil from the gum resin of the myrrh species Commiphora myrrha, compounds of olfactory interest remain to be chemically characterized in order to complete the knowledge of these plants. Another exudate deserving to be studied with regard to its odorant virtues is the one from Cistus ladanifer, whose resin "labdanum" still enters in the composition of numerous perfumes. A powerful odor emanates from this typical plant of our Mediterranean region, and an exhaustive identification of the odorants composing it is essential.Although many works have been done to elucidate the complete composition of these resins, numerous compounds remain to be characterized and quantified in order to make the best use of these resins. Therefore, the study of these aromatic raw materials is essential today to unravel the secrets of their coveted virtues. To that end, various techniques of extraction of these raw materials (maceration, Soxhlet extraction, hydro-distillation), and techniques of separation of these compounds (flash chromatography, separation on silica column in normal phase or grafted with silver nitrate) were used throughout this thesis work. In addition, several powerful analytical tools to identify, characterize, quantify (GC-MS, NMR, GC-Olfactometry, UHPLC-Orbitrap) and isolate (GC-preparative) these compounds have been adopted and optimized, and will be discussed here. In a first step, a chapter allowing to situate the bibliographic context of the studies carried out on these three raw materials will be presented. A second chapter will present our analytical approach to characterize and valorize non-volatile and semi-volatile compounds of various incense species for their medicinal interest. Several methods of extraction and analysis of compounds of medicinal interest were tested, optimized and adapted to the nature of the compounds to be identified. Enzymatic activity tests were also applied to several extracts of an incense species, in order to valorize it. A third chapter will allow to characterize and quantify the high impact odorants of these raw materials, thanks to a method developed and designed for the analysis of trace compounds (GC-MS-SIDA), as well as by the use of efficient extraction techniques (Kugelrohr distillation, vacuum distillation). This work will end with a chapter including a discussion and a general conclusion on the results obtained during the work carried out during this thesis, and will open the discussion on future work and perspectives to complete the characterization and valorization of various aromatic raw materials

Les émissions odorantes constituent un enjeu environnemental dont l'importance n'a cessé de croître dans les zones urbaines et industrielles. Les émissions anthropogéniques de composés soufrés contribuent à une concentration locale excédant fortement le seuil de perception. Afin de satisfaire des contraintes règlementaires de plus en plus strictes, les procédés biologiques dont la biofiltration sont une alternative intéressante car respectueuse de l'environnement et de moindre coût. Les seuils de perception des composés soufrés, très bas (µg. m-3), obligent à atteindre des efficacités d'abattement particulièrement élevées, le résiduel de concentration pouvant être à l'origine d'un impact notable sur les populations riveraines. L'étude a donc consisté à améliorer les performances des biofiltres concernant l'élimination des composés soufrés i) en ajustant certains paramètres opératoires clefs tels que le sens de circulation de l'effluent gazeux, le pH et l'ensemencement du matériau support, ii) en considérant le dimensionnement des biofiltres mis en œuvre (unités pilotes de laboratoire et semi-industrielles) et iii) la complexité du gaz à traiter (mono-polluant et mélange de composés à traiter)
Odorous emissions are a serious concern whose importance became higher in urban and industrial areas. Anthropogenic emissions of sulphur compounds lead to local concentration that exceeds strongly the odour threshold of human nose. In order to fulfil legal requirements that have become stricter in recent years, biological processes and biofiltration more accurately are an interesting alternative as biofilters provide an expanding variety of opportunities for economical and environmentally friendly solutions for many waste gas emissions. The odour thresholds of sulphur compounds are very low (µg.m3 air) and then require that biofilters provide high removal efficiency as the residual concentration can induce an odorous impact on neighbourhood populations.Hence, the study consisted in improving biofilters performances concerning sulphur compounds treatment i) by upgrading important operating parameters such as air flow distribution, pH and inoculation of packing material, ii) by considering biofilters design (laboratory and semi-industrial pilot units) and iii) the gaseous effluent complexity (only one pollutant and mixture of different compounds)

Hintergrund: Zur Begutachtung von Riechschäden werden immer häufiger objektive Befunde benötigt. Die bisher meist übliche Registrierung olfaktorisch evozierter Potenziale (OEP) ist technisch aufwändig und von der Atemtechnik des Probanden abhängig. Zur Diagnostik der Anosmie und Parosmie wird hier die methodisch einfachere Messung der "contingent negative variation" (CNV) eingesetzt. Patienten und Methode: An 25 Probanden mit normalem Riechvermögen und 16 Patienten mit dem subjektiven Befund einer Anosmie nach Unfallverletzung wurden OEP- und CNV-Messungen vorgenommen. Bei der "direkten" CNV sollte der Proband einen Ton aufmerksam erwarten, der einem Duftreiz nach 1,5 s folgte. Für die "selektive" CNV wurde nur einer von zwei zufällig wechselnden Duftreizen mit einem Ton als Zweitreiz markiert, der eine Erwartungsreaktion auslösen sollte. Ergebnisse: Für die beiden Versuchsarten wurde bei 21 bzw. 23 der Probanden mit normalem Riechvermögen eine eindeutige CNV gefunden. Das OEP fehlte in 4,3 % aller Messungen. Bei den Patienten mit Anosmie war in keinem Fall ein OEP bzw. eine CNV vorhanden. Die Amplituden der "selektiven" CNV sind signifikant höher als die der "direkten" CNV. Für die Ergebnisse bei weiblichen und männlichen Probanden ergab sich kein signifikanter Unterschied. Schlussfolgerung: Die Ergebnisse zeigen, dass ein objektiver klinischer Riechtest mit CNV-Ableitung möglich ist. Im Gegensatz zur OEP-Messung, deren Ergebnis von der Reaktion auf die Reizparameter abhängt, ist die CNV ein Maß für die kognitive Bedeutung des Reizes. Die einfache Reiz- und Messtechnik könnte zur weiteren Verbreitung der objektiven Olfaktometrie beitragen.
