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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
21

Microwave-assisted cloud point extraction coupled with DRC-ICP-MS for the determination of Cr, Cu, Cd and Pb in water samples

Gu, Yu-chang 08 February 2010 (has links)
none
22

Ultrasound Assisted And Supercritical Carbon Dioxide Extraction Of Antioxidants From Roasted Wheat Germ

Gelmez, Nilufer 01 February 2008 (has links) (PDF)
This study covers the extraction of antioxidants from wheat germ / which is the byproduct of the flour-milling industry and a rich source of antioxidants / with Ultrasound Assisted (UAE) and Supercritical Carbon Dioxide (SC-CO2) extractions. Extraction conditions were ultrasonication time (1&ndash / 11 min), temperature (20&ndash / 60&deg / C) and ethanol level (5&ndash / 95%) for UAE, and pressure (148&ndash / 602 bar), temperature (40&ndash / 60&deg / C) and time (10&ndash / 60 min) for SC-CO2 extraction. The extraction conditions were optimized based on yield (%), total phenolic contents (TPC, mg GAE/g extract) and antioxidant activities (AA, mg scavenged DPPH&amp / #729 / /g extract) of the extracts, using Central Composite Rotatable Design. Total tocopherol contents (TTC) of the extracts were determined, as well. UAE (at 60&deg / C) with low ethanol level (~5-30%) and short times (1-3 min) provided protein rich extracts with high yield, medium TPC and AA. On the other hand, with high ethanol level (~90%) and long times (6-11 min), waxy structured extracts with low yield but high TPC and AA were obtained. SC-CO2 extraction at 442 bar, 40&ordm / C and 48 min. enabled almost 100% recovery of wheat germ oil (9% yield) but TPC and AA of the extracts were low. On the contrary, the extracts obtained at lower pressures (~150bar) and shorter times (~10 min) at 50-60&ordm / C had high TPC and AA since the oil yield was low. However, TPC and AA of these extracts were only half of those extracted by UAE. Maximum tocopherol (7.142 mg tocopherol/g extract) extraction was achieved at 240 bar, 56&ordm / C for 20 min. Both of the methods extracted high amounts of tocopherols from roasted wheat germ (SC-CO2 extraction / 0.31 mg tocopherol/g germ, UAE / 0.33 mg tocopherol/g germ) but TTC of the extracts obtained by SC-CO2 extraction was superior compared to 1.170 mg tocopherol/g extract obtained by UAE at 9 min, 58&ordm / C and 95% ethanol level. All these extracts with different characteristics have potential uses in cosmetic and food industry depending on the targeted specific application.
23

Recuperação de compostos bioativos do resíduo do processamento do café (silverskin) : otimização do processo de extração; caracterização química, capacidade antioxidante e toxicidade dos extratos

