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A fatal forensic intoxication with fenarimol: analysis by HPLC/DAD/MSD

Proença, P.; Marques, E. Pinho; Teixeira, H.; Castanheira, F.; Barroso, M.; Ávila, S.; Vieira, D. N.
Fonte: Universidade de Coimbra Publicador: Universidade de Coimbra
Tipo: Artigo de Revista Científica Formato: aplication/PDF
ENG
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46.44%
Fenarimol (Rubigan®) is a pyrimidine ergosterol biosynthesis inhibitor used as a systemic fungicide. The authors present a fatal fenarimol intoxication case analysed in the Forensic Toxicology Service of the National Institute of Legal Medicine. The results were used to compare two different HPLC techniques, regarding selectivity and sensitivity: an HPLC system with a diode array detector (DAD) and an HPLC system with a DAD and a mass spectrometry detector (MSD) with an electrospray interface. All biological samples were submitted to a solid-phase extraction procedure. The detection and quantification limits of fenarimol, linearity, precision and accuracy were evaluated. The fenarimol concentration levels determined were of 89.0 mg/ml in gastric contents, 1.9 mg/g in liver and 0.4 mg/g in kidney. Blood was not available at autopsy. No published data related to fenarimol self-poisoning were found, so it was not possible to interpret the results obtained by comparison with toxic/lethal levels.; http://www.sciencedirect.com/science/article/B6T6W-488NYVD-R/1/712bf23bb727a7110f22a36460ab32fb

Cultivar influence on carotenoid composition of loquats from Brazil

FARIA, Adelia Ferreira de; HASEGAWA, Patricia N.; CHAGAS, Edvan Alves; PIO, Rafael; PURGATTO, Eduardo; MERCADANTE, Adriana Z.
Fonte: ACADEMIC PRESS INC ELSEVIER SCIENCE Publicador: ACADEMIC PRESS INC ELSEVIER SCIENCE
Tipo: Artigo de Revista Científica
ENG
Relevância na Pesquisa
46.57%
Cultivar, growing conditions and geographical origin are factors that influence the carotenoid composition in fruits. Because the loquat cultivars evaluated in this study, CentenAria, Mizauto, Mizuho, Mizumo and Nectar de Cristal, have not previously been investigated, the present work was carried out to determine and compare the carotenoid composition of these five loquat cultivars, by applying high-performance liquid chromatography connected to a photodiode array and mass spectrometry detectors (HPLC-PDA-MS/MS). Twenty-five carotenoids were separated on a C(30) column, and 23 of them were identified. All-trans-beta-carotene (19-55%), all-trans-beta-cryptoxanthin (18-28%), 5,6:5`,6`-diepoxy-beta-cryptoxantilin (9-18%) and 5,6-epoxy-beta-cryptoxanthin (7-10%) were the main carotenoids. The total carotenoid content ranged from 196 mu g/100 g (cv. Nectar de Cristal) to 3020 mu g/100 g (CV. Mizumo). The carotenoid profile of cv. Nectar de Cristal was different from the other cultivars, which was in agreement with its cream pulp colour, in contrast to the other four cultivars with orange pulp colour. Cultivars Mizauto, Mizuho, Mizumo and CentenAria showed provitamin A values between 89 and 162 mu g RAE/100 g, and can be considered good source of this provitamin. (C) 2009 Elsevier Inc. All rights reserved.; Brazilian Funding Agencies FAPESP (Fundacao de Amparo a Pesquisa do Estado de Sao Paulo); CAPES (Coordenacao de Aperfeicoamento de Pessoal de Nivel Superior)

Investigação do perfil químico de esponjas do gênero Aplysina por LC-PDA-MS; Investigation of the chemical profile of sponges of the genus Aplysina by LC-PDA-MS