Background: An objective smelling test is indicated for a reliable assessment of olfactory disorders. Usually olfactory evoked potentials (OEP) are registered. But the technique of this measurement is complicated and the generation of the OEP depends on the respiration of the subject. Alternatively, the contingent negative variation (CNV) can be used in the diagnosis of anosmia and parosmia, requireing only a simple olfactory stimulator. Subjects and Method: OEP and CNV were derived from 25 adults with normal smelling and from 16 patients with anosmia after head injury. First, the "direct" CNV was registered when the subjects expected a tone following a smell stimulus after 1.5 s. Using two different odors in a random order, the tone only followed one of them, so the "selective" CNV was scored. Results: In both tests a distinct CNV was found in 21 and 23 normal smelling subjects, respectively. OEPs were absent in 4.3 % of this control group. No patient with anosmia showed an OEP or a CNV. The amplitudes of the "selective" CNV are significantly higher than those of the "direct" CNV. No gender dependency was found. Conclusion: The results show that an objective olfactometry can be realized by registration of CNV. Contrary to the measurement of OEP which depend on the physical parameters of olfactory stimuli, CNV correlates well with the cognitive identification of odor.

Afin d’identifier les composés responsables de l’arôme du gin, une procédure GC-O-MS se basant sur la fréquence de détection a été développée. Elle a permis de déterminer l’intensité odorante des composés volatils. Leur qualité d’odeur a pu être définie par le développement d’une roue des odeurs utilisée pour catégoriser les descripteurs obtenus. Cette approche nous a dans un premier temps permis d’identifier les composés potentiellement importants pour l’arôme du gin. L’origine de ces composés a ensuite été déterminée par l’étude de la fraction volatile de différents « botanicals » appartenant à la recette du gin. Cette stratégie nous a permis de constater que les baies de genièvre et les graines de coriandre étaient les principaux contributeurs en composés volatils d’impact. A l’opposé, les racines d’iris, la réglisse et les amandes ont semblé n’en apporter aucun. Nous avons donc distingué les « botanicals majeurs » et les « botanicals mineurs » selon leurs apports en composés volatils d’impact. Cette hypothèse a été globalement validée par différents tests sensoriels sur des mélanges de distillats. Enfin, une stratégie de recombinaison a été proposée dans le but de valider une sélection des composés d’impact. Une approche multicritères (intensité odorante, qualité d’odeur, propriétés physico-chimiques…) a abouti à la création de plusieurs recombinaisons. Celles-ci ont ensuite été analysées sensoriellement grâce à un test de tri-libre qui a permis de déterminer leur proximité avec le gin cible ainsi que les distances entre elles. Ainsi, une quinzaine de composés ont pu être identifiés comme influençant de manière importante la qualité aromatique du gin
In order to identify the compounds responsible for gin aroma, a GCO-MS procedure based on detection frequency analysis has been developed. It allowed the determination of volatile compound odorant intensity. Their odor quality has been defined thanks to a developed aroma wheel, used to categorize the obtained descriptors. This approach permitted the identification of gin aroma potential impact compounds. The origin of these compounds has then been determined by studying the different botanicals involved in the gin recipe. The obtained results showed that juniper berries and coriander seeds were the main contributors in terms of volatile impact compounds. At the opposite, orris roots, liquorice and almond did not seem to provide any of them. We thus differentiated the “major botanicals” from the “minor botanicals” according to their supply in volatile impact compounds. This hypothesis has been globally validated by different sensory tests on botanical distillate mixtures. Finally, a recombination procedure has been proposed in order to validate a selection of impact compounds. A multicriteria approach (odor intensity, odor quality, physic-chemical properties…) led to the creation of several recombinates. They have been sensorially analyzed by a free sorting task, which allowed determining their proximity with the target gin and the distance between them. Thus, around fifteen compounds have been identified as key compounds for gin aroma

En esta Tesis Doctoral se aplica la cromatografía de gases con detector olfatométrico (la nariz humana) en el análisis de los compuestos volátiles aromáticos de distintos alimentos: el vinagre de vino con Denominación de Origen Protegida “Vinagre de Jerez”, los pistachos tostados y el aceite de oliva. Los distintos métodos de preparación de muestra (la microextracción en fase sólida sobre el espacio de cabeza, o HS-SPME, y la extracción directa con disolvente, o DSE) han proporcionado extractos representativos del aroma de estos productos, y gracias a la técnica olfatométrica empleada (Aroma Extract Dilution Analysis o AEDA) se han identificado los odorantes más potentes. Así se ha logrado caracterizar el aroma de dichos alimentos, recogiéndose los resultados de las investigaciones realizadas en distintos artículos publicados en varias revistas internacionales.
