Relevant bibliographies by topics / Static headspace method (SHS)

Academic literature on the topic 'Static headspace method (SHS)'

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Published: 4 June 2021
Last updated: 20 February 2023

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Journal articles on the topic "Static headspace method (SHS)"

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Trivedi, Manisha, Elsy Raynil John, Faraat Ali, Anuj Prakash, Robin Kumar, and Gyanendra Nath Singh. "Development and Validation of an Automated Gas Chromatography Method for Determination of Dichloromethane in Ampicillin Sodium by Using Capillary Column Technology." Current Pharmaceutical Analysis 16, no. 7 (August 17, 2020): 901–8. http://dx.doi.org/10.2174/1573412915666190416125604.

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Background: The main aim of the study was to develop an automated static headspace gas chromatography (SHS-GC) method for determination of dichloromethane (DCM) in ampicillin sodium by using a capillary column. Methods: SHS-GC also known as gas chromatography-headspace is the technique of choice due to its high sensitivity, excellent separation abilities, low limit of detection and simplicity of the instrumentation used for the technique. The headspace sampling method has more appropriate sensitivity than the direct injection method because it can clearly separate volatile analytes from the sample matrix and effectively concentrate them. Therefore, this method results in less complex sample preparation, decreased instrument contamination, and increased capillary column life. Results: The developed SHS-GC method showed symmetrical peak shape reasonable retention time for DCM. A linear relationship was obtained over the range of 2-240 μg mL-1 with a correlation coefficient (r2) of 0.993. The recovery, system precision and robustness of the method were within the acceptable values. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were 0.5 μg mL-1 and 2 μg mL-1 respectively. Conclusions: The results obtained in this study demonstrate that SHS-GC method is selective, precise, linear, accurate and robust for determination of dichloromethane in ampicillin sodium and its formulation (injection).
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Najdoska-Bogdanov, Menče, Jane B. Bogdanov, and Marina Stefova. "Changes in Volatile Compounds during Aging of Sweet Fennel Fruits-Comparison of Hydrodistillation and Static Headspace Sampling Methods." Natural Product Communications 11, no. 3 (March 2016): 1934578X1601100. http://dx.doi.org/10.1177/1934578x1601100326.

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Two extraction methods for subsequent gas chromatographic (GC) determination of volatiles from freshly harvested and aged fennel fruit samples ( Foeniculum vulgare Mill.,ssp. vulgare var. dulce) have been compared. Hydrodistillation followed by GC-FID and GC-MS analysis was used as a standard method for essential oil characterization, while static headspace followed by GC (SHS-GC-FID) was used as a comparative method for determination of volatile components. As the fennel fruit ages, there is a gradual loss of the volatile components as indicated by the lower yield of essential oil and lower content of volatiles, as indicated by the alternative SHS-GC-FID analysis. Slight differences observed for the main components ( trans-anethole, estragole, fenchone, and limonene) using the two methods are negligible, indicating that these volatiles did not undergo chemical transformation during the sample preparation procedures. A difference in anisaldehyde content was observed when the composition of the hydrodistilled essential oil was compared with the SHS-GC-FIDanalysis of volatiles and explanation for the variation of anisaldehyde content and the origin of other compounds was suggested. Comparison of the obtained results showed that limonene oxides, carvone and carveolare detectable in SHS-GC-FID analysis of the aged fennel fruits, while in hydrodistilled samples analyzed by GC-FID they were not present. Another observed difference was the appearance of products in significant amounts with higher retention times than trans-anethole, namely threo- and erythro-anethole β-hydroxymethylether and anethole glycol that are not detectable in the essential oil obtained by hydrodistillation. So, the relative abundance of the major components is comparable between these two methods for fennel seed up to 3 years from harvest and they can be used interchangeably depending on the purpose and amount of material. Furthermore, SHS-GC-FID can be used for assessment of maximum storage time and quality of fennel fruit suitable for human consumption.
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Zhang, Wei, and Xianrui Liang. "Headspace Gas Chromatography-Mass Spectrometry for Volatile Components Analysis in Ipomoea Cairica (L.) Sweet Leaves: Natural Deep Eutectic Solvents as Green Extraction and Dilution Matrix." Foods 8, no. 6 (June 11, 2019): 205. http://dx.doi.org/10.3390/foods8060205.

