Dissertations / Theses on the topic 'Extraction en phase solide – Purification'
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Bartuma, Ninorta. "Optimizing purification of oligonucleotides with reversed phase trityl-on solid phase extraction." Thesis, Örebro universitet, Institutionen för naturvetenskap och teknik, 2019. http://urn.kb.se/resolve?urn=urn:nbn:se:oru:diva-76844.
Maury, Delphine. "Méthodes de purification des signaux impliqués dans la mise en place de la symbiose endomycorhizienne." Toulouse 3, 2007. http://www.theses.fr/2007TOU30241.
EThe research tasks undertaken in this thesis lie within the scope of “durable development” and more especially in the agronomic sector. Indeed, one of the possible methods to decrease the excessive contributions of manures, often harmful with the environment, is to support the installation of the plant-microorganism natural interactions. Among them, the endosymbioses including nitrogen fixing and mycorhizal appear. The molecular dialogue between the two partners highlights the presence of a symbiotic signal in the case of the nitrogen fixing symbiosis, called nod factor, which is not other than a lipochito-oligomer. By considering a similarity in the signalising of the two symbioses, it is possible to imagine the existence of a “myc” factor with structure closed to the factor nod one. Nevertheless, the corresponding structure of “myc” factor still remains unspecified. The objective of this thesis is to seek these myc factors to even purify them and in fine, to isolate them. Work was completed according to three approaches. One the basis of an a priori of structure with the nod factor, the molecular imprinting technique was used around a lipochito-oligomer. Then a protocol of labelling with the 2-aminobenzamide was developed. Last, without an a priori of structure, a series of extractions of biological media according to a more traditional biochemical approach was carried out and the activity of the residual fractions was tested directly on the plants. The results from these various approaches made it possible to purify fractions containing compounds of “fungic” origin and to open the way to promising prospects
Simmons, Steven Tyler. "Commercial Applicability of an Innovative Anthocyanin Purification Technique, Utilizing Mixed-Mode Solid-Phase Extraction." The Ohio State University, 2012. http://rave.ohiolink.edu/etdc/view?acc_num=osu1332267706.
Sahyoun, Wissam. "Analyse de pesticides dans les fruits et légumes : développement analytique et application de méthode QuEChERS, d-SPE et GC-MS/MS." Electronic Thesis or Diss., Université de Lille (2022-....), 2022. http://www.theses.fr/2022ULILR082.
Due to the widespread use of pesticides, a fraction of pesticide residues are present in fruits and vegetables. Pesticide contamination of food has become one of the serious problems. Global pesticide consumption has increased over the past decade due to continued population growth and rapid urbanization. Pesticides are highly toxic and long-term exposure to these chemicals causes health risks including neurological and respiratory diseases.This study focuses on the evaluation of the concentration of 34 pesticides in 60 conventionally and organically grown vegetables and fruits from various origins. Among these samples, some were studied in different forms, with and without washing, with and without skin. The purpose of the latter is to evaluate whether there is a simple gesture to reduce the content of pesticides in fruits and vegetables and thus reduce the health impacts of consumers.The work focuses firstly on the optimization of the extraction method, purification and final analysis of the extracts. The extraction method QuEChERS (Quick, Easy, Cheap, Rugged, Effective and Safe) and the purification method d-SPE (dispersive Solid Phase Extraction) were used. The final extracts were analyzed by gas chromatography coupled to a tandem mass spectrometer (GC-MS/MS) for the identification and quantification of each pesticide. The set of procedures has been optimized and it provides good sensitivity, selectivity, good yield that varies from 70% to 120%, and good precision with RSD <20%. The application of the method on real samples allows the determination of pesticides in 85% of the samples. The concentrations of pesticides detected in vegetables and fruits did not exceed the maximum residue limits (MRLs) for the majority of pesticides. However, some pesticides were found at levels above MRLs for fruits and vegetables from Akkar in Northern Lebanon. Moreover, among the pesticides detected at high levels are those that have already been banned as in the case of Endosulfan. The results showed that some simple gestures can reduce the levels of pesticide residues in fruits and vegetables. Indeed, washing with tap water and peeling significantly reduce pesticide residues in fruits and vegetables. Organically grown fruits and vegetables have lower pesticide concentrations than conventionally grown ones. Very low pesticide concentrations or in some cases concentrations below the limit of quantification were determined for organically grown fruits and vegetables
He, Jian. "Isolation of Anthocyanin Mixtures from Fruits and Vegetables and Evaluation of Their Stability, Availability and Biotransformation in The Gastrointestinal Tract." The Ohio State University, 2008. http://rave.ohiolink.edu/etdc/view?acc_num=osu1222108733.
Leong, Yoong Kit. "Extraction and purification of green polymers using aqueous two-phase extraction (ATPE)." Thesis, University of Nottingham, 2018. http://eprints.nottingham.ac.uk/48807/.
Jajuli, Maizatul Najwa. "Extraction liquid-liquide modulée électrochimiquement et microextraction en phase solide de composés pharmaceutiques sélectionnés." Electronic Thesis or Diss., Université de Lorraine, 2019. http://www.theses.fr/2019LORR0127.
Conventional sample preparation methods for the determination of polar compounds such as liquid-liquid extraction (LLE) and solid phase extraction (SPE) are generally not effective because of their multiple steps, low recovery and high consumption of organic solvents. Thus, this thesis deals with the development of new sample preparation methods, i.e, electrochemically modulated liquid-liquid extraction (EMLLE) and bar-micro solid phase extraction (bar-μ-SPE) to determine selected pharmaceutical compounds, i.e., metformin (MET), buformin (BUF), phenformin (PHEN), and propranolol (PROP) having varied lipophilicity in biological samples. In the EMLLE method, the aid of electric field was utilized to extract the pharmaceutical compounds across the interface between two immiscible electrolyte solutions (ITIES). ITIES formed when two bulk solvents aqueous phase (lithium chloride) and organic phase (I,2-dichloroethane), both containing electrolytes are brought into contact. Transfer potential for each analyte was analysed by voltammetry. The trend of transfer potential followed their lipophilicity; propranolol < phenformin < phenyl biguanide < metformin. Extraction of the analytes was performed by applying fixed potential to the biphasic system using potentiostat for 15 mins. The extraction performance was poor. Design of another ITIES cell and imposing interfacial potential by chemical polarization was done to enhance the extraction performance of this method. Thus, the EMLLE technique based on application of interfacial potential due to the presence of different concentrations of tetramethylammonium ion (TMA+) as common ion in each phase was studied. The optimum extraction conditions for this method are, [TMA+]o = 10 mM, [TMA+]w = 0.001 mM, Vorg = 2 mL, pHsample = 9, rotation speed = 900 rpm, extraction time = 600 s. The optimised parameters for back-extraction are: [TMA+]back = 50 mM, Vfinal = 0.1 mL, pHback = 2 . Nearly 100 % extraction of targeted analytes was achieved, and the enrichment factor obtained was up to ~ 60 for biguanide compounds. In the bar-μ -SPE method, adsorbent and a tiny metal rod was placed in a polypropylene membrane bag. Among the various adsorbents studied, graphene and zeolite showed some potential. Thus, extraction conditions were optimised for each adsorbent and adsorbent mixture. Despite the optimisations, the extraction was low (5.03-39.2 %). Nevertheless, enrichment factors of 1.49 -14.9 were obtained. Both proposed methods were applied to the determination of the analytes in urine. On the whole, the newly proposed methods are simple and markedly reduced consumption of organic solvents
Balasubramaniam, Deepa. "Lysozyme Separation from Tobacco Extract by Aqueous Two-Phase Extraction." Thesis, Virginia Tech, 2003. http://hdl.handle.net/10919/31272.