Silva, Michelli Massaroli da
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Dissertação de Mestrado Formato: application/pdf
Publicado em 05/03/2009 PT
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57.03%
Esponjas do gênero Aplysina (Ordem: VERONGIDA) são conhecidas por apresentarem em seu metabolismo secundário compostos derivados da dibromotirosina, os quais são um importante aliado para o processo de identificação dessas esponjas. Este trabalho descreve o estudo do perfil químico de 14 espécimens de esponjas do gênero Aplysina, coletadas na Bahia de Todos os Santos-BA, no ano de 2007. Também foi desenvolvida uma metodologia de desreplicação, utilizando-se da técnica hifenada HPLC-PDA-MS(ESI), busca na literatura (MarinLit) e comparação com padrões. Os resultados obtidos demonstram claramente que essas esponjas apresentam os derivados da dibromotirosina e que a metodologia de desreplicação permitiu confirmar e/ou prever possíveis estruturas desses compostos com eficiência e sem a necessidade do seu isolamento. Entretanto, não foi possível distinguir as espécies dos organismos estudados através do seu perfil químico, uma vez que eles apresentaram praticamente os mesmos metabólitos em todas as frações analisadas. Isto demonstra que a classificação taxonômica em nível de espécie requer, necessariamente, a análise do esqueleto (espículas) das esponjas e possivelmente análises genômicas. A análise das frações aquosas permitiu apenas confirmar a presença desses derivados através da análise das absorções típicas no espectro de UV. Também...

Otimização das condições de produção microbiológica de destruxinas por Beauveria felina; Optimal conditions for the microbial production of destruxins by Beauveria felina

Urano, Raquel Peres de Morais
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Tese de Doutorado Formato: application/pdf
Publicado em 21/10/2010 PT
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46.48%
O fungo entomopatogênico Beauveria felina produz as destruxinas, hexadepsipeptídeos cíclicos que apresentam diversas atividades biológicas, como por exemplo: atividade inseticida, fitotóxica, citotóxica contra células tumorais, atividade antiviral contra o vírus da hepatite B, dentre outras. Devido à atividade inseticida das destruxinas, os fungos que as produzem têm grande importância econômica. Assim, o objetivo deste trabalho foi realizar a otimização das condições de crescimento e produção das destruxinas pelo fungo Beauveria felina utilizando diferentes meios de cultivo, a fim de se isolar destruxinas em maiores quantidades para a avaliação de seu potencial tóxico. Foram utilizados métodos de planejamento experimental e análise multivariada para a otimização das condições de crescimento, resultando em três condições ótimas de cultivo para cada um dos meios de cultura MF, PDB e SBD. Em todas as condições ótimas de cultivo foram observadas destruxinas conhecidas, desconhecidas e destruxinas que não foram isoladas anteriormente de Beauveria felina. O cultivo de Beauveria felina no meio PDB foi o que mais apresentou destruxinas desconhecidas (5). Em seguida foi realizada uma otimização das condições de análise cromatográfica de destruxinas por CLAD-DAD-DELE-EM e a validação deste método. Uma das frações obtidas do meio de cultura de Beauveria felina apresentou atividade vermífuga contra Haemonchus contortus. Duas de suas frações purificadas...

Cultivar influence on carotenoid composition of loquats from Brazil

FARIA, Adelia Ferreira de; HASEGAWA, Patricia N.; CHAGAS, Edvan Alves; PIO, Rafael; PURGATTO, Eduardo; MERCADANTE, Adriana Z.
Fonte: ACADEMIC PRESS INC ELSEVIER SCIENCE Publicador: ACADEMIC PRESS INC ELSEVIER SCIENCE
Tipo: Artigo de Revista Científica
ENG
Relevância na Pesquisa
46.48%
Cultivar, growing conditions and geographical origin are factors that influence the carotenoid composition in fruits. Because the loquat cultivars evaluated in this study, CentenAria, Mizauto, Mizuho, Mizumo and Nectar de Cristal, have not previously been investigated, the present work was carried out to determine and compare the carotenoid composition of these five loquat cultivars, by applying high-performance liquid chromatography connected to a photodiode array and mass spectrometry detectors (HPLC-PDA-MS/MS). Twenty-five carotenoids were separated on a C(30) column, and 23 of them were identified. All-trans-beta-carotene (19-55%), all-trans-beta-cryptoxanthin (18-28%), 5,6:5`,6`-diepoxy-beta-cryptoxantilin (9-18%) and 5,6-epoxy-beta-cryptoxanthin (7-10%) were the main carotenoids. The total carotenoid content ranged from 196 mu g/100 g (cv. Nectar de Cristal) to 3020 mu g/100 g (CV. Mizumo). The carotenoid profile of cv. Nectar de Cristal was different from the other cultivars, which was in agreement with its cream pulp colour, in contrast to the other four cultivars with orange pulp colour. Cultivars Mizauto, Mizuho, Mizumo and CentenAria showed provitamin A values between 89 and 162 mu g RAE/100 g, and can be considered good source of this provitamin. (C) 2009 Elsevier Inc. All rights reserved.; Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP); Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Isolation and quantitative HPLC-PDA analysis of lupeol in phytopharmaceutical intermediate products from Vernonanthura ferruginea (Less.) H. Rob.