Santos, Anai Loreiro dos January 2018 (has links)
O silverskin é um resíduo, rico em compostos antioxidantes, como o ácido 5-cafeoilquínico (5-CQA) e a cafeína (CAF), produzido durante a torrefação dos grãos de café. O objetivo deste estudo foi desenvolver uma metodologia de extração, aliando a extração assistida por ultrassom e o planejamento de experimentos, para a recuperação simultânea do 5-CQA e da CAF da silverskin. Os extratos gerados foram caracterizados e tiveram a capacidade antioxidante e a toxicidade investigadas. A metodologia de superfície de resposta e a função Desejabilidade foram empregadas na otimização da extração. A LC-DAD/MSn foi utilizada para a caracterização dos extratos, os métodos de sequestro do radical DPPH e de redução do ferro (FRAP), para avaliar a capacidade antioxidante; enquanto o ensaio da Artemia salina foi usando para avaliar a toxicidade. As condições ótimas de extração foram: 45 % de etanol em água como solvente de extração, razão amostra-solvente 1/20, extração por 7 min a 59 °C, com rendimentos de 5-ACQ e CAF de respectivamente 2,00 e 6,26 mg g-1. No total, 9 derivados clorogênicos foram tentativamente identificados. Os teores de teofilina, ácido cafeico e derivados clorogênicos foram respectivamente: 0,53, 0,06 e 4,40 mg g-1. O extrato demonstrou considerável capacidade antioxidante, com concentração eficiente de 46,87 mg L-1 e capacidade redutora de ferro de 152,71 μM de FeSO4 g-1, além de alta toxicidade. O método desenvolvido obteve rendimento similar ao da extração sólido-líquido para o 5-ACQ. / Silverskin is a waste generated during the coffee beans roasting. This residue has been showing antioxidant compounds, mainly 5-caffeoylquinic acid (5-CQA) and caffeine (CAF). The aim of this study was used the design of experiments and ultrasound-assisted extraction to develop an extraction method for the efficient recovery of 5-CQA and CAF from silverskin, simultaneously. In addition, the optimized extract was characterized, and its antioxidant capacity and acute toxicity were investigated. The response surface methodology and Desirability function were employed to optimize the extraction. The chemical characterization was carry out by LC-DAD/ESI-MSn. Antioxidant capacity was evaluated by DPPH (2, 2-diphenyl-1 picryl hydrazyl) and FRAP (ferric reducing antioxidant power) methods and the acute toxicity by Artemia salina assay. The optimal extraction conditions were 45.0 % ethanol in water, the solid-to-liquid ratio was 1:20, and extraction for 7.0 min at 59 °C. Under optimal conditions, the yield of 5-CQA and CAF were 2.00 and 6.26 mg g-1, respectively. Theophylline, caffeic acid, and total chlorogenic acid concentrations were 0.53, 0.06 e 4.40 mg g-1, respectively and 9 chlorogenic acids were identified in the extract. The extract showed considerable antioxidant capacity, with efficient concentration value of 46,87 mg L-1 in the DPPH assay and 152,71 μM FeSO4 g-1 (FRAP) and high toxicity. The developed extraction methodology showed similar performance as solid-liquid extraction to 5-CQA yield.
24

