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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.
1

Studies on the separation behaviour of nucleotides and oligonucleotides

McKeown, Alan Patrick January 1999 (has links)
No description available.
2

An evaluation of analytical procedures for detection of drug abuse with particular reference to opiates

Low, Ann Stewart January 1998 (has links)
No description available.
3

Stanovení konstant stability komplexů s nabitými cyklodextriny kapilární zónovou elektroforézou / Determination of stability constants of charged cyclodextrine complexes by capillary electrophoresis

Beneš, Martin January 2010 (has links)
Martin Beneš Determination of stability constants of charged cyclodextrin comlexes by capillary electrophoresis Abstract Stability constant characterizes binding interaction between an analyte and complexation agent. These interactions play very important role in separation processes of, in other way undistinguishable, compounds, e.g. enantiomers. The most widely used complexation agents are cyclodextrins. Affinity capillary electrophoresis (ACE) belongs to methods suitable for the determination of stability constants. The stability constant is determined from the dependence of the effective mobility of analyte on the increasing concentration of complexation agent in background electrolyte (BGE). If charged CDs are used, the attention must be paid not only to viscosity of the BGE and to the influence of Joule heating on the temperature in the capillary but also to the increasing ionic strength. The thermodynamic stability constants of R,R- and S,S-hydrobenzoin and R- and S-(3-brom- 2-methyl-1-propanol) with cationic modified β-cyclodextrin: 6-monodeoxy-6-mono(3- hydroxy)propylamino-β-cyclodextrin hydrochlorid (PABCD) were determined by affinity capillary electrophoresis. The average temperature (25řC) of the BGE in the capillary was kept constant. This was achieved by decreasing of the cassette temperature...
4

Evaluation de l’électrophorèse capillaire comme technique d’analyse des antipaludiques retenus dans le schéma thérapeutique ivoirien / Evaluation of capillary electrophoresis as an analytical technique of antimalarial drugs recommended in the ivorian therapeutic protocol