In this Doctoral Thesis, the gas chromatography with olfactometry detector (the human nose) has been applied to analyse the volatile aromatic compounds from different foodstuffs: the wine vinegar produced under Protective Denomination of Origen “Vinagre de Jerez”, the roasted pistachios and the olive oil. The different sample pre-treatment methods employed (the headspace solid-phase microextraction, or HS-SPME, and the direct solvent extraction, or DSE) have provided representative aroma extracts from these products. Furthermore, and thanks to the olfactometric technique used (the Aroma Extract Dilution Analysis or AEDA), the most potent odorants have been identified. Thus, the aroma of all these foodstuffs has been characterized. All the results obtained from the research developed have been published in different international journals.

Orientador: Lireny Aparecida Guaraldo Gonçalves
Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos
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Resumo: Pretendeu-se através deste estudo levantar dados sobre frituras, em colaboração com agências fiscalizadoras das boas práticas de frituras. Estudou-se o grau de conhecimento de manipuladores de alimentos de 13 estabelecimentos comerciais de Campinas/SP, quanto às boas práticas de frituras, e avaliou-se a qualidade do óleo usado, através de métodos analíticos. Simulou-se, em triplicata, a fritura descontínua de alimentos cárneos empanados em fritadeira com capacidade de 28 L, utilizando dois tipos de óleos vegetais isentos de gorduras trans e disponíveis comercialmente: óleo de algodão e oleína de palma. Adotou-se temperatura de 182ºC e fritura por 4,5 minutos. Por vez, fritaram-se 400-500 g de alimentos. Ao longo do dia, realizaram-se 3 operações de fritura em horários estratégicos e a fritadeira permaneceu ligada a 182ºC por 8h. Não houve reposição com óleo fresco, nem filtragem do óleo. O tempo total de estudo variou de 6 a 17 dias de fritura, sem a troca do óleo e o final dos experimentos foi definido pela avaliação dos óleos usados com testes rápidos. Monitoraram-se os óleos de fritura através de análises físico-químicas: teor de ácidos graxos livres, compostos polares totais e compostos poliméricos, cor Lovibond, dienos conjugados, composição em ácidos graxos, estabilidade oxidativa e testes rápidos para avaliação da qualidade de óleo usado. Embora fossem adotadas as mesmas condições experimentais, mesma fritadeira e mesmo tipo de alimento frito e tipo de óleo, constatou-se que não há reprodutibilidade do processo de fritura. Os alimentos foram avaliados analiticamente e verificou-se perda de umidade, incorporação de óleo nos alimentos, pequenas alterações na composição em ácidos graxos e formação de quantidades desprezíveis de trans, podendo ser rotulados como alimentos zero trans. Estudou-se Texto 265, Viscofrit e Fri-check, testes rápidos de avaliação da qualidade do meio de fritura, utilizando 59 amostras de óleo de fritura. Testo 265 e Viscofrit são alternativas viáveis, se respeitadas suas limitações. Requerem-se estudos mais aprofundados com o Fri-check. Realizou-se, ainda, análise sensorial olfatométrica, na oleína de palma usada na fritura de frango empanado, com 4 julgadores treinados, em quadruplicata, utilizando o método desenvolvido na Universidade Estadual de Oregon (OSME). Os julgadores detectaram e descreveram odores de 135 compostos voláteis presentes no óleo usado de fritura. Trinta e um deles foram identificados por cromatografia em fase gasosa com detector de massas. Dentre eles, compostos não reportados anteriormente na literatura, demonstrando ineditismo do trabalho
Abstract: This study intended to raise data about frying to contribute with supervisor agencies of good practices of frying. The level of knowledge of food manipulators from 13 commercial establishments at Campinas city/SP was studied, in relation to good practices of fryings, and the quality of used oils was evaluated by analytical methods. It was simulated the discontinous frying of meat products with flour coating with a fryer of 28 L-capacity in triplicate, using two types of commercially available zero-trans oils: cottonseed and palm olein oils. The temperature of 182ºC and frying during 4.5 minutes were adopted. Each time, 400-500 g of food samples were fried. During the day, 3 frying operations were strategically performed and the fryer remained on at 182ºC for 8h. There was neither oil replacement, nor filtering. The total time of study varied from 6 to 17 days of frying, without oil exchanging and the end of the experiments was determined by the oil evaluation using fast tests. The frying oils were monitored through physico-chemical analyses: free fatty acids content, total polar compounds and polymeric compounds, Lovibond color, conjugated dienes, composition of fatty acids, oxidative stability and fast tests for evaluation of the quality of used