Recuperação de compostos bioativos do resíduo do processamento do café (silverskin) : otimização do processo de extração; caracterização química, capacidade antioxidante e toxicidade dos extratos

Santos, Anai Loreiro dos January 2018 (has links)
O silverskin é um resíduo, rico em compostos antioxidantes, como o ácido 5-cafeoilquínico (5-CQA) e a cafeína (CAF), produzido durante a torrefação dos grãos de café. O objetivo deste estudo foi desenvolver uma metodologia de extração, aliando a extração assistida por ultrassom e o planejamento de experimentos, para a recuperação simultânea do 5-CQA e da CAF da silverskin. Os extratos gerados foram caracterizados e tiveram a capacidade antioxidante e a toxicidade investigadas. A metodologia de superfície de resposta e a função Desejabilidade foram empregadas na otimização da extração. A LC-DAD/MSn foi utilizada para a caracterização dos extratos, os métodos de sequestro do radical DPPH e de redução do ferro (FRAP), para avaliar a capacidade antioxidante; enquanto o ensaio da Artemia salina foi usando para avaliar a toxicidade. As condições ótimas de extração foram: 45 % de etanol em água como solvente de extração, razão amostra-solvente 1/20, extração por 7 min a 59 °C, com rendimentos de 5-ACQ e CAF de respectivamente 2,00 e 6,26 mg g-1. No total, 9 derivados clorogênicos foram tentativamente identificados. Os teores de teofilina, ácido cafeico e derivados clorogênicos foram respectivamente: 0,53, 0,06 e 4,40 mg g-1. O extrato demonstrou considerável capacidade antioxidante, com concentração eficiente de 46,87 mg L-1 e capacidade redutora de ferro de 152,71 μM de FeSO4 g-1, além de alta toxicidade. O método desenvolvido obteve rendimento similar ao da extração sólido-líquido para o 5-ACQ. / Silverskin is a waste generated during the coffee beans roasting. This residue has been showing antioxidant compounds, mainly 5-caffeoylquinic acid (5-CQA) and caffeine (CAF). The aim of this study was used the design of experiments and ultrasound-assisted extraction to develop an extraction method for the efficient recovery of 5-CQA and CAF from silverskin, simultaneously. In addition, the optimized extract was characterized, and its antioxidant capacity and acute toxicity were investigated. The response surface methodology and Desirability function were employed to optimize the extraction. The chemical characterization was carry out by LC-DAD/ESI-MSn. Antioxidant capacity was evaluated by DPPH (2, 2-diphenyl-1 picryl hydrazyl) and FRAP (ferric reducing antioxidant power) methods and the acute toxicity by Artemia salina assay. The optimal extraction conditions were 45.0 % ethanol in water, the solid-to-liquid ratio was 1:20, and extraction for 7.0 min at 59 °C. Under optimal conditions, the yield of 5-CQA and CAF were 2.00 and 6.26 mg g-1, respectively. Theophylline, caffeic acid, and total chlorogenic acid concentrations were 0.53, 0.06 e 4.40 mg g-1, respectively and 9 chlorogenic acids were identified in the extract. The extract showed considerable antioxidant capacity, with efficient concentration value of 46,87 mg L-1 in the DPPH assay and 152,71 μM FeSO4 g-1 (FRAP) and high toxicity. The developed extraction methodology showed similar performance as solid-liquid extraction to 5-CQA yield.
25

