固相萃取-高效液相色谱法测定人血浆中的川芎嗪  

Determination of Ligustrazine in Human Plasma by High Performance Liquid Chromatography with Solid-Phase Extraction

作　　者：翁伟宇[1] 沈腾[1] 徐惠南[1] 张建芳[1] 黄建明[1] 黄照昌[1] 蔡佳[1] 

机构地区：[1]复旦大学药学院,上海200032

出　　处：《色谱》2005年第3期276-278,共3页Chinese Journal of Chromatography

摘　　要：建立了高效液相色谱测定人血浆中川芎嗪浓度的方法。色谱条件:分析柱为LunaC18(150mm×4.6mmi.d.,5μm),流动相为甲醇乙腈醋酸盐缓冲液(pH5.0)(体积比为50∶8∶42),流速1.0mL/min,柱温40℃,检测波长280nm。血浆样品预处理采用C8固相小柱萃取法。方法的线性范围为25～5000μg/L,线性相关系数为0.9999。高、中、低浓度的川芎嗪在标准血浆样品中的平均提取回收率为96.72%～100.90%,日内和日间相对标准偏差(RSD)小于8.64%,准确度为99.59%～103.26%,检测限为10μg/L。该方法的各项效能指标符合生物样品的分析要求,可用于川芎嗪制剂的人体药代动力学研究。A high performance liquid chromatographic method was developed for the determination of ligustrazine in human plasma. The chromatographic separation was performed on a Luna C 18 column (150 mm×4.6 mm i.d., 5 μm) at column temperature of 40 ℃. The mobile phase, a mixture of methanol-acetonitrile-acetate buffer of pH 5.0 (50∶8∶42, v/v), was delivered at a flow rate of 1.0 mL/min. The detection wavelength was 280 nm. Plasma samples were prepared with a C 8 solid-phase extraction column. Linearity was confirmed in the mass concentration range of 25- 5000 μg/L with the correlation coefficient of 0.9999. The extraction recovery of ligustrazine ranged from 96.72% to 100.90%. The relative standard deviations (RSDs) of intra- and inter-day assay at the mass concentrations of 50, 500 and 3000 μg/L were less than 8.64% and the accuracies were between 99.59%-103.26%. The limit of detection (LOD) was 10 μg/L. The results of this method validation satisfactorily meet the acceptance criteria of bioanalysis and the method is applicable to the pharmacokinetic studies of ligustrazine in human beings.

关 键 词：反相高效液相色谱法 川芎嗪 人血浆 

分 类 号：O658[理学—分析化学]