Amin, N'Cho Christophe 09 April 2013 (has links)
La nécessité de garantir la qualité des médicaments antipaludiques disponibles sur le marché pharmaceutique d'Afrique subsaharienne est l'une des stratégies mises en œuvre pour réduire les taux élevés de morbidité et de mortalité liés au paludisme. L'objectif de ce travail de thèse était de proposer des méthodes de dosage par électrophorèse capillaire (EC) de combinaisons antipaludiques à base de sulfadoxine/pyriméthamine (SDX/PYR), artésunate/amodiaquine (AS/AQ) et artéméther/luméfantrine (AM/LUM) retenues dans le schéma thérapeutique ivoirien et commercialisées sous forme de comprimés.Cet objectif a été atteint en employant trois modes de séparation : l'électrophorèse capillaire de zone (CZE) pour SDX/PYR, la chromatographie électrocinétique micellaire (MEKC) pour AS/AQ et la chromatographie électrocinétique par microémulsion (MEEKC) pour AM/LUM. Les méthodes développées ont été validées selon les règles d'ICH et appliquées à des comprimés provenant d'officines ou vendues sur les marchés de rue en Côte d'Ivoire. Elles présentent une répétabilité satisfaisante (CV < 3%, n = 7 procédures analytiques). La méthode de CZE qui utilise un tampon pH 7 pour la séparation de SDX et PYR a donné des résultats de dosage concordants avec la méthode de chromatographie liquide décrite dans l'USP-NF. Sur les neuf formulations de comprimés analysées, une formulation prélevée dans le marché de rue s'est révélée sous-dosée en SDX. La méthode MEKC utilisant le dodécylsulfate de sodium (SDS) dans un tampon borate pH 9,2 a permis le dosage d'AS et AQ. L'application à l'analyse de quatre formulations issues de l'officine a donné des teneurs en AS et AQ conformes aux teneurs déclarées. Enfin, la microémulsion octane-butanol-SDS-tampon borate en MEEKC s'est révélée appropriée au dosage d'AM et LUM, molécule très hydrophobe. L'application à l'analyse de quatre formulations prélevées à l'officine a révélé des teneurs conformes aux teneurs déclarées et la présence dans une formulation d'un ingrédient non déclaré. Le potentiel de screening de cette méthode MEEKC, évalué sur 22 antipaludiques et la sulfaméthoxazole et la triméthoprime, a donné une résolution partielle ou totale pour 17 composés.L'EC peut être utilisée comme technique alternative à la chromatographie liquide pour le contrôle des antipaludiques retenus dans le schéma thérapeutique ivoirien. / The need to ensure the quality of antimalarials available on the pharmaceutical market in sub-Saharan Africa is one of the strategies implemented to reduce the high morbidity and mortality rates associated with malaria. The aim of this thesis was to propose capillary electrophoresis (CE) methods for the determination of combinations of antimalarials containing sulfadoxine/pyrimethamine (SDX/PYR), artesunate/amodiaquine (AS/AQ) and artemether/lumefantrine (AM/LUM) recommended in the Côte d'Ivoire therapeutic protocol and marketed as tablets.The objective was achieved by employing three separation modes: capillary zone electrophoresis (CZE) for SDX/PYR, micellar electrokinetic chromatography (MEKC) for AS/AQ and microemulsion electrokinetic chromatography (MEEKC) for AM/LUM. The developed methods were validated according to ICH rules and were applied to various tablet formulations bought in pharmacies or on the street-market in Côte d'Ivoire. The methods presented satisfactory repeatability values (CV <3%, n = 7 analytical procedures). CZE method used a buffer of pH 7 for the simultaneous separation of SDX and PYR and gave results that were compliant with the dosage by the liquid chromatography method described in the U.S. Pharmacopoeia. Of the nine tablet formulations analyzed, one formulation bought on the street-market had a low SDX content. An MEKC method using SDS in a borate buffer pH 9.2 allowed the determination of AS and AQ in bilayer tablets. Application to four commercial formulations with different dosages gave a content in good agreement with the declared content. Finally, butanol-octane-SDS-borate buffer microemulsion in MEEKC was found to be suitable for the determination of AM and LUM, a very hydrophobic compound. Application to four commercial tablet formulations gave a content in good agreement with the declared content and evidenced the presence in a formulation of an undeclared ingredient. The potential screening capacity of this MEEKC method was evaluated on 22 antimalarials and on sulfamethoxazole and trimethoprim. Partial or complete resolution of 17 compounds was obtained.CE can be used as an alternative technique to liquid chromatography for the control of antimalarial drugs recommended in the national therapeutic protocol against malaria.
5

Separação de fármacos antimaláricos por eletroforese capilar / Separation of antimalarial drugs by capillary electrophoresis