Master of Science
Samatou, Joachim [Verfasser]. "Modelling and Simulation of Antibody Purification by Aqueous Two-Phase Extraction / Joachim Samatou." München : Verlag Dr. Hut, 2013. http://d-nb.info/1035049988/34.
Holste, Angela Sarah. "Développement des méthodes bio analytique pour l’analyse quantitative et qualitative des peptides et protéines marqués par le couplage de la chromatographie et la spectrométrie de masse." Thesis, Pau, 2014. http://www.theses.fr/2014PAUU3004/document.
This PhD thesis was a Cotutelle between the Université de Pau et des Pays de l’Adour (UPPA) in Pau, France and the Christian-Albrechts University (CAU) in Kiel, Germany. In the course of this international collaboration, bio-analytical methods for the quantitative and qualitative analysis of labelled peptides and proteins were developed, which were based on the hyphenation of chromatography with mass spectrometry. Peptides and protein digests were lanthanide labelled using DOTA-based compounds according to an optimised protocol. Separation on the peptide level was performed using IP-RP-nanoHPLC. Complementary data sets were acquired using MALDI-MS for identification and ICP-MS for quantification. In this context, an online precleaning step was developed and implemented in the nanoHPLC separation routine, which allowed for effective removal of excess reagents. This lead to lowered metal backgrounds during ICP-MS measurements and thus better data interpretability, while guarding peptide recovery at a maximum level. An alternative offline purification using solid phase extraction (SPE) resulted in important peptide losses and can be considered unsuitable for quantitative analysis. Additives to the nanoHPLC eluents, such as HFBA and EDTA were tested and not deemed beneficial for the analysis of normal peptide samples. HFBA can be reconsidered for special application on very hydrophilic peptide species. A set of labelled peptides was developed, which due to application of known quantities could be employed for quick and simple quantification of a low complexity digest sample. In addition this peptide set allowed for the reliable superposition of chromatograms, enabling sample comparability especially for complementary ICP-MS and MALDI-MS data. Experiments for application of fsLA-ICP-MS on MALDI-MS target plates were conducted and showed very promising results. For this purpose, samples that were already identified using MALDI-MS were supposed to be remeasured using fsLA-ICP-MS. First quantification attempts on the modified steel target plate were successful and in the range of expectance. Adjusted parameters for MALDI-MS allowed for proper peptide identifications
Guéhenneux, Gaëlle. "Etude des composés organiques semi-volatils en milieux extrêmes par micro-extraction en phase solide." Université Joseph Fourier (Grenoble), 2003. http://www.theses.fr/2003GRE10161.
Mündges, Jan [Verfasser]. "Investigation and Intensification of Monoclonal Antibody Purification by Aqueous Two-Phase Extraction / Jan Mündges." München : Verlag Dr. Hut, 2015. http://d-nb.info/107976805X/34.
Moussa, Manel. "Développement de polymères à empreintes ioniques pour l'extraction sélective des lanthanides dans des échantillons environnementaux." Thesis, Paris 6, 2016. http://www.theses.fr/2016PA066585/document.
The analysis of the lanthanide ions present at trace level in complex environmental matrices requires often a purification and preconcentration step. The solid phase extraction (SPE) is the most used sample preparation technique. To improve the selectivity of this step, Ion Imprinted Polymers (IIPs) can be used as SPE solid supports. The aim of this work was the development of IIPs for the selective extraction of lanthanide ions from environmental samples. In a first part, IIPs were prepared according to the trapping approach using 5,7-dichloroquinoline-8-ol as non-vinylated ligand. For the first time, the loss of the trapped ligand during template ion removal and sedimentation steps was demonstrated by HPLC-UV. Moreover, this loss was not repeatable, which led to a lack of repeatability of the SPE profiles. It was then demonstrated that the trapping approach is not appropriate for the IIPs synthesis.In a second part, IIPs were synthesized by chemical immobilization of methacrylic acid as vinylated monomer. The repeatability of the synthesis and the SPE protocol were confirmed. A good selectivity of the IIPs for all the lanthanide ions was obtained. IIPs were successfully used to selectively extract lanthanide ions from tap and river water. Finally, IIPs were synthesized by chemical immobilization of methacrylic acid and 4-vinylpyridine as functional monomers and either a light (Nd3+) or a heavy (Er3+) lanthanide ion as template. Both kinds of IIPs led to a similar selectivity for all lanthanide ions. Nevertheless, this selectivity can be modified by changing the nature and the pH of the washing solution used in the SPE protocol
Gaillard, Yvan. "Analyse des xénobiotiques après extraction en phase solide en pharmaco-toxicologie : applications cliniques, médico-légales et sportives." Lyon 1, 1999. http://www.theses.fr/1999LYO1T122.
Ross, Kristin Coby. "Separation of Recombinant β-Glucuronidase from Transgenic Tobacco by Aqueous Two-Phase Extraction." Thesis, Virginia Tech, 2008. http://hdl.handle.net/10919/43471.
Master of Science
Nait-Si, Youssef. "Extraction, purification, comportement chimique de l'hypéricine et de la pseudohypéricine du millepertuis (hypericum perforatum)." Aix-Marseille 3, 2002. http://www.theses.fr/2002AIX30073.
St. -John's-wort (Hypericum perferatum) is a medical plant with multiple activities which contains two characteristic compounds, hypericin and the pseudohypericin, in wich one attributed some of these activities. This work had for object the settling of processes allowing to obtain the two naphthdianthrons at an high degree of purity. Firstly a criterion of purity of the two compound was elaborated. Subsequently, protocols for extracting the plant and purifying extracts were finalized for obtaining an extract enriched in hypericin and pseudohypericin. The compounds are then separated by two successive chromatographies using silica gel and silica gel C-18 reversed phase and obtained pure up to 95 % by precipitation. The study of their behavior showed that the hypericin is stable in hydrated medium while the pseudohypericin is transformed into isopseudohypericin, a new naphthodianthron. We shown an equilibrum between pseudo and isopseudohypericin in neutral hydrated medium and the a full deplacement of the equilibrum to isopseudohypericin in weakly alkaline medium and to pseudohypericin in weakly acid one
Larroque, Virginie. "Développement d'une méthode de micro-extraction sur phase solide pour l'analyse de composés organiques volatils dans l'air intérieur." Pau, 2006. http://www.theses.fr/2006PAUU3038.
Indoor air quality is a recent concern and to improve the knowledge in this field, analytical methods are required for pollution characterisation. In this aim, SPME was studied as alternative to traditional sampling methods for the analysis of VOCs in indoor air. Despite its numerous advantages, SPME shows some limits for quantitative analysis. Therefore, an equilibrium sampling method was developed to overcome competitive adsorption. Operating conditions involves PDMS/Car fibre and static extraction in a fixed sample volume. Adsorption kinetics of model compounds were determined for 3 volumes in order to find the best compromise between extraction time and performance. 250 mL and 3h extraction were retained. Limits of detection in the sub -µg. M-3 order are reached in GC/MS and quantitative analysis is possible up to 9 µmol. M-3, even with 70% RH air humidity. For a better understanding of sampling mechanisms, a theoretical approach, based on diffusion modelling, was studied. Then, the method developed was compared to non-equilibrium methods involving short extraction times. Best results were obtained for the equilibrium method: linearity domains are larger and limits of detection are at least twice lower. Fibre storage was studied to avoid both contamination and losses before and after sampling. The methodology was then successfully applied to the analysis of VOCs in classrooms of two nursery schools built according to two different rules of building (traditional and HEQ). The effect of floor cleaning on VOCs content in air was also shown
Boussetta, Sabrina. "Greffage de résine et membrane polymères par des agents chelatants : application à l'extraction en phase solide de cations métalliques." Toulon, 2004. http://www.theses.fr/2004TOUL0009.