Oliveira,Ezequiane Machado Silva; Freitas,Sabrine Lemes; Martins,Frederico Severino; Couto,Renê Oliveira; Pinto,Mariana Viana; Paula,José Realino; Conceição,Edemilson Cardoso; Bara,Maria Teresa Freitas
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/01/2012 EN
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46.48%
Prior to obtain a standardized dried extract from V. ferruginea, lupeol was first time isolated from leaves and used as chemical maker. An analytical method using HPLC-PDA for lupeol determination in V. ferruginea intermediate products was developed using a C8 reverse-phase column, acetonitrile-acetic acid (99.99:0.01, v/v) as mobile phase at 0.8 mL min-1, oven temperature at 23-25 ºC, sample injection volume at 30 µL and detection at 210 nm. The method presented linearity from 10 to 160 µg mL-1, accuracy, precision, robustness and suitable sensitivity proving to be a useful tool to the obtainment process of lupeol standardized dried extracts of V. ferruginea.

Justicia pectoralis Jacq: , Acanthaceae: preparation and characterisation of the plant drug including chromatographic analysis by HPLC-PDA

Fonseca,Francisco N.; Silva,Aline Holanda; Leal,Luzia K. A. M.
Fonte: Sociedade Brasileira de Farmacognosia Publicador: Sociedade Brasileira de Farmacognosia
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/12/2010 EN
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66.69%
Justicia pectoralis Jacq., Acanthaceae, is a herb popularly known in Brazilian northeast as "chambá" and used in folk medicine for the treatment of respiratory tract conditions such as asthma, cough and bronchitis. This species is included in the National Register of Plants of Interest to the National Health System. The aim of the present study was to develop a protocol for the preparation of the plant drug from J. pectoralis and to characterise the plant drug for its use as a pharmaceutical raw material. The aerial parts of J. pectoralis, after drying chamber with forced air circulation (35 °C) for different periods of time (1-5 days), presented after one day a moisture content below the maximum allowed for plant drugs. The powder of the plant drug was classified as moderately coarse, and the total ashes content and the water- or ethanol-soluble extractives were determined. Analysis of hydroalcoholic (ethanol 20%) extract of J. pectoralis by high performance liquid chromatography-photo diode array (HPLC-PDA) determined the content of coumarin and umbelliferone (16.2 and 0.81 mg/g plant drug, respectively). The preparation conditions of the plant drug and the quality control parameters established for J. pectoralis in this study are of interest for the development of phytomedicines which use this active raw material.

Study of the Specificity of Cross-Povidone (PVPP) as binding agent in the quantification of polyphenolic compounds

Verza,Simone G.; Pavei,Cabral; Ortega,George G.
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/01/2008 EN
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46.69%
Cross-povidone, or polyvinylpyrrolidone (PVPP) affords an analytical alternative instead of hide-powder and casein as binding agent in the content assay of vegetable tannins. In this work we studied the specificity of PVPP to bind polyphenolics in the presence of flavonoids. Gallic acid, tannic acid, catechin and pyrogallol were used as polyphenolic reference substances (PRS), along with an aqueous extract from Psidium guajava L. leaves. The binding specificity was assayed by UV-Vis and High Performance Liquid Chromatography-Photodiode array (HPLC-PDA) methods. The analyses of PRS-rutin mixtures showed clearly that PVPP binding is a non-specific reaction, unrelated to the amount of PVPP used. HPLC-PDA analysis revealed peaks which could be characterized as flavonoids in the Psidium guajava extract, beside catechin and gallic acid. All these flavonoids, catechin and gallic acid peaks decreased as PVPP was added; this confirms the lack of specificity. Since the polyphenolic-PVPP reaction depends on specific structural features, any extensive conclusion should be avoided.