oils. Although the same experimental conditions, the same fryer and the same types of fried food and oil were adopted, it was observed that there was no reproductivity in the frying process. The foods were analytically evaluated and loss of humidity, oil incorporation on foods, small changes in fatty acids composition and minimal amounts of trans-fatty-acid formation were verified, which enables to label them as zero trans food. Testo 265, Viscofrit and Fri-check, fast tests for evaluation of frying fat quality were studied, using 59 samples of frying oil. Testo 265 and Viscofrit are feasible alternatives, if their limitations are respected. Further studies with Fri-check are required. It was still performed olfactometry sensory analysis in the palm olein used in frying chicken breast with flour coating, through the Oregon State University method (OSME), with 4 trained judges, in quadruplicate. Judges detected and described odors of 135 volatile compounds present in the used frying oil. Thirty-one of them were identified by gaschromatography equipped with mass detector. Among them, it was found compounds not previously reported in the literature
Doutorado
Mestre em Tecnologia de Alimentos

Turkish Air Quality Control Regulation (AQCR) is in force since 1986. However, AQCR does not contain any standards for odour control. In order to respond to various odour complaints and handle odour problems in Turkey, a regulation for odour control is necessary. Since Turkey is a candidate country for European Union, environmental legislation of Turkey has to be improved to the standards of the other member countries. The purpose of this study is to investigate the &ldquo
odour problem&rdquo
in Turkey, specifically in Ankara, and to establish the odour measurement techniques. The techniques and information acquired throughout this study will form the basis of &ldquo
Odour Regulation&rdquo
in Turkey. For this purpose, odorous gas samples were collected from different industries in Ankara and these samples were analysed with the Olfactometer TO7. The results of the emission measurements have shown that there are numerous industries in Ankara which are discharging high concentrated odorous gases into the environment. Also, field measurements (immission measurements) were performed around a sugar factory in order to determine immission levels. At the end of the immission measurements, a setback distance (buffer zone) of 1.5 km is determined that should be around a sugar factory. The implementation of an odour regulation and odour control technologies in Turkey is expected in near future.

Ce travail de recherche a pour objectif de caractériser le vieillissement aromatique des grands vins blancs et rouges, afin de mieux comprendre l’impact de la perméabilité à l’oxygène des obturateurs (OTR) sur leur évolution. Le premier volet présente l’adaptation d’un protocole de coulométrie permettant de caractériser l’OTR du système d’obturation et son lien avec l’évolution sensorielle et moléculaire d’un vin blanc de Sauvignon conservés 12 ans en bouteille. Ces résultats ont permis de confirmer la forte hétérogénéité des vieux bouchons en liège naturel et plus généralement l’impact de l’obturateur sur un ensemble de marqueurs connus (thiols volatils, aldéhydes de Strecker, SO2 libre, DCO2) et de nouveaux marqueurs associés au bouquet. Ces résultats obtenus sur un nombre limité de vieux vins ont été étendus à l’ensemble des vins blancs d’une appellation de Bordeaux pour lesquels l’importance de la teneur en SO2 libre à la mise en bouteille et le choix d’un obturateur un liège microaggloméré figurent parmi les bonnes pratiques permettant de préserver le potentiel de garde de ce type de vins.Le second volet est dédié à l’étude du bouquet de vieillissement des vins rouges en lien avec l’OTR. Nos connaissances étant moins étendues que pour les vins blancs, ce travail a débuté par la caractérisation moléculaire de ce type d’évolution par deux approches d’identifications distinctes. Une fois préparé, l’extrait organique a été fractionné par CLHP. Après flairage des fractions, les plus intéressantes ont été analysées par chromatographie en phase gazeuse couplée à l’olfactométrie (CPG-O-TOF MS). Cette stratégie nous a permis d’identifier l’abhexone (5-ethyl-3-hydroxy-4-methyl-5H-furan-2-one) dans les vins rouges. La quantification de ce composé chiral par CPG-MS/MS sur colonne capillaire de type non-polaire ou chirale, montre l’impact de la durée du vieillissement sur la distribution de ses énantiomères. Pour la seconde approche nous avons développé une nouvelle stratégie de réduction accélérée (ART) à partir d’extraits de chêne (Q. petraea). Une fois les conditions de réaction optimisées, l’analyse des extraits par CPG bidimensionnelles (CPG-CPG-O-TOF MS) nous a permis d’identifier de nouveaux thiols rappelant le caractère « viande grillée » : le 2-methoxybenzenethiol, le 5-methylfurfurylthiol, le 2,5-dimethylfuran-3-thiol, l’o-toluenethiol, le 2,6-dimethylbenzenethiol et le 2,6-dimethoxybenzenethiol. Ce sont des composés soufrés dérivés du bois de chêne et produits par la réaction ART. Leur identification dans les vieux vins rouges a été réalisée conjointement par CPG-PFPD et CPG-MS/MS. L’étude de leur distribution en lien avec l’OTR du bouchon et leurs propriétés sensorielles montrent qu’ils contribuent, pour partie, au bouquet de vieillissement des vins rouges