With the view to know sizing impact on interphase nature and properties of a cyanate/D glass fibre composite, four types of samples were achieved : a series of three composites, processed by vacuum moulding and which differ by absence or presence of sizing (with or partially extracted), and resin samples. The dynamic mechanical analysis was selected to study these composites. Mechanical relaxations, particularly main relaxation associated to resin Tg, are largely modified by the state of the interphase. A elaborate study of this transition enables us to express assumptions on the formation and the nature of the interphase for this system. These results are corroborated by complementary analysis (infra-red microscopy, micro thermal analysis. . . ). Lastly, ageings were realized on the composites and the resin in order to characterize this interphase more finely
Gignac, Fanny. "Développement de supports solides fonctionnalisés par des aptamères pour l’analyse d’ions présents à l’état de trace dans des échantillons complexes." Electronic Thesis or Diss., Sorbonne université, 2023. https://accesdistant.sorbonne-universite.fr/login?url=https://theses-intra.sorbonne-universite.fr/2023SORUS522.pdf.
Many metal ions are recognized as essential for the proper functioning of our organism, but some of them, such as cadmium or lead ions, are harmful even in trace amounts. Other ions, like copper ions, can also become harmful when a deficiency or excess is observed in the body. Standards and normal thresholds have been established, particularly in food products, as well as in biological matrices such as blood. Therefore, it is necessary to be able to quantify these trace metals in complex matrices. In order to overcome the performance limitations of elemental analysis instruments, such as lack of specificity or sensitivity to matrix effects, a preliminary sample treatment step is required, such as solid-phase extraction. However, conventional supports lack specificity, leading to the co-extraction of multiple metal ions. To overcome this lack of specificity, new highly specific supports are being developed, such as ion-imprinted polymers whose potential has already been demonstrated, but whose synthesis and implementation can be complex. The objective of this thesis is to investigate the use of aptamers, simple DNA or RNA strands, to develop highly specific and selective extraction supports for metal ions. While their potential has already been demonstrated for the extraction of organic molecules, few studies have focused on the extraction of metal ions such as cadmium, lead, and copper, which are targeted in this study. Following a literature review on the use of specific aptamers for these metal ions, especially in the context of sensor development, specific sequences of interest were selected for each target. These sequences were covalently attached to activated CNBr Sepharose. After evaluating the theoretical capacity of the supports by measuring the grafting rates, a detailed study of the effect of percolation and washing media on the retention of targeted ions was conducted thanks to ICP-MS measurement of each fraction, demonstrating the strong influence of ions present in the medium on specificity and selectivity. These two parameters were investigated respectively by studying the retention of other divalent cations on sorbent grafted with specific aptamers and by studying the retention of targeted ions on supports grafted with so-called control sequences, i.e. with no known affinity for targeted ions. After optimizing the procedures for each of the most promising supports capable of extracting one of the target ions, the capacities of the supports were determined. Then, the supports were successfully applied to the extraction of targeted ions from real samples such as serum, illustrating the strong potential of aptamers for the extraction of metal ions
Urdaneta, Zurbarán Erika Cristina. "Purification of UV cross-linked RNA-protein complexes by phenol-toluol extraction." Doctoral thesis, Humboldt-Universität zu Berlin, 2020. http://dx.doi.org/10.18452/21318.
RNA binding proteins play key functions in post-transcriptional regulation of gene expression. By binding to RNA, they control RNA editing, transport, stability and translation. In the last decade, significant advances have been made in the elucidation of bacterial post-transcriptional mechanisms. It is becoming increasingly clear that this layer of regulation also plays an important role in pathogenesis and antibiotic resistance. The analysis of RNA-protein complexes (RNPs) at the proteome level has been driven by the (m)RNA interactome capture technology which isolates the proteome cross-linked to poly-adenylated (m)RNA. This has resulted in the identification of hundreds of novel RBPs in a diversity of eukaryotic species ranging from humans to yeast. However, poly-adenylation is absent in functional RNA from bacteria and other classes of -eukaryotic- regulatory RNAs. This work was aimed to overcome that limitation by developing a novel and unbiased method for the purification of UV-cross-linked RNPs in living cells: PTex (Phenol Toluol extraction). The purification principle is solely based on physicochemical properties of cross-linked RNPs versus unbound proteins or RNA, and it is impartial towards specific RNA or proteins; enabling for the first time a system-wide analysis of non-poly(A) RNA interacting proteins in both eukaryotic (HEK293) and prokaryotic (Salmonella Typhimurium) cells.
Costa, Sara Henriques da Silva e. "Development of aqueous micellar two-phase systems for the selective extraction and purification of IgG from real matrixes." Master's thesis, Universidade de Aveiro, 2016. http://hdl.handle.net/10773/21244.
Os anticorpos, mono e policlonais, têm sido alvo de estudo intenso pelas indústrias farmacêuticas e biotecnológicas, resultando num extraordinário crescimento do mercado de produção de anticorpos. Este crescente interesse deve-se principalmente às vantagens que estas biomoléculas compreendem, tais como a sua aplicação terapêutica e a sua incorporação numa vasta variedade de técnicas de quantificação. A imunoglobulina G (IgG) é um dos anticorpos já aprovados pela Food and Drug Administration (FDA) que oferece uma grande variedade de aplicações em diversas áreas e, portanto, reconhecida como uma proteína de valor acrescentado. Apesar da vasta oferta de técnicas de purificação de anticorpos, ainda existem grandes desvantagens associadas à sua purificação. As técnicas atualmente utilizadas centram-se em técnicas cromatográficas, as quais envolvem materiais dispendiosos e longos períodos de operação, sendo responsáveis por 50-80% dos custos totais do produto. Copulativamente, estas técnicas apresentam grandes limitações relativamente à escalabilidade do processo. Como alternativa, este trabalho foca-se na aplicação de sistemas micelares de duas fases aquosas convencionais e mistos, utilizando líquidos iónicos com carácter tensioativo, como uma técnica de purificação não cromatográfica para a extração e purificação de IgG a partir de soro de coelho. Foram otimizados alguns parâmetros associados ao processo de purificação, tais como a concentração de surfactante, a presença/ ausência de líquidos iónicos como co-surfactantes, o efeito da sua concentração e as suas características estruturais. Após o estudo de otimização, os sistemas convencionais foram confinados a uma percentagem de 10% de Triton X-114 a pH 7, alcançando purezas de IgG de 24,6%. Com a aplicação de sistemas micelares mistos de duas fases aquosas compostos por líquidos iónicos obtiveram-se ainda melhores fatores de purificação. Os sistemas que conduziram a melhores purezas foram os sistemas com adição de [C16mim]Cl a 0,7 wt%, [P4,4,4,14]Cl a 1,0 wt% e [P6,6,6,14]Br a 0,7wt%, obtendo-se purezas de IgG de 26,3%, 28,1% e 29,2%, respectivamente. Estes resultados de pureza são superiores aos reportados na literatura relativamente à purificação de IgG a partir do soro do coelho utilizando sistemas de duas fases aquosas, confirmando o potencial desta técnica na extração e purificação de anticorpos ou outros produtos de valor acrescentado de matrizes complexas.