Avaliação de um sistema FI-HG-MF-AAS e extração assistida pro micro-onda na especiação de arsênio inorgânico / Evaluation of a FI-HG-MF-AAS system and microwave-assisted extraction on inorganic arsenic speciation

Lehmann, Eraldo Luiz, 1981- 20 August 2018 (has links)
Orientadores: Marco Aurélio Zezzi Arruda, Anne-Hélène Fostier / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Química / Made available in DSpace on 2018-08-20T06:38:49Z (GMT). No. of bitstreams: 1 Lehmann_EraldoLuiz_M.pdf: 2472831 bytes, checksum: 9197e3f8344d1f42efcc6e44cd1ffe01 (MD5) Previous issue date: 2012 / Resumo: Nessa Dissertação foram avaliados um sistema de injeção em fluxo com geração de hidretos acoplado a um espectrômetro de absorção atõmica com atomizador forno metálico de liga Inconel 600® (FI-HG-MF-AAS), bem como a técnica de extração assistida por micro-onda (MAE) como método de preparo de amostra para especiação de arsênio inorgânico. Para o sistema FI-HG-MF-AAS, condições brandas (pH tamponado em 4,5 e concentração de tetraidridoborato(1-) 0,1% (m/v)) foram utilizadas para que apenas a espécie Asi(III) gerasse o seu respectivo hidreto (arsano - AsH3), atingindo-se limites de detecção de 2,0 mg L e quantificação de 6,6 mg L, tornando o método adequado para uso em análises que atendam a portaria de potabilidade de água de acordo com o Ministério da Saúde e Organização Mundial da Saúde (WHO). O Asi(V) não apresentou qualquer sinal nas condições brandas, e apenas o uso de L-cisteína como pré-redutor foi eficiente para sua conversão a Asi(III). O teste de recuperação foi realizado utilizando material de referência NIST 1643e, Traços de elementos em água, com 60,45 mg L de arsênio total. O resultado mostra que Asi(III) não está presente na amostra em concentração acima do limite de detecção, e usando L-cisteína na concentração de 3% (m/v), obteve-se 60,5 mg L de Asi total, atingindo 100% de recuperação. A técnica de extração assistida por micro-onda mostrou-se eficaz para a extração de As total no material certificado de plâncton BCR414, atingindo um nível 93% de recuperação. Também se mostrou eficiente para manter as espécies de As inorgânico (Asi(III) e Asi(V)) inalteradas, sendo assim uma técnica promissora para o preparo de amostras para a análise de especiação / Abstract: In this work a Flow Injection - Hydride Generation - Metallic Furnace - Atomic Absorption Spectrometry (FI-HG-MF-AAS) system was evaluated, using an Incone600 ® alloy tube as a metallic oven, as well as the technique of microwave-assisted extraction (MAE) for sample preparation aiming speciation of inorganic arsenic. For the FI-HG-MF-AAS system, mild conditions (buffered media at pH 4.5 and concentration of tetrahydridoborate (1-) 0.1% (m/v)) allow that only iAs(III) generates hydride (arsane - AsH3), reaching a detection limit of 2.0 m gL and limit of quantification of 6.6 mg L, making suitable for its use in analysis according to Brazilian's Ministry of Health and World Health Organization (WHO) for drinking water. The inorganic As(V) did not show signal in mild conditions, and only the use of L-cysteine as pre-reducing agent was efficient in its conversion to inorganic As(III). The recovery test was carried out using reference material NIST 1643e, Trace elements in water, with 60.45 mg L of total arsenic. The result shows that inorganic As(III) is not present at concentration above the limit of detection, and using L-cysteine 3% (w/v), was obtain a total inorganic As concentration of 60.5 mg L, reaching a recovery of 100%. Microwave-assisted extraction technique was effective for the extraction of the total arsenic in certified plankton BCR414material, reaching a recovery level of 93%. Additionally, it also proved to be effective in preserving the species of unchanged inorganic arsenic, making it a promising technique for sample preparation aiming a speciation analyzes / Mestrado / Quimica Analitica / Mestre em Química
26