The aim of this research is to characterize the aromatic aging of great white and red wines, in order to gain a better understanding of the impact of the oxygen permeability of the obturators (OTR) on their development. The first part presents the adaptation of a coulometric protocol to characterize the OTR of the obturator system and its relationship with the sensory and molecular evolution of a Sauvignon white wine aged 12 years in bottle. These results confirmed the considerable heterogeneity of old natural corks and, more generally, the influence of the closure on a series of known aromatic markers (volatile thiols, Strecker aldehydes, SO2, DCO2) and new markers associated with the bouquet. These results, obtained on a limited number of old wines, have been extended to all the white wines of a Bordeaux appellation, for which a high level of free SO2 at bottling and the choice of a microagglomerated cork stopper are among the best practices for preserving the ageing potential of this type of wine.The second part was dedicated to the study of the ageing bouquet of red wines in relation to OTR. Since our knowledge is less extensive than for white wines, this work began with the molecular characterization of this type of evolution using two separate identification approaches. Once prepared, the organic extract was fractionated by HPLC. After illuminating the fractions, the most interesting ones were analyzed by gas chromatography coupled with olfactometry (GPC-O-TOF MS). This strategy allowed the identification of abhexone (5-ethyl-3-hydroxy-4-methyl-5H-furan-2-one) in red wines. Quantification of this chiral compound by CPG-MS/MS on a non-polar or chiral capillary column shows the influence of ageing time on the distribution of its enantiomers. For the second approach, we developed a new accelerated reduction strategy (ART) using oak (Q. petraea) extracts. After optimizing the reaction conditions, the analysis of the extracts by two-dimensional GPC (CPG-O-TOF MS) allowed us to identify new thiols with a "grilled meat" character: 2-methoxybenzenethiol, 5-methylfurfurylthiol, 2,5-dimethylfuran-3-thiol, o-toluenethiol, 2,6-dimethylbenzenethiol and 2,6-dimethoxybenzenethiol. These are sulfur compounds derived from oak and produced by the ART reaction. Their identification in old red wines was carried out jointly by CPG-PFPD and CPG-MS/MS. The study of their distribution in relation to the OTR of the cork and their sensory properties show that they contribute, in part, to the ageing bouquet of red wines

Le nitrite est un ingrédient essentiel à la fabrication du jambon cuit, pourtant les risques sanitaires dont il est accusé remettent en question son utilisation. L’emploi de cet unique additif permet de remplir de nombreuses fonctions comme la protection antioxydante et antimicrobienne mais aussi le développement de la couleur et de l’arôme. C’est sur cette dernière fonction que ce travail de thèse s’est focalisé avec pour objectif la suppression du nitrite dans la fabrication du jambon cuit. La mise en œuvre de plusieurs techniques complémentaires de chromatographie en phase gazeuse couplées à l’olfactométrie a permis dans une première partie d’identifier le 2-methyl-3-furanthiol, 2-methyl-3-(methyldithio)furan, et le bis(2-methyl-3-furyl)disulfide comme les molécules soufrées responsables de l’arôme du jambon cuit. Il est apparu qu’en l’absence de nitrite et par conséquent en absence de protection antioxydante, les composés odorants issus de l’oxydation sont produits massivement et ont tendance à perturber l’arôme global du jambon cuit. Afin de restaurer l’arôme en l’absence de nitrite, l’étude a été organisée selon 2 axes : le premier visant à favoriser la production des molécules soufrées clés de l’arôme et le second visant à limiter la formation des composés d’oxydation perturbateurs de l’arôme grâce à l’utilisation d’antioxydants naturels. Les recherches ont été conduites sur des mini-jambons cuits modèles. La thiamine a été identifiée comme précurseur majoritaire du 2-methyl-3-furanthiol, du 2-methyl-3-(methyldithio)furan, et du bis(2-methyl-3-furyl)disulfide dans les conditions de fabrication du jambon cuit et des extraits d’acérola, de canneberge, d’oignon et de thé ont été sélectionnés pour leurs propriétés antioxydantes. L’évaluation en parallèle de l’oxydation et de l’arôme a montré que ces quatre extraits utilisés en mélange permettaient, non seulement d’égaler les performances antioxydantes du nitrite, mais aussi de rehausser la note aromatique « jambon cuit » par rapport à la formulation non nitritée de référence. L’association de la thiamine et des extraits végétaux a finalement permis de réaliser des jambons non nitrités qui, en termes d’arôme et d’oxydation, se rapprochent fortement d’un jambon nitrité. Les formulations réalisées constituent donc une première piste satisfaisante pour répondre à la problématique de la suppression du nitrite dans le jambon cuit. La protection antimicrobienne des nouvelles formulations doit être validée et la restauration de la couleur rose du jambon demeure une problématique organoleptique