Os anticorpos, mono e policlonais, têm sido alvo de estudo intenso pelas indústrias farmacêuticas e biotecnológicas, resultando num extraordinário crescimento do mercado de produção de anticorpos. Este crescente interesse deve-se principalmente às vantagens que estas biomoléculas compreendem, tais como a sua aplicação terapêutica e a sua incorporação numa vasta variedade de técnicas de quantificação. A imunoglobulina G (IgG) é um dos anticorpos já aprovados pela Food and Drug Administration (FDA) que oferece uma grande variedade de aplicações em diversas áreas e, portanto, reconhecida como uma proteína de valor acrescentado. Apesar da vasta oferta de técnicas de purificação de anticorpos, ainda existem grandes desvantagens associadas à sua purificação. As técnicas atualmente utilizadas centram-se em técnicas cromatográficas, as quais envolvem materiais dispendiosos e longos períodos de operação, sendo responsáveis por 50-80% dos custos totais do produto. Copulativamente, estas técnicas apresentam grandes limitações relativamente à escalabilidade do processo. Como alternativa, este trabalho foca-se na aplicação de sistemas micelares de duas fases aquosas convencionais e mistos, utilizando líquidos iónicos com carácter tensioativo, como uma técnica de purificação não cromatográfica para a extração e purificação de IgG a partir de soro de coelho. Foram otimizados alguns parâmetros associados ao processo de purificação, tais como a concentração de surfactante, a presença/ ausência de líquidos iónicos como co-surfactantes, o efeito da sua concentração e as suas características estruturais. Após o estudo de otimização, os sistemas convencionais foram confinados a uma percentagem de 10% de Triton X-114 a pH 7, alcançando purezas de IgG de 24,6%. Com a aplicação de sistemas micelares mistos de duas fases aquosas compostos por líquidos iónicos obtiveram-se ainda melhores fatores de purificação. Os sistemas que conduziram a melhores purezas foram os sistemas com adição de [C16mim]Cl a 0,7 wt%, [P4,4,4,14]Cl a 1,0 wt% e [P6,6,6,14]Br a 0,7wt%, obtendo-se purezas de IgG de 26,3%, 28,1% e 29,2%, respectivamente. Estes resultados de pureza são superiores aos reportados na literatura relativamente à purificação de IgG a partir do soro do coelho utilizando sistemas de duas fases aquosas, confirmando o potencial desta técnica na extração e purificação de anticorpos ou outros produtos de valor acrescentado de matrizes complexas.
Duran, Renan Ravetti. "Procédés d’extraction et de purification de molécules à haute valeur ajoutée issues de la biomasse bois." Thesis, Université de Lorraine, 2015. http://www.theses.fr/2015LORR0325.
By-products from wood industry, particularly knots, contain different types of molecules that can be valued as a source of bioactive components meeting therapeutic needs. It is on this idea that the project "Le Bois Santé" was designed. Through the collaboration of several partnerships, the present work aims initially to develop a "green" extraction processes (solid-liquid and supercritical) to obtain an extract rich in lignans from a mixture of norway spruce and silver fir knots. The effects of operating conditions on the extraction yield of each target compound and the antioxidant activity of the extracts were determined. To understand the entire process, the project aims to investigate the impact of concentration and drying processes using vacuum evaporation and lyophilisation. Moreover, the separation and purification of the compounds have been developed and optimized using frontal chromatography technique
Belghith, Hafedh. "Production et extraction-purification d'une alcool oxydase : réalisation et développement d'un capteur à alcools." Compiègne, 1985. http://www.theses.fr/1985COMPI211.
Bakaï, Marie-France. "Développement d’un procédé de réduction des sulfites dans les vins." Thesis, Bordeaux, 2015. http://www.theses.fr/2015BORD0374/document.
SO2 is an additive used in enology for its antiseptic, antioxidant and antioxydasic properties. It is introduced in wines in large quantities due to its high binding power with carbonyl compounds, which limits its activity. The maximum SO2 content authorized is notalways enough to avoid fermentative phenomena during wine storage. The main objective of this project was to develop a method to reduce the sulfur dioxide concentration in wines byeliminating some of carbonyl compounds responsible for the SO2 binding. The method used was solid-phase extraction (SPE). It involves interactions between a liquid and a porous solid support modified with an extractive function. Previous work allowed to select hydrazine andsulfonylhydrazine as extractive reagents. These functions were fixed on organic polymersupports according to two routes : functionnalization of commercial sulfonic resins and suspension copolymerization of glycidyl methacrylate (followed by the functionnalization). The solid supports obtained were characterized in order to validate the functionnalization.Then selective extractions were executed on model solutions. The diminution of carbonylcompounds concentration and SO2 content was showed by those experiments. The presence of contaminants in the solutions was investigated before applying the method to wine
Lardon, François. "Synthèse et caractérisation de mésophases silice/tensioactif/ligand pour l'extraction solide-liquide des cations métalliques en phase aqueuse : Application à l'Américium (III) et à l'Europium (III)." Université Louis Pasteur (Strasbourg) (1971-2008), 2006. http://www.theses.fr/2006STR13183.
This work deals with the reprocessing of spent nuclear fuels by solid-liquid extraction. We study in particular the use of micelle-templated mesostructured materials as a silica-based adsorbent. The key idea is to take advantage of the lipophilic properties of the immobilized surfactant to introduce inside a silica framework ligand-molecules which have affinity for actinides. The design and synthesis of such new functionalized materials and extraction experiments on aqueous solutions of americium(III) and europium(III), two elements of the spent nuclear fuel, have been done. X-ray diffraction, transmission electronic microscopy and nuclear magnetic resonance experiments have been realized. From the information obtained, a model of molecular organization, in connection with the extraction properties, is proposed
Brothier, Fabien. "Développement d'outils bioanalytiques miniaturisés : greffage de biomolécules sur monolithes en capillaire couplés à la nanochromatographie pour l'analyse d'échantillons complexes." Thesis, Paris 6, 2014. http://www.theses.fr/2014PA066299/document.
The analysis of ultra-traces from complex matrices (environmental, foodstuff or biological) often requires a step of purification and preconcentration before their analysis by chromatographic separation methods. Therefore, extraction sorbents based on a molecular recognition mechanism can be developed and used for the selective extraction of target molecules thus rendering their quantitative analysis in complex samples more reliable and sensitive. These extraction sorbents may result, among others, from the immobilization of biomolecules such as antibodies and aptamers (i.e. oligonucleotides whose sequence is specific for a target molecule). This selective sample pretreatment step is particularly necessary when developing miniaturized devices such as separative microsystems on chip because of the decrease of the resolution that results from the use of a shorter length separation channel. In this context, the aim of our study was to develop miniaturized bioanalytical devices for the analysis of small molecules or proteins in complex samples. For the development of these devices, in-situ synthesis of a porous hybrid organic-inorganic monolith in capillaries (100 µm i.d.) by sol-gel approach was firstly optimized and characterized in terms of repeatability. Secondly, two model toxins of low molecular weight were chosen: microcystin-LR (MC-LR) and ochratoxin A (OTA). Monoclonal antibodies and aptamers specific to one and the other target molecules were then grafted on the monolithic capillaries. The resulting miniaturized immunosorbent (mIS) and oligosorbent (mOS) were then coupled on-line to nanoLC. Specific retention of MC-LR and OTA on the mIS and the mOS, respectively, was demonstrated in pure water. Synthesis repeatability and capacity of the miniaturized sorbents were evaluated. Finally, these miniaturized tools were applied to the selective extraction of MC-LR or OTA from complex samples, i.e. blue-green algae extracts, environmental waters or beer. In a third part, immobilized enzyme reactors (IMERs) were prepared by grafting two proteolytic enzymes (pepsin and trypsin) on monoliths in order to transpose the developed selective tools to the analysis of proteins. These IMERs were then coupled on-line to nanoLC-MS² for the analysis of a model protein, cytochrome C. Digestion yields on IMERs presented a good repeatability. However, digestion efficiency on the pepsin-based IMERs remains so far insufficient and grafting or digestion procedure needs to be readjusted
Belhadj-Kaabi, Faten. "Développement et caractérisation de polymères à empreintes moléculaires pour l'extraction de composés pharmaceutiques à l'état de traces dans les fluides biologiques : miniaturisation du format de synthèse et couplage en-ligne à la nano-chromatographie." Paris 6, 2008. http://www.theses.fr/2008PA066542.