Production d'extraits aqueux à partir d'Ulva sp, au moyen de procédés d'hydrolyse enzymatique : caractérisatin, valorisation et perspectives de développement. / Production of water soluble extracts from Ulva sp. using enzymatic hydrolysis processes : characterization, upgrading and potential development

Hardouin, Kévin 30 June 2015 (has links)
Ces travaux de thèse CIFRE, réalisés au sein du Laboratoire de Biotechnologie et Chimie Marines de l’Université de Bretagne-Sud et du Groupe Olmix, s’inscrivent dans le cadre d’un projet national de valorisation de biomasses d’algues vertes, le projet ULVANS. Ce projet est le fruit d’une collaboration entre cinq industriels bretons et deux laboratoires universitaires. Les objectifs de ces travaux de thèse concernent i) la caractérisation approfondie de la matière première, en particulier des polysaccharides matriciels solubles (ulvanes) et des protéines, ii) la mise au point d’un procédé d’extraction assistée par enzymes des métabolites algaux, iii) la caractérisation biochimique et moléculaire des hydrolysats enzymatiques, avec pour objectif la compréhension de l’effet des enzymes commerciales sur les algues, iv) l’évaluation des activités antioxydantes et antivirales des hydrolysats, v) l’étude de l’influence des paramètres d’hydrolyse en vue de déterminer les conditions optimales pour l’extraction des métabolites d’intérêt et enfin vi) de conclure, à partir des éléments fournis par l’étude, sur la viabilité d’un tel procédé à l’échelle industrielle. En conclusion de ces travaux, l’hydrolyse enzymatique apparait comme un procédé intéressant pour le bioraffinage des algues vertes. Bien que les préparations enzymatiques commerciales utilisées ne soient pas spécifiques des composés algaux, les protéases ont conduit à une augmentation significative des rendements d’extraction, alors que l’effet des carbohydrases reste modéré. L’étude de l’influence des paramètres d’hydrolyses a confirmé les résultats préliminaires et montré que la température, la concentration d’enzyme et la méthode de broyage présentaient peu d’effets sur les activités des protéases testées. Un résultat majeur de cette étude aura été la mise en évidence d’activités anti-herpétiques dans les hydrolysats. La caractérisation des fractions actives a montré que les activités étaient liées à la présence de protéines ou glycoprotéines dans les extraits. Ce résultat présente un intérêt majeur car à l’heure actuelle, a priori, aucune activité de ce type n’a été identifiée chez Ulva sp. / This PhD Thesis works, conducted in the Laboratoire de Biotechnologie et Chimie Marines of the Université de Bretagne-Sud and in the Olmix Group, was included in a national project for the upgrading of green seaweed biomasses, the Ulvans project. This project results in the collaboration of five industrial companies and two academic research laboratories. The objectives of this thesis works had been i) the characterization of the raw material, particularly the soluble matrix polysaccharides (ulvans) and proteins, ii) the development of an enzyme-assisted extraction process of algal metabolites, iii) the biochemical and molecular characterization of the enzymatic hydrolyzates, with the aim of understanding the effect of enzymes on algae thallus, iv) the screening of antioxidant and antiviral activities of hydrolyzates, v) the study of the influence of hydrolysis parameters to determine the optimum conditions for the extraction of metabolites of interest and finally vi) to conclude, according to the results provided by this study, on the viability of the industrial upscaling of the process. In conclusion of this work, enzymatic hydrolysis appeared to be an effective process for biorefinery of green seaweeds. Although commercial enzymatic preparations were not specific of algal compounds, protéases led to a significant increase in the extraction yields, whereas the effect of carbohydrases were moderate. The study of hydrolysis parameters confirmed the preliminary results and showed that the temperature, the concentration of enzyme and the grinding method had no effect on the protease used. A major result of this study has been the highlighting of anti-oxidant and anti-herpetic compounds in hydrolyzates. The antiviral activity of ulvans had several times been demonstrated but the biochemical characterization of actives fractions showed that the activity could be associated to proteins or glycoproteins. This result is very interesting because, a priori, any antiviral activity has also been related to this type of compounds in Ulva sp.
27