Sodium nitrite is an essential ingredient in the cooked ham production process, yet its use is under challenge due to food safety concerns. Sodium nitrite is a multifunctional additive used for its ability to act on several fronts—from inhibiting oxidation and preventing microbial growth to giving desirable colour and aroma. This study focused on the aroma function under a wider objective to reduce nitrite use in cooked ham processing. Using several complementary methods with gas chromatography–olfactometry, we first identified 2- methyl-3-furanthiol, 2-methyl-3-(methyldithio)furan and bis(2-methyl-3-furyl)disulfide as the odour- active sulphur-compounds responsible for cooked ham flavour. It emerged that in the absence of nitrite—and therefore the absence of inhibited oxidation—the massive formation of an array of odour-active compounds produced by oxidative breakdown tended to disrupt the overall aroma of the final cooked ham. Next, in an effort to restore this aroma in the absence of nitrite, the study was organized into two strands, where the first strand aimed to promote the production of key aroma-active sulphur-compounds while the second strand aimed to minimize the formation of aroma-disruptive oxidation compounds by using natural antioxidants. This research was led on model cooked mini-hams. We identified thiamine as the major precursor of 2-methyl-3-furanthiol, 2-methyl-3-(methyldithio)furan and bis(2-methyl-3-furyl)disulfide under cooked ham production conditions, and we selected acerola, cranberry, onion and tea extracts as natural antioxidants. The coupled evaluations of oxidation and aroma showed that the formulated mixture of these four extracts not only equalled the antioxidant performances of added sodium nitrite but also lifted the “cooked ham” head note compared to the reference no-added-nitrite formulation. The association of thiamine and vegetal extracts ultimately made it possible to produce no-added-nitrite hams that, in terms of aroma and oxidation levels, proved almost identical to nitrite-added ham. The engineered formulations thus offer a good research track to suppress the sodium nitrite in cooked ham. The problem of how to restore the distinctive pink colour of cooked ham is an issue that remains to be resolved, and the ability of these new formulations to inhibit microbial growth needs to be validated

Ce mémoire de doctorat rassemble les travaux réalisés dans le cadre d’une étude analytique approfondie et systématique des substances à odeur boisée. Ces substances définissent une famille d’ingrédients unanimement appréciés pour leurs notes puissantes et recherchés par les parfumeurs pour composer les accords parmi les plus emblématiques de la profession. Les matières premières inscrites au programme de cette étude sont les essences de Gaïac, d’Araucaria, de Patchouli, de Cyprès Jaune d’Alaska, de Vétiver et d’Agarwood, ainsi que certains de leurs produits dérivés. La plupart de ces matières premières sont couramment utilisées par l’industrie du parfum. Leur spécificité provient de leur composition chimique très largement dominée par les dérivés sesquiterpéniques, conférant ainsi à ces extraits une complexité moléculaire indéniable. Les principaux objectifs de cette thèse de doctorat ont consisté à améliorer la connaissance de ces matières premières en termes de composition chimique, à déterminer autant que possible les composés odorants contribuant à leur odeur, et enfin d’explorer d’éventuelles voies de valorisation pour ces mêmes ingrédients à l’échelle industrielle.La méthodologie analytique développée tout au long de l’étude a nécessité l’utilisation combinée d’un large éventail de techniques chromatographiques, spectrométriques et spectroscopiques pour parvenir à caractériser ces matières premières au plus près et à réaliser l’isolement de leurs constituants inconnus. Ainsi, ces travaux s’articulent autour de quatre outils centraux : la chromatographie gazeuse bidimensionnelle intégrale couplée à la spectrométrie de masse (GC × GC–MS), la chromatographie gazeuse couplée à l’olfactométrie (GC–O), la chromatographie gazeuse semi-préparative (GC prép.) et la résonance magnétique nucléaire (RMN). Près de 190 composés ont été isolés et caractérisés dont 107 sont décrits pour la première fois comme constituants d’extraits naturels