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In this study, natural deep eutectic solvents (NADESs) were used as both the extraction and dilution matrix in static headspace gas chromatography-mass spectrometry (SHS-GC-MS) for the analysis of volatile components in Ipomoea cairica (L). Sweet (ICS) leaves. Six NADESs were prepared and the NADESs composed of choline chloride and glucose with a 1:1 molar ratio containing 15% water were preferred due to the better peak responses. A total of 77 volatiles in ICS leaves were detected and tentatively identified by mass spectral matching with the US National Institute of Standards and Technology (NIST, 2014) Mass Spectral Library and the retention index-assisted qualitative method. These 77 volatile components were mainly terpenoids, aromatics, and aliphatics. Among them, β-elemene, β-caryophyllene, α-humulene, and 2, 4-di-tert-butylphenol were found to be the main components. This investigation verified that the use of NADESs is an efficient green extraction and dilution matrix of the SHS-GC-MS method for direct volatile component analysis of plant materials without extra extraction work.
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Sugaya, Naeko, Mitsuko Takahashi, Katsumi Sakurai, Maiko Tahara, and Tsuyoshi Kawakami. "Headspace GC/MS Analysis of Residual Solvents in Dietary Supplements, Cosmetics, and Household Products Using Ethyl Lactate as a Dissolution Medium." Journal of AOAC INTERNATIONAL 103, no. 2 (March 2020): 407–12. http://dx.doi.org/10.5740/jaoacint.19-0260.

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Abstract Background: The static headspace technique is one of the most popular techniques for residual solvent analysis and dimethyl sulfoxide (DMSO) and N,N-dimethylformamide (DMF) are widely use as the dissolution media. Objective: This study aims to establish ethyl lactate (EL), a solvent with low toxicity and less environmental impact, as an alternative dissolution medium to DMSO and DMF for the static headspace analysis of toxic residual solvents in food, cosmetics, and similar complex organic matrices. Methods: Samples (a sample of dietary supplement and two samples each of cosmetics and household products) spiked with benzene, carbon tetrachloride, 1,2-dichloroethane, 1,1-dichloroethene, and 1,1,1-trichloroethane were dissolved in EL, DMSO, and DMF. Static headspace GC/MS and the standard addition method were used to detect and quantify the residual solvents. Results: The dissolution and dispersion of these samples, especially the ones which were water-insoluble, were better than those in DMSO and DMF. The recoveries, except that of benzene in an aerosol spray, in EL ranged from 77 to 110%. The relative SDs in EL ranged from 2.5 to 11% and were better or equivalent to those in DMSO and DMF. Conclusions: EL was suitable as the dissolution medium for such samples, which may contain large amounts of organic solvents or various ingredients, in static headspace GC/MS analysis of residual solvents.
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Sakac, Marijana, Lato Pezo, Pavle Jovanov, Natasa Nedeljkovic, Anamarija Mandic, Mladenka Pestoric, and Aleksandra Misan. "Application of the SHS-GC-FID method and HPLC-DAD method in the prediction of the shelf-life of gluten-free cookies." Journal of the Serbian Chemical Society 82, no. 12 (2017): 1343–55. http://dx.doi.org/10.2298/jsc170421074s.

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The aim of this study was to compare the sensitivity of two analytical methods for the prediction of the shelf-life of unpacked and packed gluten-free rice?buckwheat cookies kept at ambient (23?1?C) and elevated (40?1?C) temperature during storage, namely the static headspace gas chromatographic method with flame ionisation detection (SHS-GC-FID) for volatile saturated aldehydes (propanal (C3), pentanal (C5), hexanal (C6), heptanal (C7) and octanal (C8)) and the HPLC method for malondialdehyde (MDA) determination. Both methods resulted in obtaining the same end-points of cookie shelf-life, i.e., 3 and 5 months for unpacked and packed cookies kept at elevated temperature, respectively, and 11 and 14 months for unpacked and packed cookies kept at ambient temperature, respectively. Two computational approaches, i.e., the second order polynomial (SOP) and artificial neural network (ANN) models, were used accordingly. The calculations of the contents of aldehydes and MDA could be predicted with an overall coefficient of determination of 0.722 using the ANN model compared to 0.312?0.773 for SOP models. According to sensitivity analysis, it might be suggested that the relevant parameter for the prediction of the end-point of cookie shelf-life is the MDA rather than the C3, C5, C6, C7 and C8 content.
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Bennett, Chonlada, Woraprapa Sriyotai, Sirakorn Wiratchan, Natthawat Semakul, and Sugunya Mahatheeranont. "Determination of 2-Acetyl-1-pyrroline via a Color-Change Reaction Using Chromium Hexacarbonyl." Molecules 27, no. 12 (June 20, 2022): 3957. http://dx.doi.org/10.3390/molecules27123957.

