HPLC柱切换法测定抗癌药米托蒽醌血浆浓度

新抗癌药米托蒽醌治疗剂量低,与血浆蛋白结合率较高,用一般样品预处理技术,操作麻烦费时。本文采用HPLC柱切换技术,以甲醇沉淀血浆蛋白,经超声振荡10 min,以YWG-CN为预处理柱(5cm×4.6 mm ID),水为预处理流动相,在线富集样品;以Shimpack CLC-ODS为分析柱(15cm×6 mm ID),甲醇—乙酸铵缓冲液(0.2 mol/L,pH 1.9)(48:52)为流动相,658 nm检测,内标法定量。净化富集样品操作简便,回收率好(85.5%);米托蒽醌的检测限为0.5 ng。血浆中最低检出浓度为6 ng/ml。日内变异系数为2.8～11%,日间变异系数为4.0～13.8%。在浓度为10～1000 ng/ml血浆范围内,呈线性关系。

DETERMINATION OF ANTITUMOUR DRUG MITOXANTRONE IN PLASMA USING HPLC COLUMN SWITCHING TECHNIQUE

An automated clean up and concentration method by column switching is described for the assay of mitoxantrone,an antitumour drug in plasma .The system uses a YWG- CN short precolumn for on- line clean up and concentration and a Shimpack CLC-ODS analytical column for separation. Water is used as pretreat mobile phase and 48% methanol in ammonium acetate (0.2 mol/L pH 1.9)is used as analytical mobile phase. The plasma sample is treated with methanol and ultrasonated for 10 min. The supernatant of treated sample is directly injected to precolumn .The recovery of clean up is 85%. The wavelength used for detection is 658 nm and the concentration of detection limit is 6 ng/ml in plasma. The procedure is simple and the method is sensitive.