色谱

色谱

• 研究简报 • 上一篇    下一篇

固相萃取-高效液相色谱法测定人血浆中的川芎嗪

翁伟宇,沈腾,徐惠南,张建芳,黄建明,黄照昌,蔡佳   

  1. School of Pharmacy, Fudan University, Shanghai 200032, China
  • 收稿日期:2004-04-29 修回日期:1900-01-01 出版日期:2005-05-30 发布日期:1988-09-25
  • 通讯作者: 徐惠南
  • 基金资助:

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

WENG Weiyu, SHEN Teng, XU Huinan, ZHANG Jianfang, HUANG Jianming, HUANG Zhaochang, CAI Jia   

  1. School of Pharmacy, Fudan University, Shanghai 200032, China
  • Received:2004-04-29 Revised:1900-01-01 Online:2005-05-30 Published:1988-09-25

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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。

关键词: 川芎嗪, 反相高效液相色谱法, 人血浆

Abstract: 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×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 C8 solid-phase extraction column. Linearity was confirmed in the mass concentration range of 25-5000 μg/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 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.

Key words: human plasma , ligustrazine, high performance liquid chromatography