A simple HPLC method for determining 2-(3-chlorophenyloamino)-5-(2,4-dihydroxyphenyl)-1,3,4-thiadiazole in brain and plasma of animals: Application to a pharmacokinetic study

Abstract

Summary. The development, optimization, and validation of a new high-performance liquid chromatography ultraviolet (HPLC-UV) method is presented for determining 2-(3-chlorophenyloamino)-5-(2,4-dihydroxy-phenyl)-1,3,4-thiadiazole (ClABT) in biological samples of rat plasma and brain tissue. ClABT was extracted directly from a plasma supernatant fraction following protein precipitation with acetonitrile and high speed centrifugation. Reverse phase HPLC separation was performed using an ODS-2 Hypersil column with the mobile phase consisting of 0.05 M triethylammonium phosphate buffer solution in acetonitrile and methanol (120:280:600, v/v/v), at room temperature, 1.2 mL min −1 flow rate, and UV-diode-array detection (DAD), at 335 nm. A linear response was obtained between 12.5 and 2000 ng mL −1 at analytically acceptable levels of precision (intra/inter-day) and accuracy. Mean recoveries ranged from 92.7% to 107.9%. It was concluded that the method was specific and precise and thus suitable for quantitative analysis in clinical pharmacokinetic studies of ClABT.

Electrochemical Oxidation of 2,5-Dimercapto-1,3,4-thiadiazole on Carbon Electrodes Modified with Ru(III) Schiff Base Complex

“…The most commonly used analytical techniques for the determination and quantification of DMcT are capillary zone electrophoresis (CZE) and high performance liquid chromatography (HPLC) with UV detection. 7,8 These methods require expensive and non-portable instrumentation, trained personnel, sophisticated sample preparation, and suffer from numerous chemical interferences. The electrochemical techniques have some advantages like simplicity, fast response, wide linear dynamic range, ease of miniaturization, high sensitivity and low cost compared to other methods.…”

Eletrodos impressos descartáveis: aplicações em amostras ambientais, alimentícias e combustíveis

“…Por outro lado, as principais técnicas analíticas para determinação e quantificação de tiadiazóis são cromatografia líquida de alta eficiência (HPLC) e eletroforese capilar de zona (CZE) ambos com detecção por UV. Contudo, a instrumentação cara, a não portabilidade e o tempo de preparo das amostras (extrações em série) são algumas dificuldades associadas a estes métodos (CHERNOV'YANTS; ALESHINA;BURYKIN, 2011;RASZEWSKI et al, 2014).Inicialmente foi estudada a proporção volumétrica ideal de etanol e água na composição do eletrólito suporte para possibilitar a miscibilidade completa das amostras, principalmente do óleo mineral. A seleção de eletrólito é um ponto chave para determinar o DMCT devido à natureza complexa das amostras analisadas nesta tese.…”