Rodrigues, Karina Trevisan 24 August 2012 (has links)
A malária é a doença que mais mortes causa no mundo. O uso de fármacos antimaláricos representa a solução mais eficaz para o combate e controle da doença e o interesse pelo desenvolvimento de novos fármacos é grande devido a problemas de resistência. Existe uma grande variedade de fármacos antimaláricos, sendo que muitos deles são quirais, vendidos e administrados como mistura racêmica. Nas últimas décadas, houve um aumento no interesse quanto aos aspectos farmacodinâmicos e farmacocinéticos de fármacos quirais, devido ao conhecimento de que um dos isômeros pode ser mais ativo ou mais tóxico que o outro. Sendo assim, tem-se a necessidade do desenvolvimento de métodos analíticos enantiosseletivos, e a eletroforese capilar tem emergido como uma técnica de separação quiral com alto poder de resolução. Além disso, a inexistência de métodos oficiais para fármacos antimaláricos e os poucos estudos que relatam aplicações na análise de formulações farmacêuticas, demandam o desenvolvimento e validação de novos métodos para tal finalidade. Este trabalho tem como objetivo o desenvolvimento de dois métodos analíticos, não quiral e quiral, para a determinação de fármacos antimaláricos em formulações farmacêuticas por eletroforese capilar. O método não quiral utilizou eletroforese capilar de zona, sendo otimizado para a separação de 7 fármacos antimaláricos (cloroquina, hidroxicloroquina, primaquina, quinidina, quinina, quinacrina e mefloquina) com um eletrólito composto por 45 mmol L-1 de tampão citrato, pH 4,50, e apresentou um tempo de análise de 10 minutos, permitindo a separação dos diastereoisômeros quinina e quinidina sem a adição de aditivos. O método quiral utilizou eletroforese capilar de zona modificada por ciclodextrina e foi otimizado para separação enantiosseletiva de cloroquina, mefloquina, hidroxicloroquina, primaquina, quinina e quinidina com um eletrólito composto por 50 mmol L-1 de tampão citrato, e 2% de S-&#946;-CD, pH 2,7. A separação dos fármacos antimaláricos e seus enantiômeros foi alcançada com tempo de análise de 12 minutos. Os métodos desenvolvidos foram validados de acordo com os protocolos oficiais, apresentando características adequadas e foram aplicados na determinação de cloroquina, hidroxicloroquina e mefloquina em formulações farmacêuticas. Como figuras de mérito para o método não quiral, tem-se: linearidade (R2 > 0,99), LD (7,43 - 24,4 &#181;mol L-1), LQ (22,5 - 73,8 &#181;mol L-1), precisão intermediária (0,76 - 1,7% RSD), recuperação (97,8 - 102,2%). Para o método quiral, tem-se: linearidade (R2 > 0,99), LD (7,43 - 9,58 &#181;mol L-1), LQ (22,8 - 29,0 &#181;mol L-1), precisão intermediária (0,50 - 1,8% RSD), recuperação (97,7 - 102,5%). Um ensaio de robustez para ambos os métodos foi realizado para comparar os resultados obtidos aplicando-se pequenas variações de tensão e temperatura. Observou-se que não existe uma diferença significativa entre os resultados, a um nível de confiança de P = 95 %. / Malaria is a disease that causes a large number of deaths worldwide. The use of antimalarial drugs is the most effective solution to combat and control the disease and interest in the development of new antimalarial drugs is still of great importance due to resistance issues. There is a wide variety of antimalarial drugs, many of which are chiral, sold and administered as racemic mixtures. In recent decades there has been an increased interest regarding the pharmacodynamic and pharmacokinetic aspects of chiral drugs, due to the knowledge that one of the isomers can be more active or more toxic than the other. Thus, there is a need for the development of enantioselective analytical methods, and capillary electrophoresis has emerged as a chiral technique separation with high resolving power. Moreover, the lack of official methods for antimalarial drugs and the few studies reporting applications in the analysis of pharmaceutical formulations, demands the development and validation of new methods for this purpose. This work aims at the development of two analytical methods, non-chiral and chiral, for the determination of antimalarial drugs in pharmaceutical formulations by capillary electrophoresis. The non-chiral method used capillary zone electrophoresis, being optimized for the separation of 7 antimalarial drugs (chloroquine, hydroxychloroquine, primaquine, quinidine, quinine, quinacrine and mefloquine) with an electrolyte consisting of 45 mmol L-1 of citrate buffer, pH 4.50, and had an analysis time of 10 minutes, allowing separation of isolated diasteroisomers quinine and quinidine without any additives. The chiral method used capillary zone electrophoresis modified by cyclodextrin and was optimized for enantioselective separation of chloroquine, mefloquine, hydroxychloroquine, primaquine, quinine and quinidine with an electrolyte consisting of 50 mmol L-1 citrate buffer and 2% S-&#946;-CD, pH 2.7. The separation of the antimalarial drugs and their enantiomers was achieved in less than 12 minutes. The proposed methods were validated following official protocols, with adequate results and were used for determination of chloroquine, hydroxychloroquine, and mefloquine in pharmaceutical formulations. Figures of merit for the non-chiral method include: linearity (R2> 0.99), LD (7.43 to 24.4 &#181;mol L-1), LQ (22.5 to 73.8 &#181;mol L-1), intermediary precision (0.76 to 1.7% RSD), and recovery (from 97.8 to 102.2%). For the chiral method, we have: linearity (R2> 0.99), LD (7.43 to 9.58 &#181;mol L-1), LQ (22.8 to 29.0 &#181;mol L-1), intermediary precision (0.50 to 1.8% RSD), and recovery (from 97.7 to 102.5%). For both methods a robustness test was performed to compare the results obtained by applying slight variations in voltage and temperature. It was observed that there is no significant difference between the results, a confidence level P = 95%.
6

Vaistinių arbatų sudėties ir antioksidacinių savybių įvertinimas / Evaluation of composition and antioxidant activity of the functional teas extracts