Nouri, Bahia. "Dosage des pesticides dans l'eau : mise au point et application des méthodes de dosage par extraction liquide-solide et analyse par chromatographie en phase liquide et en phase gazeuse." Montpellier 1, 1997. http://www.theses.fr/1997MON13501.
Arrambide, Cruz Carlos. "Méthodologies de synthèse de résines formo-phénoliques chélatantes : vers une extraction solide-liquide optimisée des métaux stratégiques." Thesis, Montpellier, 2017. http://www.theses.fr/2017MONTT169.
Extraction of specific targeted species (rare earth, heavy metals, transition metals, radionuclides) from industrial (mining deposit and urban mining) and nuclear effluents is an important issue in the recycling and / or decontamination processes. A large number of organic and inorganic solids, chelating or ion-exchanging materials, have been developed for selective ionic separation by solid / liquid process. Metal-specific ligands incorporate in the structure of the resin itself is an interesting way to perform ion separation taking the advantage of the selectivity of chelating agents. The aims of this project are firstly the synthesis of chelating original systems and then prepare specific ion exchange resins.From formo-phenolic resins incorporating catechol and 8-hydroxyquinoline, we have been able to show that the selective recovery of germanium from silicon or zinc was possible, , depending on their proportion of each phenolic precursors in the polymeric matrix.The synthesis of the phenolic precursors integrating ligands such as diglycolamic acid and diglycolamides allowed the use of resin for the recovery of rare earths elemnets. A study on the understanding of the synthesis of resins as well as their performance of extraction was thus realized and was able to highlight the potential of these resins for the recovery and valorization of the rare earths elements.An opening towards other possibilities of synthesis of this type of resins (porous materials, in the form of foam, etc.) is also proposed in order to increase the contact surfaces during solid-liquid extractions and thus increase the performance of these materials
Delaunay-Bertoncini, Nathalie. "Developpement d'immunoadsorbants à base d'anticorps monoclonaux pour l'extraction selective de familles de micropolluants organiques contenus dans des matrices complexes : comparaison avec des polymères à empreinte moléculaire." Paris 6, 2001. http://www.theses.fr/2001PA066507.
Madru, Benjamin. "Développement d'un support d'extraction sélective à base d'aptamères : synthèse, caractérisation et application à des matrices complexes." Phd thesis, Université Pierre et Marie Curie - Paris VI, 2010. http://pastel.archives-ouvertes.fr/pastel-00538840.
Tachon, Romain. "Apport de la chromatographie en phase liquide couplée à la spectrométrie de masse pour l'analyse de traces d'explosifs : optimisation des conditions d'extraction et de purification pour le traitement d'échantillons récupérés sur une scène d'attentat." Paris 6, 2008. http://www.theses.fr/2008PA066669.
Comte, Julien. "Mise au point d’une méthodologie d’échantillonnage utilisant la micro-extraction sur phase solide pour la quantification de goudrons sur des procédés de thermolyse de la biomasse." Grenoble 1, 2008. http://www.theses.fr/2008GRE10152.
The gasification of biomass by thermochemical processes is presently a promising method of producting H2 and CO which are used for synthesis of biogasoil. However, the thermal treatment of biomass leads to the production of unwanted compounds referred to as "tar" (heavy hydrocarbons) of which the content in syngas must to be inferior to 0. 1 mg. Nm-3. Knowledge oftar content is consequently needed. To this end, a sampling methodology using SPME (Solid Phase MicroExtraction) was developed for the quantification of "model compounds" which represents the total tar content mainly emitted by two gasification or pyrolysis processes. Introduction of the notion of model compounds is intended to simplify the sampling methodology on one hand to overcome the possible limitations related to the sampling system developed in this work to allow SPME extraction on the other. For the two thermochemical processes,15 model compounds were selected. The quantification of these compounds required calibration of SPME fibres (polydimethylsiloxane coating) which allow us, over a range oftemperatures, to establish the absorption profiles and to determine distribution coefficients. Influence of the sampling conditions on the absorption and performance of the coupled SPME-gas Chromatography were also evaluated. Ln order to avoid repetitive calibrations, a model based on thermodynamic considerations was developed to speed-up determination of the distribution coefficient
Guyomard, Philippe. "Étude de faisabilité d'un extrudeur bivis en pressage-extrusion de graines oléoprotéagineuses." Compiègne, 1994. http://www.theses.fr/1994COMPD753.
Casas, Mora Alba. "A catch-and-release purification method to simplify the synthesis of cysteine-rich peptides." Thesis, Orléans, 2017. http://www.theses.fr/2017ORLE2050/document.
Although solid phase peptide synthesis (SPPS) is a mature and widely popularized technique for simple peptides, some sequences are still complicated to produce, such as disulfide-rich peptides (DRPs). These natural products are able to selectively bind a wide number of therapeutically relevant targets, hence they are considered as promising drug candidates and pharmacological tools. The large proportion of cysteines in their sequence (more than 10%) confers them remarkable properties, but also limits their synthesis, lead ingto delicate HPLC purifications associated with low yields and poor purity.With the aim to simplify the chemical production of DRPs, we have developed an N-terminal linker: Boc-Cys(Trt)-1-{6-[1,3-dimethyl-2,4,6(1H,3H,5H)trioxopyrimidine-5-ylidene]hexyl}, which can be used for non chromatographiccatch-and-release purifications. It has been designed to be completely compatible with unprotected cysteine-containing peptides. Following solid phase elongation, this linker is selective lyintroduced at the N-terminus of the target peptide, leaving unreacted truncated acetylated peptides which are the main co-products of SPPS. After cleavage from the SPPS resin, the target peptide is immobilized on a second solid support through native chemical ligation (NCL). The truncated peptides are then removed by simple filtration. Cleavage of the linker finally releases the purified peptide into solution.Having in mind the future extension our strategy to the synthesis of very long DRPs through successive solid-supported NCLs of multiple peptide segments, we have studied in detail the stability and cleavage conditions of the N-terminal linker.To explore the scope and limitations of the method, it has been applied to the purification of two biologically-relevant cysteine-rich peptide sequences: chicken AvBD2 (36 AA), a β defensin antimicrobial peptide, and Bv8 (77 AA), a prokineticin-like peptide from yellow-bellied toad
Gervais, Gaël. "Rôle des paramètres opératoires sur la fiabilité d’une analyse multi-résidus de micropolluants dans l’eau : extraction sur phase solide, séparation par chromatographie liquide à très haute pression et détection par spectrométrie de masse en tandem." Rennes 1, 2010. http://www.theses.fr/2010REN1S057.
