固相萃取-高效液相色谱法测定人血浆中的川芎嗪

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Luna C18(150 mm×4.6 mm i.d.,5 μ m),流动相为甲醇-乙腈-醋酸盐缓冲液(pH 5.0)(体积比为50∶8∶42),流速1.0 mL/min,柱温40 ℃,检测波长280 nm。 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25～5000 μg/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10 μg/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。

Determination of Ligustrazine in Human Plasma by High Performance Liquid Chromatography with

A high performance liquid chromatographic method was developed for the determination of ligustrazine in human plasma. The chromatographic separation was performed on a Luna C18 column (150 mm x 4.6 mm i.d., 5 microm) at column temperature of 40 degrees C. 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 C8 solid-phase extraction column. Linearity was confirmed in the mass concentration range of 25-5000 microg/L with the correlation coefficient of 0.9999. 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 3000 microg/L were less than 8.64% and the accuracies were between 99.59%-103.26%. The limit of detection (LOD) was 10 microg/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.