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摘要
A conical microcolumn packed with gamma-methacryloxypropyltrimethoxysilane (gamma-MPS)-modified silica particles was developed for the separation/preconcentration of trace carbamazepine, amitriptyline, quetiapine, clozapine, clomipramine, and thioridazine in rat plasma and environmental water samples followed by liquid chromatography method coupled with ultra-violet detector. The chromatographic analysis was performed on a C-18 column under optimal conditions (mobile phase: ammonium acetate (0.03 mol L-1)-methanol-acetonitrile (37.0:44.1:18.9, v/v/v); flow rate: 1.0 mL min(-1); detection wavelength: 238 nm; column temperature: 25 A degrees C). The prepared gamma-MPS-modified silica particles were characterized by Fourier transform infrared spectroscopy and a Varian Infinity-plus400 NMR spectrometer. Various influencing factors such as pH, elution solvent and volume, flow rate and sample volume were investigated systematically. Under the optimal conditions, the method detection limits and the limits of quantitation were 0.7 and 2.1 ng mL(-1) for carbamazepine, 0.4 and 1.3 ng mL(-1) for amitriptyline, 0.6 and 1.8 ng mL(-1) for quetiapine, 0.7 and 2.1 ng mL(-1) for clozapine, 1.5 and 4.7 ng mL(-1) for clomipramine, 0.8 and 2.6 ng mL(-1) for thioridazine, respectively. The relative standard deviations for six replicates of analytes at 0.050 A mu g mL(-1) were less than 4.1 %. The proposed method was applied to the determination of trace amounts of the analytes in the spiked rat plasma and environmental water samples with satisfactory recoveries. It showed wide potential application in the field of the analysis of pharmaceuticals in real environmental water samples and the therapeutic drug monitoring.
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单位波谱与原子分子物理国家重点实验室; 华中科技大学; 中国科学院武汉物理与数学研究所
