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目的建立大鼠脑组织中文拉法辛及其对映体的含量测定方法。方法大鼠脑组织样品经碱化、液-液提取后采用非手性与手性色谱系统相结合的方法,测定文拉法辛对映体的含量。在非手性色谱条件下,采用Diamonsil C18色谱柱(200 mm×4.6 mm,5μm),以乙腈-pH6.8磷酸盐缓冲液-三乙胺(体积比20∶80∶1,磷酸调pH值至3.5)为流动相,流速为1.0 mL.min-1;在手性色谱条件下,采用以α1-酸性糖蛋白为手性固定相的Chiral-AGP色谱柱,流动相为甲醇-80 mmol.L-1醋酸铵缓冲液(pH6.5)(体积比5∶95),流速为0.8 mL.min-1;检测波长230 nm。结果文拉法辛质量浓度在0.05～2.0 mg.L-1内与峰面积呈良好的线性关系,r=0.999 2(n=6),最低定量限为0.05 mg.L-1。低、中、高3种质量浓度样品的提取回收率分别为86.3%、90.2%、88.9%,日内及日间精密度均小于8%(n=6)。结论本方法简单、快速、灵敏、可靠,可用于大鼠脑组织中文拉法辛及其对映体的含量测定。
OBJECTIVE: To establish a method for the determination of venlafaxine and its enantiomers in rat brain. Methods The rat brain tissue samples were alkalized and liquid-liquid extracted. The enantiomers of venlafaxine were determined by achiral and chiral chromatographic methods. Chromatography was performed on a Diamonsil C18 column (200 mm × 4.6 mm, 5 μm) under achiral conditions using acetonitrile-pH 6.8 phosphate buffer-triethylamine (20: 80: To 3.5) as the mobile phase at a flow rate of 1.0 mL · min-1. Chiral-AGP with chiral stationary phase of α1-acidic glycoprotein was used under the condition of chiral chromatography. The mobile phase was methanol-80 mmol. L-1 ammonium acetate buffer (pH6.5) (volume ratio 5:95) at a flow rate of 0.8 mL.min-1. The detection wavelength was 230 nm. Results Venlafaxine had a good linear relationship with the peak area in the range of 0.05-2.0 mg.L-1, r = 0.999 2 (n = 6), and the lowest limit of quantification was 0.05 mg.L-1. The recoveries of low, medium and high quality samples were 86.3%, 90.2% and 88.9%, respectively. The intra- and inter-day precision were less than 8% (n = 6). Conclusion The method is simple, rapid, sensitive and reliable and can be used for the determination of norafaxine and its enantiomers in rat brain.