A method for dextruxin analysis by HPLC-PDA-ELSD-MS

Morais,Raquel P.; Lira,Simone P.; Seleghim,Mirna H. R.; Berlinck,Roberto G. S.
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/12/2010 EN
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46.5%
Destruxins (Dtx) are cyclodepsipeptides produced by enthomopathogenic fungi, which are used in biological control of different agricultural insect plagues. The present investigation reports a new approach for analysis of destruxins produced by the fungal strain Beauveria felina, using LC-PDA-ELSD-MS. Compared to previous methods, the new approach uses a clean-up on C18 cartridges, which effectively removes growth media constituents. Moreover, the use of 50:50 (v/v) MeCN/MeOH as the strongest eluting solvent in a gradient system over 0.1% H2O proved to give a better resolution of chromatographic peaks. Simultaneous detection using photodiode array (PDA), evaporative light scattering detector (ELSD) and mass spectrometry (MS) indicated a practically identical response of all detectors for destruxins analysis. Five samples obtained from the culture media of B. felina were analysed, and indicated the presence of twenty known destruxins and six yet unreported cyclodepsipeptides. Considering the reduced use of MeCN, and the effectiveness of ELSD as a detector for destruxins, the method proved to be valuable and cost-effective for quality control analysis of destruxin-producing fungal strains.

1H NMR-based metabolomics combined with HPLC-PDA-MS-SPE-NMR for investigation of standardized Ginkgo biloba preparations

Agnolet, Sara; Jaroszewski, Jerzy W.; Verpoorte, Robert; Staerk, Dan
Fonte: Springer US Publicador: Springer US
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
46.48%
Commercial preparations of Ginkgo biloba are very complex mixtures prepared from raw leaf extracts by a series of extraction and prepurification steps. The pharmacological activity is attributed to a number of flavonoid glycosides and unique terpene trilactones (TTLs), with largely uncharacterized pharmacological profiles on targets involved in neurological disorders. It is therefore important to complement existing targeted analytical methods for analysis of Ginkgo biloba preparations with alternative technology platforms for their comprehensive and global characterization. In this work, 1H NMR-based metabolomics and hyphenation of high-performance liquid chromatography, photo-diode array detection, mass spectrometry, solid-phase extraction, and nuclear magnetic resonance spectroscopy (HPLC-PDA-MS-SPE-NMR) were used for investigation of 16 commercially available preparations of Ginkgo biloba. The standardized extracts originated from Denmark, Italy, Sweden, and United Kingdom, and the results show that 1H NMR spectra allow simultaneous assessment of the content as well as identity of flavonoid glycosides and TTLs based on a very simple sample-preparation procedure consisting of extraction, evaporation and reconstitution in acetone-d6. Unexpected or unwanted extract constituents were also easily identified in the 1H NMR spectra...

Identification and determination of major constituents in a traditional Chinese medicine compound recipe Xiongdankaiming tablet using HPLC-PDA/ESI-MSn and HPLC-UV/ELSD* #