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At present, there is no colorimetric method for the quantitation of the aroma compound 2-acetyl-1-pyrroline (2AP). A novel colorimetric method was developed for the determination of 2AP content using chromium hexacarbonyl (Cr(CO)6) as a reagent. The reaction of synthetic 2AP with chromium hexacarbonyl reagent solution in the presence of light produced a green product with an absorption maximum (λmax) at 623 nm. GC–MS was used to confirm the color-change reaction, which showed the loss of 2AP after the addition of Cr(CO)6. This novel method enables facile and cost-effective determination of 2AP in fragrant rice. A comparative analysis of fragrant and nonfragrant rice grain extracts showed that no color-change reaction occurred with the nonfragrant rice sample. A limit of detection (LOD) of 2.00 mg L−1 was determined by method validation with an effective linear concentration ranging from 5.00 to 60.00 mg L−1 of 2AP. The results obtained using the developed colorimetric method were consistent with those obtained by automated static headspace gas chromatography with nitrogen-phosphorus detection (SHS-GC–NPD).
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Thammarat, Poowadol, Chadin Kulsing, Kanet Wongravee, Natchanun Leepipatpiboon, and Thumnoon Nhujak. "Identification of Volatile Compounds and Selection of Discriminant Markers for Elephant Dung Coffee Using Static Headspace Gas Chromatography—Mass Spectrometry and Chemometrics." Molecules 23, no. 8 (July 31, 2018): 1910. http://dx.doi.org/10.3390/molecules23081910.

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Elephant dung coffee (Black Ivory Coffee) is a unique Thai coffee produced from Arabica coffee cherries consumed by Asian elephants and collected from their feces. In this work, elephant dung coffee and controls were analyzed using static headspace gas chromatography hyphenated with mass spectrometry (SHS GC-MS), and chemometric approaches were applied for multivariate analysis and the selection of marker compounds that are characteristic of the coffee. Seventy-eight volatile compounds belonging to 13 chemical classes were tentatively identified, including six alcohols, five aldehydes, one carboxylic acid, three esters, 17 furans, one furanone, 13 ketones, two oxazoles, four phenolic compounds, 14 pyrazines, one pyridine, eight pyrroles and three sulfur-containing compounds. Moreover, four potential discriminant markers of elephant dung coffee, including 3-methyl-1-butanol, 2-methyl-1-butanol, 2-furfurylfuran and 3-penten-2-one were established. The proposed method may be useful for elephant dung coffee authentication and quality control.
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Carrillo, Jeniffer, and Cristhian Durán. "Fast Identification of Bacteria for Quality Control of Drinking Water through a Static Headspace Sampler Coupled to a Sensory Perception System." Biosensors 9, no. 1 (February 8, 2019): 23. http://dx.doi.org/10.3390/bios9010023.