This Ph.D. dissertation sums up the work carried out as part of a thorough and systematic analytical study of woody-scented substances. These substances define a family of ingredients unanimously appreciated for their powerful notes, and sought by perfumers to compose some of the most emblematic accords in perfumery. The raw materials included in the frame of this study are the oils of Guaiac, Araucaria, Patchouli, Alaska Yellow Cypress, Vetiver, and Agarwood, as well as some of their by-products. Most of these raw materials are ingredients commonly used by the perfume industry. Their chemical specificity comes from their composition largely dominated by sesquiterpene derivatives, giving these extracts an undeniable molecular complexity. The main objectives of this Ph.D. thesis were to improve the knowledge of these raw materials in terms of chemical composition, to determine as much as possible the odorous compounds contributing to their odor, and finally to explore possible ways of valorization for these products on an industrial scale.The analytical methodology developed throughout this study required the combined use of a wide range of chromatographic, spectrometric, and spectroscopic techniques in order to characterize these raw materials as precisely as possible and achieve the isolation of their unknown constituents. Thus, our work revolved around four central tools: comprehensive two-dimensional gas chromatography-mass spectrometry (GC × GC-MS), gas chromatography-olfactometry (GC–O), preparative capillary-gas chromatography (pc-GC) and nuclear magnetic resonance (NMR). Almost 190 compounds have been isolated and characterized, 107 of which are described for the first time as constituents of natural extracts

The natural enemies reported as biocontrol agents of stored products pests have showed promising characteristics to keep the damaging insects under the economic damaging level. Mainly, the studies conducted until now have been focalised on those natural enemies belonging to the families: Pteromalidae, Ichneumonidae, Braconidae and Trichogrammatidae. The biology and the applicative aspects of the parasitoids belonging to the family Bethylidae have been only partially evaluated, thus a lack of knowledge is present. The aim of this study was to collect the studies reported in the literature in order to summarize the information on bethilds reported as biological control agents. Afterwards, three experimental phases were conducted aiming at evaluating two bethilds candidate as biocontrol agents for stored products: Holepyris sylvanidis (Brèthes) e Cephalonomia waterstoni (Gahan) (Hymenoptera: Bethylidae). For the first natural enemy some aspects of the biology have been evaluated trying to underline possible applicative consequences. For both the parasitoids, the host searching behaviour has been evaluated in a four-chamber olfactometer.

Mestrado em Engenharia do Ambiente
As emissões de odores são cada vez mais valorizadas sob os pontos de vista ambiental e social, e resultam de várias fontes e actividades, tais como processos industriais e tratamento de resíduos e águas residuais. A implementação de medidas destinadas a minimizar o impacto de odores exige a respectiva avaliação da intensidade, do tom hedónico e da concentração de odor. Para realizar a medida da concentração de odor o método de referência usado baseia-se na Norma Europeia 13725. Este trabalho descreve o conjunto de especificações e procedimentos previstos na norma, para o efeito do desenvolvimento de uma tecnologia de olfactometria dinâmica, baseada num modelo de diluição dinâmica que é aplicado num equipamento. Os resultados preliminares obtidos mostram que a tecnologia desenvolvida tem condições mecânicas para cumprir as especificações da norma. Contudo o equipamento necessita da realização de um mais amplo conjunto de ensaios, ajustes, avaliação e cumprimento das especificações da referida norma. ABSTRACT: Emissions of odours are increasingly valued in the views environmental and social, and arise from various sources and different activities, such as industrial processes, waste and sewage treatment. The implementation of measures to minimize the impact of these odours requires the monitoring designed to assess the intensity, hedonic tone and odour concentration. The measurement of the odour concentration is carried out using the reference method based on the European Standard 13725. This work describes the set of specifications and procedures that standard requires, and also the model of dynamic dilution that is applied in a prototype. The preliminary results already obtained show that technology has the necessary conditions to be successful. However the prototype needs additional adjustments and an evaluation of the parameters described in the standard.