Wang, Shu-fang; Leng, Jing; Xu, Yi-min; Feng, Mei-ling
Fonte: Zhejiang University Press Publicador: Zhejiang University Press
Tipo: Artigo de Revista Científica
Publicado em /07/2013 EN
Relevância na Pesquisa
46.7%
Xiongdankaiming tablet (XDKMT), a well-known compound in traditional Chinese medicine, is widely used for the treatment of acute iridocyclitis and primary open-angle glaucoma. In this paper, accurate and reliable methods were developed for the identification of 20 constituents using high-performance liquid chromatography with photo-diode array and electron spray ionization-mass spectrometry (HPLC-PDA/ESI-MSn), and determination of nine of the constituents (chlorogenic acid, gentiopicroside, isochlorogenic acid B, diosmetin-7-O-β-D-glucopyranoside, apigenin, diosmetin, tauroursodeoxycholic acid, acacetin, and taurochenodeoxycholic acid) was developed using HPLC with ultraviolet absorption detector and evaporative light scattering detector (HPLC-UV/ELSD) for the first time. The best results were obtained on a Zorbax SB-C18 column with gradient elution using water (0.1% formic acid) (A) and methanol (0.1% formic acid) (B) at a flow rate of 0.7 ml/min. Tauroursodeoxycholic acid and taurochenodeoxycholic acid, owing to their low UV absorption, were detected by ELSD. The other seven compounds were analyzed by HPLC-UV with variable wavelengths. The calibration curves of all nine constituents showed good linear regression (R 2>0.9996) within the linearity ranges. The limits of detection and quantification were in the ranges of 0.0460–9.90 μg/ml and 0.115–24.8 μg/ml...

Resveratrol-Loaded Polymeric Nanoparticles: Validation of an HPLC-PDA Method to Determine the Drug Entrapment and Evaluation of Its Antioxidant Activity

da Rocha Lindner, Gabriela; Khalil, Najeh Maissar; Mainardes, Rubiana Mara
Fonte: Hindawi Publishing Corporation Publicador: Hindawi Publishing Corporation
Tipo: Artigo de Revista Científica
Publicado em 24/10/2013 EN
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36.6%
Poly(lactic acid) (PLA) and PLA-poly(ethylene glycol) (PLA-PEG) nanoparticles containing resveratrol (RVT) were developed, and their antioxidant activity was evaluated. An analytical method using high performance liquid chromatography (HPLC)/photodiode array (PDA) detection was also developed and validated for RVT determination in nanoparticles. The mobile phase consisted of methanol : water (51 : 49, v/v) flowed at 0.9 mL/min, and the PDA detector was set at wavelength of 306 nm. The mean diameter of the nanoparticles varied between 180 and 220 nm, and the encapsulation efficiency of RVT ranged from 60% to 88%. The nanoparticles containing RVT were evaluated for their ability to scavenge the radical (2,2-azinobis (3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt) (ABTS•+). The profile obtained from the PLA nanoparticles containing RVT demonstrated that after 24 h, there was almost no increase in antioxidant activity, which was lower than that of the free RVT and RVT-loaded PLA-PEG nanoparticles. For PLA-PEG nanoparticles, the radical-scavenging activity of RVT was shown to increase with time, and after 48 h, it was similar to that observed with free RVT.

Correction: Determining the degradation efficiency and mechanisms of ethyl violet using HPLC-PDA-ESI-MS and GC-MS

Lu, Chung-Shin; Lin, Wan-Yu; Wang, Jian-Xun; Wu, Chia-Wei; Chen, Chiing-Chang
Fonte: BioMed Central Publicador: BioMed Central
Tipo: Artigo de Revista Científica
Publicado em 17/04/2014 EN
Relevância na Pesquisa
46.48%
This is a correction to the following paper: Determining the degradation efficiency and mechanisms of ethyl violet using HPLC-PDA-ESI-MS and GC-MS, Wen-Hsin Chung, Chung-Shin Lu, Wan-Yu Lin, Jian-Xun Wang, Chia-Wei Wu, Chiing-Chang Chen, Chemistry Central Journal 2012, 6:63 (30 June 2012).

Hepatoprotective and Antioxidant Effect of Bauhinia hookeri Extract against Carbon Tetrachloride-Induced Hepatotoxicity in Mice and Characterization of Its Bioactive Compounds by HPLC-PDA-ESI-MS/MS