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The aim of this study was to develop and implement a methodology composed by a Static Head-Space-Sampler (SHS) coupled to a Sensory Perception System (SPS) for the extraction of Volatile Organic Compounds (VOC’s) emitted by bacterial species in the water. The SPS was performed by means of a chamber of 16 Metal-Oxide-Semiconductor (MOS) gas sensors and a software with pattern recognition methods for the detection and identification of bacteria. At first, the tests were conducted from the sterile and polluted water with the Escherichia coli bacteria and modifying the incubation temperatures (50 °C, 70 °C and 90 °C), with the objective to obtain an optimal temperature for the distinguishing of species. Furthermore, the capacity of the methodology to distinguish the important compounds was assessed, in this case, E. coli and other bacteria like Pseudomonas aeruginosa and Klebsiella oxytoca, which formed similar analytes. The validation of the proposed methodology was done by acquiring water samples from different unitary operations of an aqueduct of the municipality of Toledo (North of Santander, Colombia), which were analyzed by the membrane filter technique in the laboratories of the University of Pamplona, along with the SHS-SPS system. The results showed that it was possible to distinguish polluted water samples in a fast way through the sensory measurement equipment using pattern recognition techniques such as Principal Component Analysis (PCA), Discriminant Function Analysis (DFA) and a probabilistic neural network (PNN), where a 95% of differentiation was obtained through PCA and 100% of the classification with DFA. The PNN network achieved the 86.6% of success rate with the cross-validation technique “leave one out”.
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Héthelyi, É., S. Szarka, É. Lemberkovics, and É. Szőke. "SPME-GC/MS identification of aroma compounds in rose flowers." Acta Agronomica Hungarica 58, no. 3 (September 1, 2010): 283–87. http://dx.doi.org/10.1556/aagr.58.2010.3.11.

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The content and composition of active ingredients and essential oils in medicinal and aromatic plants have been studied for several decades. The volatile compounds in essential oils have been analysed routinely using gas chromatography (GC) since 1966, and with GC coupled to mass spectrometric detection (GC/MS) since 1978.The 13 rose varieties selected for chemical analysis varied for colour, shape and fragrance. The static headspace solid phase microextraction (sHS-SPME) technique recently developed for sample preparation and sample enrichment was used to study the volatile aromatic components.The main volatile compound of a sweet-smelling purple rose was found to be phenyl ethyl alcohol (33–52%). The phenyl ethyl alcohol content of fragrant rose flowers with blackish-purple petals increased continuously from early summer to late autumn (from 17 to 70 %). The dominant aromatic components of the yellow, orange and pink rose flowers were hexanol, hexenyl acetate and benzyl alcohol. Phenyl ethyl alcohol and orcinol dimethyl ether were the main constituents of the fragrant pink and white rose varieties. Methyl vinyl anisol and orcinol dimethyl ether were dominant in rose flowers with beige petals. In summary, it can be concluded that the SPME-GC/MS method is suitable for the characterization of rose varieties and for the chemical analysis of aromatic volatile compounds.
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Jacq, Karine, Ed Delaney, Andrew Teasdale, Steve Eyley, Karen Taylor-Worth, Andrew Lipczynski, Van D. Reif, et al. "Development and validation of an automated static headspace gas chromatography–mass spectrometry (SHS-GC–MS) method for monitoring the formation of ethyl methane sulfonate from ethanol and methane sulfonic acid." Journal of Pharmaceutical and Biomedical Analysis 48, no. 5 (December 2008): 1339–44. http://dx.doi.org/10.1016/j.jpba.2008.09.028.

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Dissertations / Theses on the topic "Static headspace method (SHS)"

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Tronson, Deidre A., of Western Sydney Hawkesbury University, of Science Technology and Environment College, and of Science Food and Horticulture School. "Volatile compounds in some eastern Australian Banksia flowers." THESIS_CSTE_SFH_Tronson_D.xml, 2001. http://handle.uws.edu.au:8081/1959.7/140.

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This project was the very beginning of research into the chemistry of eastern Australian banksia flowers. Using dynamic headspace sampling (DHS) analysis, differences in volatile components, consistent with detection of differences in odour, were detected among three different species and one commercial cultivar. Infraspecific variation was also observed between two known subspecies of Banksia ericifolia and between differently coloured forms of Banksia spinulosa var. collina. The cultivar, Banksia 'Giant Candles', was shown to have some of the chemical components of each of its supposed ancestors. The absence of known wound-response chemicals indicated that this DHS method was successful in leaving the inflorescences undamaged throughout the sampling procedure. The Likens-Nickerson modification of classical hydrodistillation methods was useful. The static headspace method (SHS) was easily automated and was shown to be chemically robust and sufficiently sensitive to detect volatile compounds from only a few flowers. The milder DHS method, which minimised mechanical and heat damage to the plant tissue, produced a different set of results. From the results of this project, a suite of volatile compounds has been proposed that may be useful in future behavioural studies to help determine whether animals are attracted to components of banksia odours. These candidates include some compounds that have been reported in animal secretions, wound-response chemicals that may be produced by the plant to aid its communication with other organisms, and a compound (suggested to be sulfanylmethyl acetate) not previously reported from natural sources. The mildest of the three analytical methods used, dynamic headspace sampling, was shown to be suitable for the potential chemotaxonomic evaluation of some members of the Banksia genus.
Doctor of Philosophy (PhD)
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Bock, Emily Maclauren. "Greenhouse Gas Production and Nutrient Reductions in Denitrifying Bioreactors." Thesis, Virginia Tech, 2006. http://hdl.handle.net/10919/64278.

