用HPLC柱切换法血浆直接进样测定法莫替丁

DIRECT INJECTION OF PLASMA TO DETERMINE FAMOTIDINE IN PLASMA USING HPLC COLUMN SWITCHING TECHNIQUE

本文采用HPLC柱切换技术,建立了以YWG-C18(3cm)为预处理柱,乙酸(0.2mol/L)为预处理流动相,血浆直接进样。在线(on-line)固相净化血浆样品;以Shimpack CLC-ODS(15 cm)为分析柱,甲醇-0.2 mol/L乙酸铵缓冲液(14:86)为流动相,267 nm波长检测,采用外标法定量。测定H_2-受体拮抗剂法莫替丁人体血药浓度的方法。该法净化过程简便,为自动净化血浆样品提供了一选择方法。回收率好(81.10～84.75%);法莫替丁的检测限约为2.4 ng,血浆中最低检出浓度约为12 ng/ml。日内变异系数为4.1%,日间变异系数为4.9%;在浓度为15～210 ng/ml血浆范围内呈线性关系。

An automated high performance liquid chromatographic switching system is described for the analysis of famotidinc, an H_2-receptor antagonist in plasma. The system used YWG-C18 short precolumn for on-line sample clean-up and a Shimpack CLC-ODS analytical colunm for separation. A solution of 0.2 mol/L acetic acid was used as prctrcatmcnt mobile phase and 14%(v/v) methanol in ammonium acetate (0.2mol/L) was used as analytical mobile phase. The detection was at 267 nm and the detection limit was 12 ng/ml plasma. Plasma sample was diluted with acetic acid (0.2mol/L) andinjected directly on the HPLC system. The procedure of clean-up is simple and automatic. The recovery of clean-up is 84.1%.