Zykevičiūtė, Justina 10 August 2009 (has links)
Vaistinės arbatos mišiniai vertingi dėl jose esančių komponentų, kaip fenoliniai junginiai (atsakingi už antimikrobinį veikimą) ir flavonoidai (natūralūs antioksidantai, surišantys laisvuosius radikalus). Flavonoidų cheminės savybės apžvelgtos darbe. Šio darbo tikslas - atlikti flavonoidų ir fenolinių junginių kiekybinę ir kokybinę analizę bei nustatyti bendrą antioksidacinį aktyvumą vaistinių arbatų mišinių ekstraktuose. Paruošti metanoliniai vaistinių arbatų mišinių ekstraktai po kietafazės ekstrakcijos buvo analizuojami spektrofotometru, kapiliarine elektroforeze ir efektyviąja skysčių chromatografija su reakcijos detektoriumi. Spektrofotometru išmatuotas bendras fenolinių junginių, flavonoidų kiekis vaistinėse arbatose. Įvertintos metanolinių ekstraktų laikymo sąlygos šaldytuve bei sausos žaliavos laikymo sąlygos sausoje, vėsioje vietoje. Efektyviąja skysčių chromatografija įvertintas fenolinių junginių kiekis ir jų antioksidacinis aktyvumas su 2,2 - difenil – 1 - pikrilhidrazilo (DPPH ) laisvuoju radikalu. Blukinimo reakcija matuota UV detektoriumi ties 517 nm. Efektyviaja skysčių chromatografija išskirstyti fenoliniai junginiai, taikant gradientą. Atliktas kapiliarinės elektroforezės metodo optimizavimas: įvertintas buferio pH, organinio tirpiklio priedo, įtampos įtaka skirstymo efektyvumui, skiriamajai gebai. Atlikti įteisinimo žingsniai: įvertintos aptikimo ir nustatymo ribos, matavimų glaudumas, stabilumas ir atrankumas. Priedo metodu buvo identifikuoti flavonoidų... [toliau žr. visą tekstą] / Previous studies refer mostly to the HPLC analysis of the flavonoids, for oxidative product deterioration and radicals scavenging action. Methanolic extracts after solid phase extraction of 6 different functional teas were analyzed by means of capillary zone electrophoresis (CZE) and high performence liquid chromatography (HPLC) with reaction detector. A rapid on-line method for screening components was developed using methanolic solution 2,2 – diphenyl – picrylhydrazyl (DPPH) as stable free radical. Bleaching reaction is detected as a negative peak by an absorbance detector at 517 nm. HPLC gradient runs with mobile phase composition ranging from 33 to 90% organic solvent (methanol) in water with 0.1% TFA. The activity of compounds in functional teas (complex mixtures) was determined. Development and validation of the CZE method was carried out.. Limits of detection and quantification were determined. The results obtained using CZE are comparable to the spectrophotometric and HPLC analysis results. The influence of the extraction conditions (with solid phase extraction (SPE) and without SPE extraction), amount of flavonoids and phenolic compounds in the various functional teas was studied. The highest content of flavonoids was obtained in Choleretic herbs mixture 2,08 mg/g and the highest content of phenolic compounds was determined in Diaphoretic functional tea 3,53mg/g in raw dry medicinal functional tea herbs. The total amount of flavonoids did not directly correlate... [to full text]
7

Separação de fármacos antimaláricos por eletroforese capilar / Separation of antimalarial drugs by capillary electrophoresis