Recuperação de compostos bioativos do resíduo do processamento do café (silverskin) : otimização do processo de extração; caracterização química, capacidade antioxidante e toxicidade dos extratos

Santos, Anai Loreiro dos January 2018 (has links)
O silverskin é um resíduo, rico em compostos antioxidantes, como o ácido 5-cafeoilquínico (5-CQA) e a cafeína (CAF), produzido durante a torrefação dos grãos de café. O objetivo deste estudo foi desenvolver uma metodologia de extração, aliando a extração assistida por ultrassom e o planejamento de experimentos, para a recuperação simultânea do 5-CQA e da CAF da silverskin. Os extratos gerados foram caracterizados e tiveram a capacidade antioxidante e a toxicidade investigadas. A metodologia de superfície de resposta e a função Desejabilidade foram empregadas na otimização da extração. A LC-DAD/MSn foi utilizada para a caracterização dos extratos, os métodos de sequestro do radical DPPH e de redução do ferro (FRAP), para avaliar a capacidade antioxidante; enquanto o ensaio da Artemia salina foi usando para avaliar a toxicidade. As condições ótimas de extração foram: 45 % de etanol em água como solvente de extração, razão amostra-solvente 1/20, extração por 7 min a 59 °C, com rendimentos de 5-ACQ e CAF de respectivamente 2,00 e 6,26 mg g-1. No total, 9 derivados clorogênicos foram tentativamente identificados. Os teores de teofilina, ácido cafeico e derivados clorogênicos foram respectivamente: 0,53, 0,06 e 4,40 mg g-1. O extrato demonstrou considerável capacidade antioxidante, com concentração eficiente de 46,87 mg L-1 e capacidade redutora de ferro de 152,71 μM de FeSO4 g-1, além de alta toxicidade. O método desenvolvido obteve rendimento similar ao da extração sólido-líquido para o 5-ACQ. / Silverskin is a waste generated during the coffee beans roasting. This residue has been showing antioxidant compounds, mainly 5-caffeoylquinic acid (5-CQA) and caffeine (CAF). The aim of this study was used the design of experiments and ultrasound-assisted extraction to develop an extraction method for the efficient recovery of 5-CQA and CAF from silverskin, simultaneously. In addition, the optimized extract was characterized, and its antioxidant capacity and acute toxicity were investigated. The response surface methodology and Desirability function were employed to optimize the extraction. The chemical characterization was carry out by LC-DAD/ESI-MSn. Antioxidant capacity was evaluated by DPPH (2, 2-diphenyl-1 picryl hydrazyl) and FRAP (ferric reducing antioxidant power) methods and the acute toxicity by Artemia salina assay. The optimal extraction conditions were 45.0 % ethanol in water, the solid-to-liquid ratio was 1:20, and extraction for 7.0 min at 59 °C. Under optimal conditions, the yield of 5-CQA and CAF were 2.00 and 6.26 mg g-1, respectively. Theophylline, caffeic acid, and total chlorogenic acid concentrations were 0.53, 0.06 e 4.40 mg g-1, respectively and 9 chlorogenic acids were identified in the extract. The extract showed considerable antioxidant capacity, with efficient concentration value of 46,87 mg L-1 in the DPPH assay and 152,71 μM FeSO4 g-1 (FRAP) and high toxicity. The developed extraction methodology showed similar performance as solid-liquid extraction to 5-CQA yield.
28