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The global nitrogen cycle has been disrupted by large anthropogenic inputs of reactive nitrogen to the environment. Excess nitrogen underlies environmental problems such as eutrophication, and can negatively affect human health. Managing the natural microbial process of denitrification is advocated as a promising avenue to reduce excess nitrogen, and denitrifying bioreactors (DNBRs) are an emerging technology harnessing this biochemical process. Previous DNBR research has established successful nitrate removal, whereas this study examines the potential to expand DNBR functionality to address excess phosphorus and mitigate the production of nitrous oxide, a potent greenhouse gas. Results from a laboratory experiment supported the hypothesis that the addition of biochar, a charcoal-like soil amendment and novel organic carbon source in DNBR research, would increase nitrate and phosphorus removal as well as decrease the accumulation of nitrous oxide, an intermediate product of microbial denitrification. In order more closely examine the ratio of the products nitrous oxide and inert dinitrogen, development of a novel analytical method to quantify dissolved gases in environmental water samples using gas chromatography mass spectrometry was undertaken. Although static headspace analysis is a common technique for quantifying dissolved volatiles, the variation in sample preparation has recently been revealed to affect the determination of dissolved concentrations of permanent gases and convolute comparison between studies. This work demonstrates the viability of internal calibration with gaseous standard addition to make dissolved gas analysis more robust to variable sample processing and to correct for matrix effects on gas partitioning that may occur in environmental samples.
Master of Science
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Bock, Emily. "Greenhouse Gas Production and Nutrient Reductions in Denitrifying Bioreactors." Thesis, Virginia Tech, 2014. http://hdl.handle.net/10919/64278.

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The global nitrogen cycle has been disrupted by large anthropogenic inputs of reactive nitrogen to the environment. Excess nitrogen underlies environmental problems such as eutrophication, and can negatively affect human health. Managing the natural microbial process of denitrification is advocated as a promising avenue to reduce excess nitrogen, and denitrifying bioreactors (DNBRs) are an emerging technology harnessing this biochemical process. Previous DNBR research has established successful nitrate removal, whereas this study examines the potential to expand DNBR functionality to address excess phosphorus and mitigate the production of nitrous oxide, a potent greenhouse gas. Results from a laboratory experiment supported the hypothesis that the addition of biochar, a charcoal-like soil amendment and novel organic carbon source in DNBR research, would increase nitrate and phosphorus removal as well as decrease the accumulation of nitrous oxide, an intermediate product of microbial denitrification. In order more closely examine the ratio of the products nitrous oxide and inert dinitrogen, development of a novel analytical method to quantify dissolved gases in environmental water samples using gas chromatography mass spectrometry was undertaken. Although static headspace analysis is a common technique for quantifying dissolved volatiles, the variation in sample preparation has recently been revealed to affect the determination of dissolved concentrations of permanent gases and convolute comparison between studies. This work demonstrates the viability of internal calibration with gaseous standard addition to make dissolved gas analysis more robust to variable sample processing and to correct for matrix effects on gas partitioning that may occur in environmental samples.
Master of Science
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Tronson, Deidre A. "Volatile compounds in some eastern Australian Banksia flowers." Thesis, 2001. http://handle.uws.edu.au:8081/1959.7/140.