The occurrence of micropollutants is a major aspect in water quality assessment. For the last few years, analytical methods combining solid-phase extraction, liquid chromatography and tandem mass spectrometry has become the main technique for the analysis of a broad range of micropollutants. On the basis of some pesticides and endocrine disruptor compounds in water analysis, impacts of the parameters: extraction, separation, detection and data processing, on the analysis reliability (repeatability, accuracy, stability, reproducibility…) have been studied. Each step of the analytical method has been optimized and the parameters, affecting substance signals have been discussed. A global reflection upon the cause of signal variations and the possible answers to apply has been conducted. Proposed answers were validated by real matrix analysis and inter-laboratory studies. This work presents the tools and the key-points to ensure the results obtained by liquid chromatography/tandem mass spectrometry analysis
Mokh, Samia. "Optimisation de techniques analytiques pour caractériser les antibiotiques dans les systèmes aquatiques." Electronic Thesis or Diss., Bordeaux 1, 2013. http://www.theses.fr/2013BOR14950.
Antibiotics are pollutants present in aquatic ecosystems ultimate receptacles of anthropogenic substances. These compounds are studied as their persistence in the environment or their effects on natural organisms. Numerous efforts have been made worldwide to assess the environmental quality of different water resources for the survival of aquatic species, but also for human consumption and health risk related. Towards goal, the optimization of analytical techniques for these compounds in aquatic systems remains a necessity. Our objective is to develop extraction and detection methods for 12 molecules of aminoglycosides and colistin in sewage treatment plants and hospitals waters. The lack of analytical methods for analysis of these compounds and the deficiency of studies for their detection in water is the reason for their study. Solid Phase Extraction (SPE) in classic mode (offline) or online followed by Liquid Chromatography analysis coupled with Mass Spectrometry (LC/MS/ MS) is the most method commonly used for this type of analysis. The parameters are optimized and validated to ensure the best conditions for the environmental analysis. This technique was applied to real samples of wastewater treatment plants in Bordeaux and Lebanon
Betton, Clélia. "Nouvelle stratégie d'extraction et de purification de l'hydrazine N2H4 de grade spatial via le procédé Raschig : synthèse, modélisations cinétiques, équilibres entre phases et schémas de procédé." Thesis, Lyon 1, 2014. http://www.theses.fr/2014LYO10366/document.
This work, funded by the CIBLE-Rhône-Alpes Region, in partnership with the HERAKLES-SAFRAN group, aims to develop a new method for extracting and purifying hydrazine N2H4, for space applications. This monopropellant must be of very high purity, with an upper mass composition of 99.5% hydrazine and a carbon content of less than 30 ppm.The first part of this study allowed us to identify the reactions of formation and degradation to establish a global kinetic model and determine the guiding parameters of synthesis. Knowledge of the compositions of reaction liquors function of operating conditions of the synthesis, has allowed us to position, on leaving the reactor, the overall mixing point in the diagrams of ternary and quaternary phases in order to define the optimum extraction conditions.The second part concerns the detailed thermodynamic study of the new method of extraction, which is, not to extract excess ammonia from the reaction mixture but maintain the in situ to extract the hydrazine in the liquid phase separation -liquid by solvent effect. The aim ultimately is to get a virtually anhydrous ammonia phase so as to eliminate multiple distillations and complex extraction and purification encountered in the traditional process. This new strategy is based on the existence of a miscibility gap in the liquid state, in the H2O-NH3-H2O-NaOH ternary system and N2H4-NH3-NaOH quaternary system at a pressure of between 15 and 20 bar.The last part deals with the process engineering component. The operation of kinetic model and phase diagrams involved allowed us to determine the optimum conditions of synthesis and isolation, to calculate the composition of the material flow at the end of each unit operation and compare them with previous industrial processes . The process diagrams for each option have been prepared and analyzed at cost, safety and specifications obtained useful product
Mokh, Samia. "Optimisation de techniques analytiques pour caractériser les antibiotiques dans les systèmes aquatiques." Thesis, Bordeaux 1, 2013. http://www.theses.fr/2013BOR14950/document.
Antibiotics are pollutants present in aquatic ecosystems ultimate receptacles of anthropogenic substances. These compounds are studied as their persistence in the environment or their effects on natural organisms. Numerous efforts have been made worldwide to assess the environmental quality of different water resources for the survival of aquatic species, but also for human consumption and health risk related. Towards goal, the optimization of analytical techniques for these compounds in aquatic systems remains a necessity. Our objective is to develop extraction and detection methods for 12 molecules of aminoglycosides and colistin in sewage treatment plants and hospitals waters. The lack of analytical methods for analysis of these compounds and the deficiency of studies for their detection in water is the reason for their study. Solid Phase Extraction (SPE) in classic mode (offline) or online followed by Liquid Chromatography analysis coupled with Mass Spectrometry (LC/MS/ MS) is the most method commonly used for this type of analysis. The parameters are optimized and validated to ensure the best conditions for the environmental analysis. This technique was applied to real samples of wastewater treatment plants in Bordeaux and Lebanon
Hajouj, Zahira. "Mélanges mécaniques de phases greffées sur gel de silice. Application en chromatographie planaire et en extraction en phase solide vis-à vis d'hydrocarbures aromatiques polycondensés et d'azaarènes, polluants de l'environnement." Aix-Marseille 3, 1997. http://www.theses.fr/1997AIX30076.
Desgranges, Nathalie. "Développement d'échantillonneurs passifs de type POCIS pour l'évaluation de la contamination en pesticides des eaux de bassins versants languedociens." Thesis, Bordeaux, 2015. http://www.theses.fr/2015BORD0041/document.
Despite a noticeable sales decrease since few years, France remains the first european user of phytosanitary products. This is not without consequences on the environment and the untargeted organisms. Several studies allowed on one hand to better understand phenomena of pesticides transfer in water-air and soils compartments and on the other hand to highlight their contamination. Data concerning the water are more numerous cause of its status of ultimate receptacle of pollution and standards established by regulatory texts. The european Water Framework Directive (WFD) adopted in 2000 aims to achieve good chemical and ecological status of water bodies by 2015 with an obligation of results. The good chemical status depends on respect for the Environmental Quality Standards (EQS) established, for instance, for 24 pesticides. In 2012, 5% of river measurement points and 19%of groundwater measurement points do not respect these EQS. For many years, Languedoc Roussillon is the first wine-producing region of France and suffers from a significant pesticide pressure. In 2014, a report from the Regional Health Agency (RHA) has mentioned a relatively recent use of banned pesticides since the early 2000’s like simazin and terbutylazin. Moreover, RHA stated that most of recognized cases of non-compliance could be linked to the presence of agricultural activity in the catchment basin.[...] The establishment of POCIS devices on the three study sites showed the predominance ofpesticides used in viticulture and showed all the interest of the tool on a qualitative point ofview. The comparison of the tool with the automated sampling shows disparities between real concentration and concentration estimated with the POCIS. However, it remains to improvethe tool on a quantitative way to obtain a reliable and robust sampler for this type of exposure medium
Lassagne, Laurent. "Conception et réalisation d'un pilote de combustion en lit fluidisé circulant : caractérisation et dosage des HAP gazeux à l'émission : développement d'une méthodologie analytique par micro extraction en phase solide." Université Joseph Fourier (Grenoble), 1999. http://www.theses.fr/1999GRE10192.
Dakas, Pierre-Yves. "Divergent synthesis of resorcyclic acid lactones : a privileged natural pharmacophore." Strasbourg, 2009. http://www.theses.fr/2009STRA6265.
