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采用激光诱导荧光检测的毛细管电泳法测定人血浆中的度洛西汀。

Determination of duloxetine in human plasma by capillary electrophoresis with laser-induced fluorescence detection.

作者信息

Musenga Alessandro, Amore Mario, Mandrioli Roberto, Kenndler Ernst, de Martino Ludovica, Raggi Maria Augusta

机构信息

Department of Pharmaceutical Sciences, Alma Mater Studiorum-University of Bologna, Bologna, Italy.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Apr 15;877(11-12):1126-32. doi: 10.1016/j.jchromb.2009.02.059. Epub 2009 Mar 3.

Abstract

A method based on capillary electrophoresis has been developed for the analysis of the novel antidepressant drug duloxetine in human plasma. The method makes use of laser-induced fluorescence detection after derivatisation of the analyte with 5-(4,6-dichlorotriazinyl)aminofluorescein at pH 11. A single step liquid/liquid extraction procedure with a mixture of hexane/2-propanol allows the sample clean-up with extraction yields always >or=84% and interference removal. The electrophoretic separation is achieved using uncoated fused silica capillaries (60.0 cm effective length, 75.0 cm total length, 50 microm internal diameter) and a background electrolyte composed of borate buffer (40 mM, pH 10.3), tetrabutylammonium bromide (10 mM), and acetone (10%, v/v). The applied voltage is 20 kV; the samples are injected by pressure (50 mbar x 8 s). The method has been fully validated in terms of linearity range (2.5-150 ng mL(-1)), LOD and LOQ (1.0 and 2.5 ng mL(-1), respectively), precision (R.S.D.<6.7%) and accuracy (recovery >78%). Application to samples obtained from patients under treatment with duloxetine gave good results. The method represents the first application of capillary electrophoresis to the analysis of duloxetine in human plasma.

摘要

已开发出一种基于毛细管电泳的方法,用于分析人血浆中的新型抗抑郁药物度洛西汀。该方法在pH 11条件下,用5-(4,6-二氯三嗪基)氨基荧光素对分析物进行衍生化后,利用激光诱导荧光检测。采用己烷/2-丙醇混合物进行单步液/液萃取程序,可实现样品净化,萃取产率始终≥84%,并能去除干扰物。使用未涂层熔融石英毛细管(有效长度60.0 cm,总长度75.0 cm,内径50 μm)和由硼酸盐缓冲液(40 mM,pH 10.3)、溴化四丁铵(10 mM)和丙酮(10%,v/v)组成的背景电解质实现电泳分离。施加电压为20 kV;样品通过压力进样(50 mbar×8 s)。该方法已在以下方面得到充分验证:线性范围(2.5 - 150 ng mL⁻¹)、检测限和定量限(分别为1.0和2.5 ng mL⁻¹)、精密度(相对标准偏差<6.7%)和准确度(回收率>78%)。将其应用于接受度洛西汀治疗的患者所获得的样品,结果良好。该方法是毛细管电泳首次应用于分析人血浆中的度洛西汀。

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