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This project was the very beginning of research into the chemistry of eastern Australian banksia flowers. Using dynamic headspace sampling (DHS) analysis, differences in volatile components, consistent with detection of differences in odour, were detected among three different species and one commercial cultivar. Infraspecific variation was also observed between two known subspecies of Banksia ericifolia and between differently coloured forms of Banksia spinulosa var. collina. The cultivar, Banksia 'Giant Candles', was shown to have some of the chemical components of each of its supposed ancestors. The absence of known wound-response chemicals indicated that this DHS method was successful in leaving the inflorescences undamaged throughout the sampling procedure. The Likens-Nickerson modification of classical hydrodistillation methods was useful. The static headspace method (SHS) was easily automated and was shown to be chemically robust and sufficiently sensitive to detect volatile compounds from only a few flowers. The milder DHS method, which minimised mechanical and heat damage to the plant tissue, produced a different set of results. From the results of this project, a suite of volatile compounds has been proposed that may be useful in future behavioural studies to help determine whether animals are attracted to components of banksia odours. These candidates include some compounds that have been reported in animal secretions, wound-response chemicals that may be produced by the plant to aid its communication with other organisms, and a compound (suggested to be sulfanylmethyl acetate) not previously reported from natural sources. The mildest of the three analytical methods used, dynamic headspace sampling, was shown to be suitable for the potential chemotaxonomic evaluation of some members of the Banksia genus.
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Klassen, Magnusson Marilyn G. "Identification of volatile odour compounds from controlled spoilage whitefish (Coregonus clupeaformis) using a gas chromatography-olfactometry static headspace method." 2004. http://hdl.handle.net/1993/16265.

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Anacleto, Beatriz Casimiro Soares. "Determination of residual solvents in pharmaceuticals: development of a general analytical method applying Quality by Design." Master's thesis, 2018. http://hdl.handle.net/10773/25630.

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The presence of residual solvents in pharmaceuticals represents one of the main concerns of the pharmaceutical industry due to its impact on both products’ properties and patients’ health. For these reasons, it is necessary to develop analytical strategies that support the decision making process in each stage of the pharmaceutical development and simultaneously maximize the efficiency and productivity of the laboratory responsible for pharmaceutical quality control. In this thesis, a general Static Headspace-Gas Chromatography method was developed applying the Analytical Quality by Design (AQbD) approach for determination of residual solvents in Hovione FarmaCiencia SA. The column flow, oven temperature program, split ratio, split at vent, vial pressure and headspace equilibration temperature and time were identified as critical method parameters. In order to optimize the selectivity, sensibility and run time, these parameters were studied through experimental design plans and statistical analysis. From the obtained design space, the final operating conditions of the method were selected. The robustness of the method was verified and confirmed. The validation results demonstrated specificity, selectivity, sensitivity, linearity, accuracy and precision, so the developed method is suitable for the determination of 29 different residual solvents in pharmaceutical samples. The application of the AQbD approach allowed to acquire the maximum understanding about the method and to minimize the impact of the sources of variability in its performance.
A presença de solventes residuais em produtos farmacêuticos representa uma das principais preocupações da indústria farmacêutica, devido ao seu impacto nas propriedades dos produtos e na saúde dos pacientes. Por estes motivos, torna-se necessário desenvolver estratégias analíticas que suportem decisões em cada fase do desenvolvimento farmacêutico e simultaneamente maximizem a eficiência e produtividade do laboratório de controlo de qualidade farmacêutico. Nesta tese foi desenvolvido um método geral de Cromatografia Gasosa com amostragem por Headspace estático aplicando a abordagem Qualidade Analítica por Design (AQbD), para a determinação de solventes residuais na Hovione FarmaCiencia SA. O fluxo da coluna, o programa de temperatura do forno, o split ratio, o split at vent, a pressão do vial e a temperatura e o tempo de equilíbrio do headspace foram identificados como parâmetros críticos do método. De forma a otimizar a seletividade, a sensibilidade e o tempo de análise, estes parâmetros foram estudados através de planos de desenho experimental e de análises estatísticas. A partir do espaço de design obtido, foram selecionadas as condições operatórias finais do método. A robustez do método foi verificada e confirmada. Os resultados de validação demonstraram especificidade, seletividade, sensibilidade, linearidade, exatidão e precisão, pelo que o método desenvolvido é adequado à determinação de 29 solventes residuais diferentes em amostras farmacêuticas. A aplicação da abordagem AQbD permitiu adquirir o máximo conhecimento acerca do método e minimizar o impacto das fontes de variabilidade na sua performance.
Mestrado em Bioquímica
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Book chapters on the topic "Static headspace method (SHS)"