Protein kinases play a fundamental role in many cellular processes and signal transduction pathways. Numerous pathologies can be attributed to a dysfunctional kinase. Their specific inhibition became a priority in therapy and is expected to allow the determination of the functionality of each individual kinases in the kinome. Most inhibitors targeting kinases are heterocycles with some reminiscence of the adenosine scaffold. As I began my thesis, the group of Professor Nicolas Winssinger had become interested in a family of natural products which has a high incidence in kinases inhibition. This family is known as resorcylic acid lactones (RALs) and contains several kinase inhibitors (Figure 1). [1] The aim of my project was to develop flexible synthetic strategies towards RALs amenable to the preparation of libraries extending beyond the diversity of the analogues accessible from natural sources
Charlot, Alexandre. "Synthèse et Evaluation de silices hybrides mésoporeuses pour l'extraction de l'uranium en milieu sulfurique." Thesis, Montpellier, Ecole nationale supérieure de chimie, 2016. http://www.theses.fr/2016ENCM0006/document.
Nuclear industries are perpetually looking for technical, economic and environmental progresses. Important volumes of acidic waste are generated by nuclear plants of the front end. The extraction of uranium from these solutions is required to decontaminate effluents (decrease of the radioactivity) and value uranium (reincorporation in the cycle). Uranium leaching is mostly achieved using sulfuric acid leading to the production of aqueous effluents that contain a large grade of sulfate complexes. In such conditions, uranyl sulfate complexes constitute the predominant uranium species in solution and its extraction represents a real scientific and technological challenge. Commonly, precipitation, solvent extraction or solid phase extraction are used. The last one is particularly adapted for low grade solutions due to it weak environmental footprint (no solvent are handling) and the facility of the process involved (i.e. fixed bed column). Among the available solid-phase extraction candidates, hybrid mesoporous silicas get a crucial part. They develop a very high specific surface areas and a driven porosity which give them a high potential of extraction capacities.In this manuscript the tailoring and the evaluation of hybrid mesoporous silicas have been investigated. Firstly, the work focus on the organic part grafted by post-synthetic pathway, the N,N-dialkylcarbamoylphosphonate based molecules have been identified to get interesting extraction properties. This study emphasizes that acid groups are required and that alkyl substituents get a real importance in the extraction efficiency. On the second hand, the role of pore size has been investigated. The results obtained disclosed that pores size diameters directly impact the grafting ratio as well as the homogeneity of the material: (1) materials with a pore size below 3 nm are heterogeneously functionalized due to steric issues, (2) a homogeneous organic monolayer grafted onto the silica skeleton occurs when the pore size ranges from 3 nm to 20 nm and (3) functionalization of material having pore size above 30 nm results in an organic multilayer covalently linked to the surface. The organic self-organization drives the extraction efficiency, only monolayers lead to promising results. At the saturation state, two molecules are required to extract one uranyl ion. To describe the molecular scale of the uranyl complex onto the solid, the local structure has been investigated by a parametric study and spectroscopic techniques (IR, EXAFS and DRX). Results reveal that two diamido-phosphonates are involved in the uranyl extraction. By this work, it is shown how the molecular scale helps to understand the macroscopic phenomena.Finally, continuous extraction in a fixed bed column confirms the extractive properties obtained in batch mode experiments and points out the potential of such material to be reused several times without any damages
Lopez, Claire. "Synthèse de polymères à empreintes moléculaires d'alcaloïdes Vinca pour leur extraction sur phase solide dans des extraits de plantes ou des fluides biologiques : développement du détecteur conductimétrique sans contact à couplage capacitif et de la technique de la double injection en électrophorèse capillaire." Thesis, Orléans, 2010. http://www.theses.fr/2010ORLE2078.
This thesis reports in a first part results obtained with molecularly imprinted polymers (MIP) during solid liquid extraction. Polymer-analyte interactions, composition of the sample matrix and selectivity of MIPs have been studied.The first application concerned the extraction of molecules in a plant extract. Two MIPs respectively prepared from the methacrylic acid (MAA) and itaconic acid ( IA) and with respectively catharanthine and vindoline as template showed their selectivity on standard solutions then on a plant extract. Experiments of cross reactivity performed with analogue of the template (dimers alkaloids) have proved the specificity of analytes recognition by the MIPs. The MIP-catharanthine is characterized by Scatchard isotherms and its capacity was estimated from the extract of Catharanthus roseus. A MIP prepared from MAA with the vinorelbine as template was applied in salt aqueous matrices for the extraction of vinflunine and its metabolite in bovine plasma and urine. High extraction recoveries were reached with a study of the impact of salts and the choice of washing solvents adapted to the matrix. The second part showed the simplicity of use and the sensibility of capacitively coupled contactless conductivity detection (C4D) for the analysis of counter-ion and active principle in pharmaceutical compounds in capillary electrophoresis (CE). The technique of double injection allowed the simultaneous analysis of cations and anions. The developed method EC-C4D was applied to Vinca alkaloids and various medicines with anionic or cationic counter-ions
Eddhif, Balkis. "Développement d'une approche analytique non ciblée pour l'étude des protéines dans les milieux complexes, environnementaux et biologiques." Thesis, Poitiers, 2017. http://www.theses.fr/2017POIT2291/document.
Recent advances in proteomics have been spurred by the rapid development of hybrid and/or high-resolution mass analysers (HRMS/MS). These powerful instrumentations have led to significant improvements in « Bottom-up » approach and have enabled to deepen our knowledge on the functionality of biological systems (structure, function, metabolism, dynamic, etc).Despite their high sensibilities, the potential of such instruments could be significantly lessened by an imperfect sample pre-treatment. In this context, current sample pretreatments follow multi-steps experimental workflows, which alternatively lead to low recoveries of proteins. In this line, this study aims at developing a simple and versatile strategy in order to reduce protein losses and enhance their detection in gel-free LC-MS analysis. First, an analytical method based on liquid chromatography and tandem mass spectrometry was developed to detect and quantify complex peptides mixture. Secondly, a universal, simple and fast purification approach was designed with the aim to purify protein extracts in only one-step. For this purpose, the molecular reactivity, dynamics and conformational changes of proteins at each development step were comprehensively investigated with a set of spectroscopic techniques, in order to select the best strategy. Finally, different factors influencing extraction of proteins were investigated with the goal in the long term to propose an on-demand extraction protocol for direct analysis of proteins by LC-HRMS/MS
Kouzayha, Abir. "Développement des méthodes analytiques pour la détection et la quantification de traces des HAP et de pesticides dans l'eau : application à l'étude de la qualité des eaux libanaises." Thesis, Bordeaux 1, 2011. http://www.theses.fr/2011BOR14414/document.
Water pollution presents a very critical problem facing industrial and developping countries. The environmental monitoring of the contaminants seems necessary to understand their sources and impacts. Among a wide variety of organic pollutants present in water,polycyclic aromatic hydrocarbons (PAHs) and pesticides are of particular importance as widespread, persistent, and toxic contaminants. They are usually present at trace levels in theacquatic surfaces; therefore their detection and control require selective and sensitiveanalytical procedures. The Solid-Phase Extraction (SPE) followed by the Gas-Chromatography coupled to Mass Spectrometry (GC-MS) are the most commonly usedtechniques for their analysis in water. Thesis objectives are focused on the development of new analytical methods for the extraction and analysis of these two families of pollutants present in water. To overcone the contraints of the traditional SPE, a new approach was developed consisting on the introduction of the centrifugation in several steps of the procedure. The new method showed practical environmental and economical advantages interms of sample preparation time, simplicity, reduction in solvent use, and cost and isparticularly suitable for routine applications requiring a high sample throughput. Aprogrammed temeperature vaporizing (PTV) injection method was also optimized and validated in order to improve the detection limits for the GC-MS analysis of PAHs. The evaluation of the quality of different water systems in Lebanon including rainwater,groundwater, drinking water and surface water was accomplished in this study
Chirita, Raluca-Ioana. "Développement de nouvelles méthodes séparatives compatibles avec une détection par spectrométrie de masse et par électrochimie pour l'analyse de traces de catécholamines et molécules apparentées." Thesis, Orléans, 2009. http://www.theses.fr/2009ORLE2043/document.
