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1.
Talanta ; 129: 552-9, 2014 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-25127632

RESUMO

Because of the high stability and potential toxic effects of non-steroidal anti-inflammatory drugs (NSAIDs), it is important to closely monitor their concentrations in the environment using a sensitive analytical method. In this study, a simple, rapid, efficient, and sensitive analytical method based on gas chromatography-mass spectrometry (GC-MS) was developed to determine the levels of seven common NSAIDs in various types of surface water. To simplify sample preparation, in situ derivatization using methyl chloroformate was combined with ultrasound-assisted emulsification microextraction. For selection and optimization of significant variables, experiments were statistically designed using Plackett-Burman design and central composite design. The resulting optimal conditions for derivatization and extraction were 100 µL of chloroform (extraction solvent), 10.0 mL of sample, and 240 µL of pyridine (catalyst as a base in derivatization). The optimized sample preparation coupled with optimized GC-MS analysis in selected ion monitoring mode provided good linearity from 0.010 to 5.0 ng mL(-1), and a limit of detection between 0.0050 and 0.010 ng mL(-1), good intra-day and inter-day precision (0.30-6.3% and 5.1-9.5%, respectively), and good accuracy (relative recovery; 91-117% at 0.20 ng mL(-1) and 77-105% at 2.5 ng mL(-1)). Compared with previously reported methods, the current method requires a small volume of sample and simple sample preparation steps for sensitive determination of NSAID levels using a conventional GC-MS system. The method was successfully applied to determine the levels of seven common NSAIDs in various types of surface water.


Assuntos
Anti-Inflamatórios não Esteroides/análise , Resíduos de Drogas/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Poluentes Químicos da Água/análise , Catálise , Química Farmacêutica/métodos , Clorofórmio/química , Monitoramento Ambiental/métodos , Limite de Detecção , Microextração em Fase Líquida , Piridinas/química , Reprodutibilidade dos Testes , Solventes/química , Ultrassom , Água/química
2.
J Org Chem ; 79(10): 4735-42, 2014 May 16.
Artigo em Inglês | MEDLINE | ID: mdl-24762192

RESUMO

A copper-catalyzed oxidative coupling of 2-carbonyl-substituted phenols and 1,3-dicarbonyl compounds with a wide range of dibenzyl or dialkyl ethers is described. This protocol provides an efficient preparation of phenol esters and enol esters in good yields with high chemoselectivity. This method represents an alternative protocol for classical esterification reactions.


Assuntos
Compostos de Benzil/química , Cobre/química , Éteres/química , Éteres/síntese química , Fenóis/química , Fenóis/síntese química , Catálise , Esterificação , Ésteres , Estrutura Molecular , Oxirredução
3.
J Microbiol Biotechnol ; 18(6): 1156-63, 2008 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-18600062

RESUMO

We performed RT-nested PCR to study the distribution of human enteric viruses in urban rivers in Korea. During 2002-2003, water samples were collected from four rivers in Gyeonggi Province, South Korea. Among 58 samples, 45 (77.6%), 32 (55.2%), 12 (20.7%), 2 (3.4%), 4 (6.9%), and 4 (6.9%) showed positive results with adenoviruses (AdVs), enteroviruses (EVs), reoviruses (ReVs), hepatitis A viruses (HAVs), rotaviruses (RoVs), and sapoviruses (SVs), respectively. According to the binary logistic regression model, the occurrence of each enteric virus, except ReVs and HAVs, was not statistically correlated with the water temperature and levels of fecal coliforms (P<0.05). AdVs were most often detected; only 4 samples (6.9%) were negative for AdVs while positive for other enteric viruses in the studied sites. Our results indicated that monitoring human enteric viruses is necessary to improve microbial quality, and that AdVs detection by PCR can be a useful index for the presence of other enteric viruses in aquatic environments.


Assuntos
Enterovirus/isolamento & purificação , Monitoramento Ambiental , Rios/virologia , Microbiologia da Água , Análise de Variância , Enterobacteriaceae/isolamento & purificação , Enterovirus/genética , Fezes/microbiologia , Fezes/virologia , Humanos , Coreia (Geográfico) , Modelos Logísticos , RNA Viral/genética , Reação em Cadeia da Polimerase Via Transcriptase Reversa , Temperatura
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