Al-Sayed, Eman; Martiskainen, Olli; Seif el-Din, Sayed H.; Sabra, Abdel-Nasser A.; Hammam, Olfat A.; El-Lakkany, Naglaa M.; Abdel-Daim, Mohamed M.
Fonte: Hindawi Publishing Corporation Publicador: Hindawi Publishing Corporation
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
46.48%
The hepatoprotective and antioxidant activity of Bauhinia hookeri ethanol extract (BHE) against CCl4-induced liver injury was investigated in mice. BHE was administered (500 and 1000 mg/kg/day) along with CCl4 for 6 weeks. The hepatic marker enzymes: alanine aminotransferase (ALT), aspartate aminotransferase (AST), and alkaline phosphatase (ALP) were determined in the serum. The antioxidant parameters: glutathione (GSH), superoxide dismutase (SOD), glutathione peroxidase (GPx), glutathione reductase (GR), glutathione transferase (GST), and malondialdehyde (MDA) were estimated in the liver homogenate. BHE treatment significantly inhibited the CCl4-induced increase in ALT (44 and 64%), AST (36 and 46%), ALP (28 and 42%), and MDA (39 and 51%) levels at the tested doses, respectively. Moreover, BHE treatment markedly increased the activity of antioxidant parameters GSH, GPx, GR, GST, and SOD. Histological observations confirmed the strong hepatoprotective activity. These results suggest that a dietary supplement of BHE could exert a beneficial effect against oxidative stress and various liver diseases by enhancing the antioxidant defense status, reducing lipid peroxidation, and protecting against the pathological changes of the liver. The hepatoprotective activity of BHE is mediated...

Identification of Chemical Constituents in the Extract and Rat Serum from Ziziphus Jujuba Mill by HPLC-PDA-ESI-MSn

Wang, Shuping; Zhang, Jingze; Zhang, Zhidan; Gao, Wenyuan; Yan, Yanan; Li, Xia; Liu, Changxiao
Fonte: Shaheed Beheshti University of Medical Sciences Publicador: Shaheed Beheshti University of Medical Sciences
Tipo: Artigo de Revista Científica
Publicado em //2014 EN
Relevância na Pesquisa
46.48%
Chinese jujube (Ziziphus jujuba Mill.) has long been widely used for human consumption and medicinal purposes in China. It has been reported to possess several vital biological activities. However, the systematic study on the chemical constituents absorbed into plasma and their metabolites is still insufficient.A high-performance liquid chromatography-photodiode array detector-electrospray ionization ion-mass spectrometry (HPLC-PDA-ESI-MSn) method was established to analyze the ethanol extract in Ziziphus jujuba Mill and the constituents absorbed into rat serum. In the present study, a dose of 10 mL/Kg of ethanol extract of jujube, which is equivalent to 12.5 g crude dried herb/Kg, was orally administrated to rats. The main components were analyzed in the ethanol extract of Ziziphus jujuba Mill and the parent constituents and metabolites were studied in rat plasma samples after oral administration of the ethanol extract of jujube.D101 macroporous polystyrene resin was a good pretreatment method to obtain better separation and impurity removal effect. Twenty-two compounds were identified in the ethanol extract of Ziziphus jujuba Mill. Four parent compounds and four metabolites were detected in rat serum. Among them, seventeen compounds were reported for the first time.

Desenvolvimento e validação de metodologia por HPLC-PDA para monitoração terapêutica dos níveis plasmáticos de zidovudina e efavirenz; Development and validation of methodology for HPLC-PDA for therapeutic monitoring of plasma levels of zidovudine and efavirenz

SOARES, Amanda Queiroz
Fonte: Universidade Federal de Goiás; BR; UFG; Mestrado em Ciências da Saúde; Ciências da Saúde - Medicina Publicador: Universidade Federal de Goiás; BR; UFG; Mestrado em Ciências da Saúde; Ciências da Saúde - Medicina
Tipo: Dissertação Formato: application/pdf
POR
Relevância na Pesquisa
36.63%
The therapeutic drug monitoring is an important tool to predict the therapeutic efficacy and possible toxicity of antirretroviral agents used to treat infection by human immunodeficiency virus (HIV). The goals of this study was to develop and validate a method of analysis and extraction to quantify the antirretrovirals efavirenz and zidovudine in human plasma, to know the clinical profile and quantify the drugs efavirenz and zidovudine in plasma of volunteers using treatment regimen efavirenz / lamivudine / zidovudine. Blood samples were collected approximately 8 h after administration of AZT and 20 h of the EFZ, were obtained from adult volunteers HIV positive in clinic monitoring at Hospital das Clínicas, Universidade Federal de Goiás and therapeutic protocol EFZ 600 mg once daily and lamivudine 150 mg + zidovudine 300 mg twice a day. After solid phase extraction using cartridge Strata 18E C 500mg, 3 mL capacity, the drugs and internal standard (5 - (4-methylphenyl)-5-fenilidantoína - MPPH) were separated by reversed-phase column ACE 5 C18 100 x 4 6 mm. The mobile phase consisted of acetonitrile and diethanolamine in water (pH 7.8), flow rate 0.5 to 2.0 mL/min and detection at wavelength of 249 nm (EFZ), 267 nm (AZT) and 240 nm (MPPH). The method showed linearity at concentration range of 50 to 5000 ng/mL for both drugs...