Karina Trevisan Rodrigues 24 August 2012 (has links)
A malária é a doença que mais mortes causa no mundo. O uso de fármacos antimaláricos representa a solução mais eficaz para o combate e controle da doença e o interesse pelo desenvolvimento de novos fármacos é grande devido a problemas de resistência. Existe uma grande variedade de fármacos antimaláricos, sendo que muitos deles são quirais, vendidos e administrados como mistura racêmica. Nas últimas décadas, houve um aumento no interesse quanto aos aspectos farmacodinâmicos e farmacocinéticos de fármacos quirais, devido ao conhecimento de que um dos isômeros pode ser mais ativo ou mais tóxico que o outro. Sendo assim, tem-se a necessidade do desenvolvimento de métodos analíticos enantiosseletivos, e a eletroforese capilar tem emergido como uma técnica de separação quiral com alto poder de resolução. Além disso, a inexistência de métodos oficiais para fármacos antimaláricos e os poucos estudos que relatam aplicações na análise de formulações farmacêuticas, demandam o desenvolvimento e validação de novos métodos para tal finalidade. Este trabalho tem como objetivo o desenvolvimento de dois métodos analíticos, não quiral e quiral, para a determinação de fármacos antimaláricos em formulações farmacêuticas por eletroforese capilar. O método não quiral utilizou eletroforese capilar de zona, sendo otimizado para a separação de 7 fármacos antimaláricos (cloroquina, hidroxicloroquina, primaquina, quinidina, quinina, quinacrina e mefloquina) com um eletrólito composto por 45 mmol L-1 de tampão citrato, pH 4,50, e apresentou um tempo de análise de 10 minutos, permitindo a separação dos diastereoisômeros quinina e quinidina sem a adição de aditivos. O método quiral utilizou eletroforese capilar de zona modificada por ciclodextrina e foi otimizado para separação enantiosseletiva de cloroquina, mefloquina, hidroxicloroquina, primaquina, quinina e quinidina com um eletrólito composto por 50 mmol L-1 de tampão citrato, e 2% de S-&#946;-CD, pH 2,7. A separação dos fármacos antimaláricos e seus enantiômeros foi alcançada com tempo de análise de 12 minutos. Os métodos desenvolvidos foram validados de acordo com os protocolos oficiais, apresentando características adequadas e foram aplicados na determinação de cloroquina, hidroxicloroquina e mefloquina em formulações farmacêuticas. Como figuras de mérito para o método não quiral, tem-se: linearidade (R2 > 0,99), LD (7,43 - 24,4 &#181;mol L-1), LQ (22,5 - 73,8 &#181;mol L-1), precisão intermediária (0,76 - 1,7% RSD), recuperação (97,8 - 102,2%). Para o método quiral, tem-se: linearidade (R2 > 0,99), LD (7,43 - 9,58 &#181;mol L-1), LQ (22,8 - 29,0 &#181;mol L-1), precisão intermediária (0,50 - 1,8% RSD), recuperação (97,7 - 102,5%). Um ensaio de robustez para ambos os métodos foi realizado para comparar os resultados obtidos aplicando-se pequenas variações de tensão e temperatura. Observou-se que não existe uma diferença significativa entre os resultados, a um nível de confiança de P = 95 %. / Malaria is a disease that causes a large number of deaths worldwide. The use of antimalarial drugs is the most effective solution to combat and control the disease and interest in the development of new antimalarial drugs is still of great importance due to resistance issues. There is a wide variety of antimalarial drugs, many of which are chiral, sold and administered as racemic mixtures. In recent decades there has been an increased interest regarding the pharmacodynamic and pharmacokinetic aspects of chiral drugs, due to the knowledge that one of the isomers can be more active or more toxic than the other. Thus, there is a need for the development of enantioselective analytical methods, and capillary electrophoresis has emerged as a chiral technique separation with high resolving power. Moreover, the lack of official methods for antimalarial drugs and the few studies reporting applications in the analysis of pharmaceutical formulations, demands the development and validation of new methods for this purpose. This work aims at the development of two analytical methods, non-chiral and chiral, for the determination of antimalarial drugs in pharmaceutical formulations by capillary electrophoresis. The non-chiral method used capillary zone electrophoresis, being optimized for the separation of 7 antimalarial drugs (chloroquine, hydroxychloroquine, primaquine, quinidine, quinine, quinacrine and mefloquine) with an electrolyte consisting of 45 mmol L-1 of citrate buffer, pH 4.50, and had an analysis time of 10 minutes, allowing separation of isolated diasteroisomers quinine and quinidine without any additives. The chiral method used capillary zone electrophoresis modified by cyclodextrin and was optimized for enantioselective separation of chloroquine, mefloquine, hydroxychloroquine, primaquine, quinine and quinidine with an electrolyte consisting of 50 mmol L-1 citrate buffer and 2% S-&#946;-CD, pH 2.7. The separation of the antimalarial drugs and their enantiomers was achieved in less than 12 minutes. The proposed methods were validated following official protocols, with adequate results and were used for determination of chloroquine, hydroxychloroquine, and mefloquine in pharmaceutical formulations. Figures of merit for the non-chiral method include: linearity (R2> 0.99), LD (7.43 to 24.4 &#181;mol L-1), LQ (22.5 to 73.8 &#181;mol L-1), intermediary precision (0.76 to 1.7% RSD), and recovery (from 97.8 to 102.2%). For the chiral method, we have: linearity (R2> 0.99), LD (7.43 to 9.58 &#181;mol L-1), LQ (22.8 to 29.0 &#181;mol L-1), intermediary precision (0.50 to 1.8% RSD), and recovery (from 97.7 to 102.5%). For both methods a robustness test was performed to compare the results obtained by applying slight variations in voltage and temperature. It was observed that there is no significant difference between the results, a confidence level P = 95%.
8