EXTRACTION TECHNIQUES FOR TRACE ELEMENT DETERMINATIONS OF BIOLOGICAL AND ENVIRONMENTAL SAMPLES INCLUDING ELEMENTAL SPECIATION OF LOBSTER USING INDUCTIVELY COUPLED PLASMA - MASS SPECTROMETRY

Brisbin, Judith Ann 11 October 2001 (has links)
No description available.
29

Polyphénols d’agrumes (flavanones) : extraction de glycosides de la peau d’orange, synthèse de métabolites chez l’homme (glucuronides) et étude physico-chimique de leur interaction avec la sérum albumine / Citrus polyphenols (flavanones) : extraction of glycosides from orange peel, synthesis of metabolites (glucuronides) found in human and a physico-chemical study to investigate their interaction with human serum albumin

Khan, Muhammad Kamran 15 November 2010 (has links)
Un groupe d'études épidémiologiques fournit une bonne preuve de la relation inverse associé à la consommation de fruits et légumes et les maladies chroniques important comme maladies cardiovasculaires et certains types de cancers. Après les longues années d'études sur phytomacronutrients, le rôle de phytomicronutrients tels que les polyphénols est désormais très étudiée et appréciée dans le contrôle de ces maladies dégénératives. La présente étude combine les études d'extraction, de synthèse et d'analyse sur les principaux polyphénols des fruits d'agrumes, FLAVANONES. Connaissance de nutritionnels et de santé a augmenté la production d'agrumes en provenance des dernières décennies. Ces productions plus générer des bye-produits. Pour leur utilisation alternative à des antioxydants extraits riches, l'extraction assistée par ultrasons (UAE) des polyphénols en particulier flavanones de l'orange (Citrus sinensis L.) par son peau en utilisant l'éthanol comme solvant de qualité alimentaire a été prouvé son efficacité en comparaison avec la méthode conventionnelle . Un plan composite central (CCD) a révélé que l'approche des conditions optimisées pour UAE ont une température de 40 ° C, une puissance de 150W sonication et un 4:1 (v / v) d'éthanol: ratio de l'eau. En outre, l'activité antioxydante déterminée par les tests DPPH et ORAC a confirmé la pertinence des UAE pour la préparation d'extraits de plantes riches en antioxydants.Les glucuronides de flavanone sont les principaux métabolites phénoliques détectés dans le plasma humain après la consommation d'agrumes. Jusqu'à maintenant, toutes les études sur les cellules liées au cancer ou les maladies cardiovasculaires ont été réalisées soit sur les aglycones ou sur leurs glycosides. Par conséquent, il ya grand besoin de glucuronides flavanone pure pour démontrer le potentiel réel de flavanones dans la prévention de ces maladies. Dans ce travail, glucuronides de naringénine (4'- et 7-O-β-D-glucuronides) et de hespérétine (3'- et 7-O-β-D-glucuronides), les aglycones flavanone majeur dans le pamplemousse et d'orange, respectivement, ont été synthétisés chimiquement par une protection et la déprotection sélective des groupements d'acide glucuronique et de flavanone. La caractérisation structurale complète de composés purifiés a été réalisée par résonance magnétique nucléaire et spectrométrie de masse.L'affinité des quatre glucuronides pour l'albumine sérum d’humaine (HSA) a été testée par leur capacité à éteindre la fluorescence intrinsèque de HSA (Trp, seul résidu de sous-domaine IIA). Leurs constantes de fixation (K) ont été estimées de l'ordre de 30 à 60 × 103 M-1 et comparées à celles de l'aglycones (70 à 90 × 103 M-1). Les enquêtes de la liaison compétitive ou non compétitive de la glucuronides dans la présence de sondes fluorescentes (sarcosine dansyl) nous a permis d'obtenir un aperçu dans les sites de liaison. L'étude a également été étendue aux chalcones hespérétine et naringénine (synthétisés en utilisant des conditions alcalines optimisée), qui sont les précurseurs de biosynthèse des flavanones / A bunch of epidemiological studies provides good evidence on the inverse relationship associated with the consumption of fruits and vegetables and the chronic diseases importantly cardiovascular diseases and some types of cancers. After the long years of study on phytomacronutrients, the role of phytomicronutrients such as polyphenols is now highly studied and appreciated in the control of such degenerative diseases. The present study combines the extraction, synthetic and analytical studies on the major polyphenols of citrus fruits, FLAVANONES.Awareness of nutritional and health facts has increased the production of citrus fruits from last few decades. These higher productions generate higher by-products. For their alternative utilisation to have antioxidants rich extracts, the ultrasound-assisted extraction (UAE) of polyphenols especially flavanones from orange (Citrus sinensis L.) peel by using ethanol as afood grade solvent has been proved its efficiency when compared with the conventional method. A central composite design (CCD) approach revealed that the optimized conditions for UAE were a temperature of 40°C, a sonication power of 150W and a 4:1 (v/v) ethanol:water ratio. Furthermore, the antioxidant activity determined by the DPPH and ORAC tests confirmed the suitability of UAE for the preparation of antioxidant-rich plant extracts. Flavanone glucuronides are the major phenolic metabolites detected in human plasma after consumption of citrus fruits. Up to now all cell studies related to cancer or cardiovascular diseases were conducted either on the aglycones or on their glycosides. Hence, there is great need of pure flavanone glucuronides to demonstrate the real potential of flavanones in the prevention of these diseases. In this work, glucuronides of naringenin (4′- and 7-O-β-D-glucuronides) and hesperetin (3′- and 7-O-β-D-glucuronides), the major flavanone aglycones in grapefruit and orange respectively, have been chemically synthesized by selective protection and deprotection of flavanone and glucuronic acid moieties. The complete structural characterisation of purified compounds were realised by nuclear magnetic resonance and mass spectrometry.The affinity of the four glucuronides for human serum albumin (HSA) was tested via their ability to quench the intrinsic fluorescence of HSA (single Trp residue in sub-domain IIA). Their binding constants (K) were estimated in the range of 30 – 60 × 103 M-1 and compared with those of the aglycones (70 – 90 × 103 M-1). Investigations of competitive or noncompetitive binding of the glucuronides in the presence of fluorescent probes (dansyl sarcosine) allowed us to get some insight in the binding sites. The study was also extended to the hesperetin and naringenin chalcones (synthesised using optimized alkaline conditions), which are the biosynthetic precursors of flavanones
30