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"We present here applications of the nanoscale metal particles for transformation of carbon tetrachloride (CT). CT is one of the most prevalent contaminants in soils and aquifers. It has been listed as priority pollutants by the U.S. Environmental Protection Agency, and also appeared on the Superfund National Priority List. There is an urgent need to develop effective control and treatment methods. The purpose of this study was aimed to measure the rate and extent of dechlorination, characterize and quantify reaction intermediates and final products. EXPERIMENTAL METHODS Synthesis of nanoscale iron particles. Nanoscale iron particles were synthesized by adding 1:1 volume ratio of FeCI3*6H20 (0.045M) into NaBH4 (0.25M) solution and mixed vigorously under room temperature (22±1 °С) for a few minutes. Ferric iron (Fe3+) was reduced to zero-valent iron (Fe°) by borohydride, a strong reductant. Metal particles from this reaction have sized mostly in the range between 1 to 100 nanometers [1,2]. BET analysis gave a specific surface area of 35 m2/g. Batch experiments. Batch experiments were conducted with 50 mL serum bottles. In each batch bottle, 20 mL deionized water was mixed with 0.25 g of the nanoscale metal particles. Then, 10 pL stock solution of CT dissolved in methanol was spiked into the solution. Initial organic concentration was about 0.1 mM. The serum bottles were capped with Teflon Mininert valves and mixed on a rotary shaker (30 rpm) at room temperature (22±1°C). Parallel experiments were also performed without the metal particles (control) and with a commercial grade iron (Aldrich, 99%, <10 pm, BET surface area 0.9m2/g ). Methods of Analyses. Organic concentrations were measured by the static headspace gas chromatograph (GC) method. At selected time intervals, 20 pL headspace aliquot was withdrawn from the batch bottle for GC analyses. Concentrations of chlorinated methanes were measured using a HP5890 GC equipped with a DB-624 capillary column (30mx0.32mm) and an electron capture detector (ECD). The detection limit of this method was less than 5 pg/L. Hydrocarbon products in the headspace were qualitatively identified with a Shimadzu QP5000 GC-MS and further quantified with GC analysis by comparing retention times and peak areas with standard gas samples (ethane, ethylene, acetylene, methane and carbon dioxide)." In Hazardous and Industrial Waste Proceedings, 30th Mid-Atlantic Conference, 70. CRC Press, 2014. http://dx.doi.org/10.1201/9781498709453-25.

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Conference papers on the topic "Static headspace method (SHS)"

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McCutcheon, Jeff W. "Ultra-Pure Viscoelastic Damping Polymers and Associated Low Outgassing Materials." In ASME 2000 International Mechanical Engineering Congress and Exposition. American Society of Mechanical Engineers, 2000. http://dx.doi.org/10.1115/imece2000-1636.

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Abstract The key to successful multifunctional materials applications for vibration, shock and acoustic control is often the proper selection of materials, geometric design and optimum application. Much work has been done in the areas of geometric designs and optimum application of the multi-functional materials. The next step is improvements in the passive damping materials themselves. The improvement in the passive materials in the past has often focused on the areas of improved damping performance (loss factor, storage modulus), material performance (acrylics, silicones, etc.) and enhanced features (thermally conductive, electrically conductive, etc). One of the newest requirements for passive damping polymers is in the area of ultra-pure viscoelastic damping polymers. This new generation of materials is finding growing use because the sensitive environment where the passive material is used require a material that will not negatively impact the components in that environment. This new generation of passive materials needs to be ultra-pure with respect to organic material outgassing, anions, catalysts and siloxanes. In addition to the viscoelastic damping polymer requirements for high purity, the associated polymeric materials (epoxies, laminating adhesives and tapes) used in the same environment must also be of a similar low outgassing, ultra-pure, ultra-clean, electronics grade or clean room performance designation. If this is not done, the environment could become contaminated and negate a portion of the benefit of using the clean damping material. This also requires an understanding of the test method used to determine each product’s cleanliness performance, as all test methods are not equal and can give significantly different test results. An example is comparing a polymer sample tested for organic outgassing and using a static headspace gas chromatography/mass spectroscopy (GC/MS) and a dynamic headspace GC/MS.
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