Desenvolvimento de um método para determinação de ácidos orgânicos em sucos de frutas utilizando Eletroforese Capilar de Zona (ECZ) / DEVELOPMENT OF A METHOD FOR DETERMINATION OF ORGANIC ACIDS IN FRUIT JUICES USING CAPILLARY ZONE ELECTROPHORESIS (ECZ)

Carvalho, José Marcos Valentim de 09 March 2010 (has links)
An electrophoretic methodology with UV detection was developed for determinations the main organic acids contained in fresh fruit juice and industrialized fruits juices produced in Sergipe/Brazil and sold in markets and supermarkets of Lagarto, Itabaiana and Aracaju. Oxalic, tartaric, citric, gallic and ascorbic (L aa) organic acids were separate and quantified in grape, orange, lemon, carambola, umbu-caja, acerola, cashew, strawberry samples of fresh juices and samples of mixed juice industrialized (mixed acerola, orange, fortified whit L aa; mixed apple, orange, tangerine and lemon; mixed orange, lemon and tangerine; guava juice and mixed apple, lemon and grape). The analyses were made employing BGE containing 100 mmol/L borate buffer pH 10.0 and 0.5 mmol/L cetyl trimethyl ammonium bromide (CTAB) as EOF-modifier, a fused silica capillary of 59 cm of length (23.7 cm effective, 75 mm of i.d.) = 214 nm. The sample injection was made in hydrodynamic mode (height 4.5 cm) for 15 s, the method was linear within 0.0040 to 0.0450 g/100mL. The calibration curves were prepared with the addition of external standard, with correlation coefficient from 0.9912 to 0.9995, the precision ranged of 1.48 to 11.46% (n= 3). The limit of detection varied from 0.0005 to 0.0155 g/100mL and the limit of quantification varied from 0.0016 to 0.0517 g/100mL. The recoveries in samples of fresh juices were 83.6 to 117.5% (n = 50) and from 83.60 to 108.7% (n=11) for the acids in fruits juices industrialized samples. The oxalic, tartaric, citric, and L aa were separated and quantified in samples of fresh juices while citric and L aa acid in samples of industrialized juices there was reduction in the concentration of 18.90%, 28.20% and 36.00% L - aa of juices of fresh acerola, orange and cashew respectively and of 100.0%, 99.40% in samples of mixed juice industrialized, mixed apple, orange, tangerine and lemon, mixed acerola, orange, fortified whit L aa respectively, was also reduction the concentration of citric acid in two samples juice industrialized 15,20% in mixed apple juice, orange, tangerine, lemon and 56,9% in guava juice. The proposed method is rapid and sensitive and can be used to analysis of organic acids in juice fruit samples. / Uma metodologia eletroforética com detecção no UV foi desenvolvida para determinação dos ácidos orgânicos contidos em sucos de frutas frescos e em sucos de frutas industrializados produzidos em Sergipe/Brasil e comercializados nos mercados e supermercados de Lagarto, Itabaiana e Aracaju. Os ácidos orgânicos: oxálico, tartárico, cítrico e o ácido ascórbico (L aa) foram separados e quantificados em amostras de sucos frescos de uva, laranja, limão, carambola, umbu-cajá, acerola, caju, morango e em amostras de sucos industrializados (misto de acerola, laranja fortificado com L aa; misto de maçã, laranja, tangerina e limão; misto de laranja, limão e tangerina; suco de goiaba e misto de maçã, limão e uva). As análises foram realizadas empregando uma solução tampão contendo 100 mmol/L de tampão borato pH 10,0 e 0,5 mmol/L de brometo de cetiltrimetilamônio (CTAB) como inversor do fluxo eletroosmótico, um capilar de sílica fundida de 59 cm de comprimento (23,7cm efetivo, 75 μm de d.i.) e detecção a l=214nm. A injeção da amostra foi feita no modo hidrodinâmico (altura de 4,5 cm) por 15 s. O método mostrou-se linear numa faixa de 0,0040 a 0,0450 g/100 mL, as curvas de calibração foram preparadas com adição de padrão externo, com coeficiente de correlação de 0,9912 a 0,9995, a precisão variou de 1,48 a 11,46% (n = 3), o limite de detecção variou de 0,0005 - 0,0155 g/100mL e o de quantificação 0,0016 - 0,0517 g/100 mL. As recuperações dos ácidos nas amostras de sucos frescos variaram de 83,60 a 117,5% (n = 50), e de 83,60 a 108,7% (n=11) para os ácidos nas amostras de sucos industrializados. Os ácidos, oxálico, tartárico, cítrico e L aa foram separados e quantificados nas amostras de sucos frescos, enquanto que os ácidos, cítrico e L aa, nas amostras de sucos industrializados, sendo que houve redução na concentração do ácido ascórbico de 18,90%, 28,20% e 36,00% nos sucos frescos de acerola, laranja e caju respectivamente, e de 100,0% no suco industrializado misto de maça, laranja, tangerina, limão e 99,40% no suco industrializado misto de acerola, laranja enriquecido com L aa, houve também redução na concentração do ácido cítrico em duas amostras de sucos industrializados, 15,20% e 56,90% nos sucos, misto de maçã, laranja, tangerina, limão, e no de goiaba. O método desenvolvido foi rápido, sensível e adequado para análise de ácidos orgânicos em amostras de sucos de frutas.
9

