Determination of Diazepam in Human Plasma by Solid-Phase Microextraction and Capillary Gas Chromatography-Mass Spectrometry |
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Authors: | M. H. De. Oliveira M. E. C. Queiroz D. Carvalho S. M. Silva F. M. Lancas |
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Affiliation: | (1) Instituto de Química de São Carlos, Universidade de São Paulo, São Carlos, SP, 13560-970, Brasil;(2) Departamento de Química, Faculdade de Filosofia Ciěncias e Letras de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, 14040-901, SP, Brasil;(3) Curso de Ciências Farmacêuticas, Universidade de Ribeirão Preto, Ribeirão Preto, SP, 14096-380, Brasil |
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Abstract: | A simple, sensitive, and reproducible solid-phase microextraction and capillary gas chromatography-mass spectrometry (SPME-GC-MS) method for determination of diazepam in human plasma is described. The optimum conditions for the SPME procedure were as following: direct extraction mode with a polydimethylsiloxane (PDMS) fiber (100 μm film thickness), 250 μL of sample plasma matrix modified with a solution containing sodium chloride (10% weight by volume) and 4.25 mL of a phosphate buffer solution (0.1mol L−1, pH 6.9), extraction temperature 55°C under a magnetic stirring rate of 2500 rpm for 30 min, followed by the drug thermal desorption (250°C) in a GC injection port for 10 min. The limit of quantification of diazepam in plasma was 10.0 ng mL−1, with a coefficient of variation lower than 14.0% and linearity from 10.0 to 1000.0 ng mL−1, which allows diazepam analyses from sub to therapeutic levels. |
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Keywords: | Gas chromatography-mass spectrometry Solid-phase microextraction Diazepam in human plasma |
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