Leaves and fruit of nine apple (Malus x domestica Borkh.) genotypes were evaluated for insect injury in 1998 and 1999. Foliar and fruit injury from 12 insect species was inconsistently affected by genotype. Spraying trees with oil affected neither fruit insect injury nor fruit phytotoxicity. In choice feeding assays, incidence of Japanese beetle (JB) feeding and leaf area consumed was greater for 'Liberty' than for 'York.' Genotypes did not differ in no-choice feeding assays. Choice and no-choice feeding assays between apple and oak indicated that JB could distinguish host plants in an artificial environment. Trichome density appeared different among three genotypes. 'York', the non-preferred genotype, had highest specific leaf weight and concentration of phloridzin, a feeding repellent. 'Liberty' the preferred genotype, had the lowest specific leaf weight, and had the highest concentration of quercitrin, a feeding stimulant. Olfactory stimuli of JB was evaluated with a Y-tube olfactometer. Beetles preferred the side of the Y-tube containing leaf tissue of apple or Virginia creeper over the side with no leaf. Beetles did not choose one plant species over the other. Bias test of beetle orientation in the Y-tube olfactometer indicated that in the morning, but not the afternoon, beetles preferentially moved into the left side of the Y-tube. Humidity did not affect beetle orientation. In darkness JB preferred a leaf disc over a paper disc and beetles tended to remain on the leaf.
Ph. D.

Depuis la fin des années 90, la Maison Hennessy, par le biais de son Comité de dégustation expert, observe une diminution de la proportion d’eaux-de-vie à fort potentiel qualitatif. Ainsi, au moyen d’une thèse CIFRE menée avec l’UMR GENIAL, celle-ci a décidé de développer des moyens de caractérisation des eaux-de-vie et d’identifier des facteurs au sein de l’étape de distillation permettant l’obtention d’eaux-de-vie nouvelles plus qualitatives.Ces travaux se sont structurés autour des axes de recherche suivants : (i) la recherche des composés volatils clés par olfactométrie, (ii) le développement d’une méthode sensorielle descriptive quantitative, (iii) la mise en place d’un outil expérimental de distillation ainsi que la réalisation d’essais structurés sous forme de plans d’expériences et enfin (iv) l’étude du comportement des composés volatils au cours de la distillation discontinue.(i) La méthode de fast GC-Olfactométrie a permis l’identification de 7 composés volatils probablement impliqués dans la discrimination du potentiel qualitatif : acétaldéhyde, caproate d’éthyle, acétate d’héxyle, 3-méthylpentanol, 3-éthoxy-1-propanol, acide acétique, acide isobutanoïque.(ii) Le développement d’une méthode sensorielle de type QDA, a abouti à l’élaboration d’une liste de 19 descripteurs sensoriels caractéristiques des eaux-de-vie à fort potentiel ainsi que la création de 22 références aromatiques pour l’entraînement du panel. Le contrôle des performances a mis en évidence la nécessité de poursuivre l’entraînement de façon à disposer d’un panel fiable au sens de la norme AFNOR.(iii) La mise en place d’un hall muni d’alambics pilotes, associée au développement d’une méthodologie de distillation expérimentale et l’utilisation de plans d’expériences ont permis d’étudier l’incidence de 5 facteurs de distillation sur la qualité des eaux-de-vie nouvelles. Les résultats laissent présager d’un effet positif d’une plus grande hauteur de col-de-cygne et de l’absence de recyclage des queues.(iv) Enfin, l’étude du comportement des composés volatils au cours de la distillation a validé une classification établie précédemment dans la littérature et a mis en évidence la possibilité d’utiliser un logiciel commercial de simulation pour représenter leur comportement
Since the end of the 1990's, the Maison Hennessy, thanks to the expertise of its Tasting Committee, has noticed a decrease in the proportion of eaux-de-vies with high qualitative potential. Thus, with the help of a CIFRE thesis led in cooperation with UMR GENIAL, it has been decided to develop means of characterisation of eaux-de-vie and identify factors within the distillation process that will enable the production of more quality-oriented new eaux-de-vie.These works have been structured around the following themes: (i) research of key volatile compounds through olfactometry, (ii) development of a descriptive and quantitative sensory method, (iii) setting up an experimental distillation tool as well as the implementation of structured trials in the shape of designs of experiments, and finally (iv) behavioural study of volatile compounds during batch distillation.(i) The fast GC-Olfactometry method enabled us to identify 7 volatile compounds probably involved in the discrimination of the qualitative potential: acetaldehyde, ethyl caproate, hexyl acetate, 3-methylpentanol, 3-ethoxy-1-propanol, acetic acid, isobutanoic acid.(ii) The development of a QDA-type sensory method led to the elaboration of a list of 19 sensory descriptors representative of eaux-de-vie with strong potential as well as the creation of 22 aromatic references for panel training. The control of performances highlighted the necessity to pursue further the training in order to benefit from a reliable panel according to AFNOR.(iii) The set-up of a dedicated room equipped with pilot pot-stills, associated with the development of an experimental distillation methodology and the use of designs of experiments, enabled to study the effect of 5 distillation factors upon the quality of new eaux-de-vie. The results foreshadow a positive influence of a taller swan's neck and an absence of recycling of tails.(iv) Finally, the behavioural study of volatile compounds during distillation validated a classification previously established in literature and has highlighted the possibility to use a commercial simulation software to describe their behaviour