Desenvolvimento e validação de uma metodologia analítica, em CLAE-PDA, para avaliação da estabilidade do 4-nerolidilcatecol na presença de seus produtos de degradação; Development and validation of an HPLC-PDA method for 4-nerolidylcatechol stability-indicating assay method

CARDOSO, Fabiana Fernandes de Santana e Silva
Fonte: Universidade Federal de Goiás; BR; UFG; Mestrado em Ciências Farmacêuticas; Ciências da Saúde - Farmácia Publicador: Universidade Federal de Goiás; BR; UFG; Mestrado em Ciências Farmacêuticas; Ciências da Saúde - Farmácia
Tipo: Dissertação Formato: application/pdf
POR
Relevância na Pesquisa
46.68%
The 4-nerolidylcatechol is the main secondary metabolite of the species Pothomorphe umbellata L. Miq. with established antioxidant, anti-inflammatory and photoprotective actions. Nevertheless, after its isolation and storage, evidence of photoinstability is observed, in a way that the characterization of the factors that influence such instability become mandatory, facing the perspective of a new drug development. Therefore, the aim of this paper was to develop and validate a hromatographic methodology able to analyze the degradation kinetic of the 4-NRC, in the presence of the degradation products, using the high performance liquid chromatography coupled to a detector with photodiodes (HPLC-PDA). Our results showed that the analytical method was selective (5 μg/mL) and linear over a wide range of concentrations (5.0 to 500.0 μg/mL) indicating high intra-day (0,02 2.83%) and inter-day precision (0.59 4.89%), besides accuracy (98.46 104.88%) and ruggedness. The photolytic study showed a fast degradation of 4- nerolidylcatechol (tR = 25 min), generating a major product after a total run time of 8 min. The hydrolytic study showed high instability of the substance in alkaline medium (pH 13.00), generating a major product after a chromatographic run time of 26 min. In acid conditions (pH 1.00)...

Validação analítica de método em HPLC-PDA para avaliação do perfil de exposição a solventes orgânicos aromáticos em comunidade universitária; Analytical method validation in HPLC-PDA to assessing the profile of exposure to aromatic organic solvents in university community

Honório, Tereza Cristina de Deus
Fonte: Universidade Federal de Goiás; Brasil; UFG; Programa de Pós-graduação em Ciências da Saúde (FM); Faculdade de Medicina - FM (RG) Publicador: Universidade Federal de Goiás; Brasil; UFG; Programa de Pós-graduação em Ciências da Saúde (FM); Faculdade de Medicina - FM (RG)
Tipo: Dissertação Formato: application/pdf
POR
Relevância na Pesquisa
67.06%
Introduction: Aromatic organic solvents (AOS) are widely used in diverse industrial and laborer activities among others involving manipulating of products likes lacquers, inks and varnishes. Among the most commonly used AOS are toluene, xylene, styrene, ethylbenzene and phenol. Occupational exposure to these compounds can cause damage to the body, which leads to a concern about the health of the worker. Biological monitoring is an important tool used to evaluate exposition to chemical substances in the work environment, that consists of quantify the biomarkers of occupational exposure in biological samples. Brazilian values of AOS biomarkers and maximum allowable biological index (IBMP) are described in the NR7 of the Brazilian legislation (Ministério do Trabalho e Emprego, MTE). Objective: The aim of this work was to validate technical in HPLC-PDA for quantifying the exposure’s biomarkers and than evaluate the exposure’s profile to toluene, xylene, styrene, ethylbenzene and phenol in workers exposed in university community. Methods: To analyze the AOS biomarkers in urine samples by HPLC-PDA, method validation was done according to the preconized parameters by ANVISA described in RE 899/2003. Participate of the study 30 occupationally exposed volunteers that provided urine samples and asked a questionnaire survey to characterize the sampling. The sampling’s characterization was done by applying a survey to volunteers. Both descriptive and multivariate statitical analysis was performed to the analytical and surveying data. Results: The analytical method was to validate and appropriated for the purposes established. About 3...