Účetní výkazy dle IFRS a jejich srovnání s českými účetními předpisy / Financial statements according to IFRS and their comparison with Czech accounting legislation

Tereščenko, Dmytro Oleksandrovyč January 2009 (has links)
The main objective of the final thesis is to emphasise the transformation of financial statements prepared according to Czech accounting legislation to financial statements prepared in accordance with International Financial Reporting Standards. There are two parts in the final thesis. The first part describes a complete set of financial statements, prepared in accordance with International Financial Reporting Standards, it is an obligatory part of the financial statements - Statement of financial position, Statement of comprehensive income, Statement of changes in equity, Statement of cash flows, summary of significant accounting policies, and other explanatory notes. The second part of the final thesis deals with an accuracy of the transfer Leases, Provisions and Deferred Taxes on Czech accounting legislation to International Financial Reporting Standards.
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Využití hmotnostní spektrometrie a dalších analytických technik pro analýzu rheniových komplexů / Utilization of mass spectrometry and other analytical techniques for analysis of rhenium complexes

Vaňátková, Petra January 2016 (has links)
Rhenium complexes coordinated with suitable organic ligand gain increased interest in radiopharmaceutical medicine. Besides suitable radiological properties given by a metal ion itself, detailed knowledge of overall chemical properties of formed complexes, namely their exact structures, chemical stabilities and possible degradation pathways are essential pre-requisites for their clinical application. Selected rhenium complexes with pyrogallol 2,3-dihydroxynaphthalene and catechol as strongly bound ligands were prepared by a reaction of tetrabutylammonium tetrachlorooxorhenate with twofold molar excess of ligand in presence of various amount of triethylamine. The structures of formed complexes and their consequent reaction products were estimated by means of mass spectrometry with electrospray ionization. The kinetics of reactions in course of complex formation and consequent decomposition were primarily followed by UV- Vis absorption spectra measurement, complemented by single or continuous electrospray mass spectrometry analyses. Optimized HPLC and CZE procedures were utilized for monitoring of the composition of reaction mixtures in course of Re complex formation and for purity check of prepared complexes. Semi-preparative HPLC mode was succesfully utilized for isolation and final purification of...

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