As neurotransmitters, catecholamines play an important role in the control and regulation of numerous brain functions. They are also believed to be implicated in different neurodegenerative disorders. First an ion pairing chromatography method using nonafluoropentanoic acid as volatile ion paring agent was developed on the new generation of C18 columns (monolith and fused core). This method is compatible with MS detection in positive ionization mode. Secondly an HILIC method was optimized using different commercially available HILIC supports, they can be classified as follows: neutral (diol, amide, and cyano bounded), positively charged (amino, triazole bounded), negatively charged (bare silica as wholly porous particles or fused core particles columns) and zwitterionic (sulfobetaine bounded). Our studies lead us to a better understanding of the HILIC retention mechanism and also to the selection of the most appropriated column for catecholamine analysis. Only the HILIC system was compatible with both positive and negative ionization modes. The two chromatographic systems were then compared in terms of resolution, efficiency, detection and quantification limits (LOD/LOQ), calibration linearity and repeatability. The LODs obtained were in the range of 1-100 ng.mL-1. A simple pre-concentration method using Oasis HLB and PGC solid phase extraction cartridges has been optimized in order to enhance the LODs. Finally the optimized SPE-LC-MS/MS method has been applied to the identification of these compounds present in brain extracts
Aftim, Nadin. "Polymères à empreinte moléculaire pour l'extraction d'un insecticide organophosphoré utilisé en oléiculture : le phosmet." Thesis, Perpignan, 2017. http://www.theses.fr/2017PERP0030.
The objective of this thesis has been the synthesis of a molecularly imprinted polymer (MIP) for the extraction of phosmet, an organophosphorus pesticide widely used in olive growing. The search for the functional monomer (FM) having the best ability to interact non-covalently with phosmet in the presence of the most suitable pore-forming solvent was carried out for the first time by means of an acetylcholinesterase sensor. This innovative strategy allowed us to better understand the kinetic mechanisms of FM-template interaction. Because of the importance of its role in determining the structure of a MIP, the selection of a crosslinking agent with adequate physicochemical characteristics made it possible to select the best MIP, whose adsorption isotherms were studied according to Freundlich and Langmuir models. Extraction of phosmet using a Molecularly Imprinted Solid Phase Extraction (MISPE) procedure was carried out via an SPE cartridge, whose capacity was evaluated from a standard solution. The choice of reagents and experimental conditions were validated by carrying out selectivity assays using another organophosphorus insecticide. Extraction of phosmet from olive oil was successfully carried out according to an optimized reverse flow extraction protocol. This work opens new opportunities for studying new FM-template interactions by means of enzymatic biosensors capable of detecting other inhibitors such as herbicides, fungicides and other pesticides
Sbruzzi, Dalva. "Análise da viabilidade econômica da purificação da bromelina das folhas de curauá em sistema bifásico aquoso PEG/Fosfato." [s.n.], 2010. http://repositorio.unicamp.br/jspui/handle/REPOSIP/266969.
Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Química
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Resumo: O curauá (Ananas Erectifolius L.B. Smith), espécie vegetal de porte herbáceo, é uma monocotiledônea pertencente à família Bromeliaceae, nativa da região norte do Brasil, especialmente da Amazônia, de onde pode ser extraída a bromelina. Essa faz parte de um grupo de enzimas proteolíticas, usadas na indústria alimentícia e como medicamento, pois oferece amplo espectro de eficácias terapêuticas: antiedemas, anti-inflamatórias, antitrombóticas e atividades fibrinolíticas. O desenvolvimento de novos processos de extração e purificação de proteínas é muito importante, uma vez que essa é uma etapa limitante na produção de bioprodutos. Sistemas de duas fases aquosas são amplamente utilizados para a separação e purificação de biomoléculas. As vantagens da extração em duas fases aquosas, em comparação com outros métodos de purificação, são o elevado rendimento, a faixa de trabalho próxima do equilíbrio, a fácil ampliação de escala e o uso em processos contínuos. Esta pesquisa propõe a caracterização da bromelina do curauá e a sua purificação por extração líquido-líquido em duas fases aquosas, formadas por um polímero (polietilenoglicol) e um sal (fosfato de potássio). Apresenta também um estudo sobre os custos do processo e o preço de venda estimado, e demonstra a sua viabilidade econômica, quer seja para uso como pré-processo nos tradicionais sistemas cromatográficos, quer para a comercialização direta, como alternativa para a bromelina do abacaxi. Os resultados da caracterização mostraram que as condições ideais de trabalho são pH 8,5 e temperatura 35º C para a variedade branca, e pH 8,5 e 30º C de temperatura para a variedade roxa. A massa molar é de 24 kDa, e o melhor sistema de partição da bromelina foi o SBA PEG 4000 em pH 9. A solução enzimática dos melhores sistemas contém 7 U de bromelina e, aproximadamente, 17 mg/L de proteína total medida por Bradford (curauá branco); e 6 U de bromelina e, aproximadamente, 23 mg/L de proteína total medida por Bradford (curauá roxo). O preço de venda calculado para um litro dessa solução enzimática, quando não se obtém lucro (margem de lucro desejada é 0%), foi estimado em R$75,06. Assim, pode-se concluir que o processo de purificação da bromelina das folhas de curauá, ao ser utilizado sistema bifásico aquoso, PEG/sal, é promissor no que diz respeito a sua possibilidade de produção em escala industrial
Abstract: Curaua (Ananas erectifolius L.B. Smith) is a mocotyledonous herbaceous specie belonging to the Bromeliaceae family and it is native to the north region of Brazil, especially the Amazonian Complex, that we can extract bromelain which belongs to a group of proteolytic enzymes derived from herbaceous species of Bromeliaceae family, which are used in food industries and as drugs as such as they offer a wide spectrum of therapeutic efficacies: antiedemateous, antiinflammatory, antithrombotic and fibrinolytic activities. The development of new extraction and purification processes of proteins is very important, as this is a limiting step in the production of bioproducts. Aqueous two-phase systems are widely used for separation and purification of biomolecules. The advantages of aqueous two-phase extraction compared to other purification methods lie in high productivity, working range close to equilibrium, easy scale up and use in continuous processes. This research proposes the curaua's bromelain characterization, and its purification by a liquid-liquid extraction in aqueous two-phase system, formed by a polymer (polyethylene glycol) and a salt (potassium phosphate). It also presents a study about the costs of this process and the estimated sale price, showing its economic viability, whether it is for use as a pre-process in traditional chromatographic systems or direct commercialization, as an alternative for the bromelain of pineapple. The curaua's bromelain characterization results showed that the ideal working conditions are pH 8.5 and 35 ºC of temperature to white variety and pH 8.5 and 30°C of temperature to purple variety. The curaua's molecular weight is 24 kDa and the best bromelain partitioning system was the SBA PEG 4000 at pH 9. The enzyme solution of the best purification system contains 7 U of bromelain and about 17 mg/L of total protein measured by Bradford (white curaua) and 6 U of bromelain and about 23 mg/L of total protein measured by Bradford (purple curaua). The estimated sale price for a liter of this enzyme solution, when profit is not achieved (0% of desired markup), was estimated at R$ 75, 06. So, the curaua's bromelain purification process using an aqueous two-phase system, PEG/salt, is promising with regard to the possibility of industrial scale production
Mestrado
Sistemas de Processos Quimicos e Informatica
Mestre em Engenharia Química