Análise toxicológica por técnicas de triagem aplicada em amostras biológicas post-mortem de casos suspeitos de intoxicação provenientes de Instituto de Criminalítisca; Systematic toxicological analysis by screening techniques applied in pos-mortem biological samples of suspected cases of poisning from Institute of Forensic

Silva, Maria Augusta Alves
Fonte: Universidade Federal de Goiás; Brasil; UFG; Programa de Pós-graduação em Ciências Farmacêuticas (FF); Faculdade Farmácia - FF (RG) Publicador: Universidade Federal de Goiás; Brasil; UFG; Programa de Pós-graduação em Ciências Farmacêuticas (FF); Faculdade Farmácia - FF (RG)
Tipo: Dissertação Formato: application/pdf
POR
Relevância na Pesquisa
47.06%
The toxicological analyzes on various samples are extremely important and can be used for multiple purposes, such as monitoring of drug addicts, forensic analysis, doping control, therapeutic monitoring, analyses of environmental contaminants, etc. The objective of this study was to analyze post - mortem blood samples of the Instituto de Criminalística de Goiás (IC) by immunochromatography and systematic toxicological analysis HPLC - PDA to check the presence or absence of toxic agents. The chromatographic conditions of the method were: mobile phase monobasic potassium phosphate buffer pH 2.3 and acetonitrile, flow rate 1 ml / min, Lichrospher RP8 column, 5μm, 250 x 4.0 mm, scanning range 200-380 nm, the calibration standards were MPPH system, caffeine, benzene and histamine. It was used the database proposed by UVTOX Pragst et al (2001). As part of the partial validation the matrix effect was evaluated by liquid-liquid extraction of whole blood samples contaminated with 8 standards in known concentration. The whole blood samples were extracted at different pH values and analyzed by HPLC -PDA. Through the areas obtained from each standard, it was calculated the standardized factor matrix which showed a coefficient of variation less than 10 %. In order to compare two screening techniques for detection of drugs of abuse...

Antifungals and acetylcholinesterase inhibitors from the stem bark of Croton heliotropiifolius

Queiroz, M. M. F.; Queiroz, E. F.; Zeraik, M. L.; Marti, G.; Favre-Godal, Q.; Simoes-Pires, C.; Marcourt, L.; Carrupt, P. A.; Cuendet, M.; Paulo, M. Q.; Bolzani, V. S.; Wolfender, J. L.
Fonte: Elsevier B.V. Publicador: Elsevier B.V.
Tipo: Artigo de Revista Científica Formato: LXXXVIII-xciii
ENG
Relevância na Pesquisa
46.73%
Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP); Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES); Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq); The ethanolic extract of the stem bark of Croton heliotropiifolius Kunth (Euphorbiaceae) showed significant in vitro inhibition of acetylcholinesterase using a dilution spectrophotometric assay and antifungal activity against Candida albicans with a thin layer chromatography (TLC) bioautographic assay. In order to isolate the active compounds, bioassay-guided fractionation was undertaken using HPLC to localize the active compounds. Different zones of the HPLC-UV chromatogram were linked to acetylcholinesterase inhibition or to antifungal activities. In parallel to this HPLC-based activity profiling, HPLC-PDA-ESI-MS and HPLC-TOF-HRMS were used for the early identification of some of the compounds present. The targeted isolation of the active compounds was performed by medium pressure liquid chromatography (MPLC-UV) and further semi-preparative HPLC. Using this approach, nine compounds were isolated, one of them being a new indole alkaloid derivative. The structures of the isolated compounds were elucidated by spectroscopic methods including UV...