Spéciation de l’arsenic dans les produits de la pêche par couplage HPLC/ICP-MS. Estimation de sa bioaccessibilité en ligne et applications à d'autres éléments traces métalliques d'intérêt / Speciation of arsenic in seafood by HPLC/ICP-MS. Estimation of its bioaccessibility online and applications to other trace metallic elements of interest

Leufroy, Axelle 02 April 2012 (has links)
L'arsenic est un élément présent dans tous les compartiments de l'environnement, et les produits de la pêche représentent une source majeure d'exposition à l'arsenic par le biais de l'alimentation. Même s'il n'existe pas à ce jour de législation sur les teneurs en arsenic dans les aliments en France, les agences gouvernementales évaluent généralement les risques liés à la présence d'arsenic dans les produits de la pêche en se basant essentiellement sur la concentration totale de l'élément, sans tenir compte des différentes espèces présentes ni de leur bioaccessibilité. Par conséquent, le développement de méthodes d'analyse de spéciation revêt un intérêt particulier dans le cadre de l'évaluation des risques. La première partie de ce mémoire présente des informations générales sur les propriétés de l'arsenic, son occurrence dans les différents compartiments de l'environnement et sa toxicité, ainsi qu'une étude bibliographique des méthodes analytiques existantes pour étudier la spéciation de l'arsenic dans les matrices alimentaires, en particulier les produits de la pêche (extraction et séparation/détection). Les différentes approches pour l'évaluation de sa bioaccessibilité et de celle d'autres éléments traces métalliques d'intérêt sont également présentées. La deuxième partie de ces travaux porte sur la validation d'une méthode d'analyse de spéciation des principales espèces d'arsenic dans les produits la pêche (As(III), MA,DMA, As(V), AsB, TMAO, AsC) par couplage entre la chromatographie d'échange d'ions (IEC) et la spectrométrie de masse à plasma induit (ICP-MS) après extraction assistée par micro-ondes (MAE). L'évaluation des performances analytiques de la méthode, les contrôles qualités internes et externes mis en place et les différentes applications, en particulier les données d'occurrence des différentes espèces d'arsenic dans les produits de la pêche les plus consommés par la population française sont présentés et discutés. Dans la troisième partie, la bioaccessibilité maximale de l'arsenic et d'autres éléments d'intérêt est estimée à l'aide d'une méthode de lixiviation en ligne (impliquant la mesure en temps réel par ICP-MS de la fraction libérée par les différents fluides digestifs artificiels). La combinaison de ce procédé avec la méthode d'analyse de spéciation validée permet ainsi d'estimer la bioaccessibilité des différentes espèces d'arsenic. / Arsenic is an element present in all compartments of the environment, and seafood constitutes a major source of exposure to arsenic through human consumption. Although there is currently no legislation on arsenic in food in France, government agencies generally assess the safety of food items based solely on the total concentration of the element, without taking into account its different species or their bioaccessibility. Therefore, the development of speciation analysis methods is particularly relevant in the context of risk assessment. The first part of this thesis focuses on the properties of arsenic, its occurrence in the different compartments of the environment and its toxicity, and a literature review of existing analytical methods to study the speciation of arsenic in food matrices, especially seafood products (extraction and separation / detection). Different approaches for evaluating its bioaccessibility and that of other trace metals of interest are also presented.The second part of this work concerns the validation of a speciation analysis method for major arsenic species in seafood (As (III), MA, DMA, As (V), AsB, TMAO, AsC) by coupling ion exchange chromatography (IEC) with inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted extraction (MAE). Evaluation of the analytical performance of the method, internal and external quality controls in place and applications of the method, particularly occurrence data of arsenic species in seafood most consumed by the French population are presented and discussed. In the third part, the maximum bioaccessibility of arsenic and other elements of interest is assessed using a continuous leaching method (involving the real-time measurement by ICP-MS of the fraction released by the different artificial digestive fluids). By coupling this leaching method with the above validated speciation analysis method, the bioaccessibility of different arsenic species is also assessed.

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