HPLC法测定替尼泊苷原料药的有关物质  

Determination of related substances in teniposide by HPLC

作　　者：范保瑞 张悦 马逢伯 曹新杰 郑清林[2] Fan Baorui;Zhang Yue;Ma Fengbo;Cao Xinjie;Zheng Qinglin(Beijing Pinggu District food and drug safety monitoring center,Beijing 101200;Beijing Purkinje General Instrument Co.,Ltd.,Beijing 101200)

机构地区：[1]北京市平谷区食品药品安全监控中心,北京101200 [2]北京普析通用仪器有限责任公司,北京101200

出　　处：《现代科学仪器》2021年第3期71-75,共5页Modern Scientific Instruments

基　　金：市区两级重大关键任务科技支撑项目:平谷特色家产品检测公共服务平台(2191100005619002)。

摘　　要：目的建立高效液相色谱法测定替尼泊苷原料药中的有关物质(木酚素P、2-噻吩甲醛、4'-去甲基表鬼臼毒素)。方法采用高效液相色谱法。色谱柱为Phenomenex Luna Phenyl-Hexyl(250×4.6mm,5μm),流动相A:乙腈-醋酸盐缓冲液(20:80);流动相B:乙腈-醋酸盐缓冲液(60:40),梯度洗脱,检测波长:284nm;柱温:30℃,流速:1.0ml/min。结果木酚素P、2-噻吩甲醛和4'-去甲基表鬼臼毒素均能与主成分完全分离。木酚素P、2-噻吩甲醛和4'-去甲基表鬼臼毒素质量浓度在0.2μg/ml~20μg/ml范围内与各自峰面积积分值呈良好的线性关系r=1、0.999、1,检测限分别为4.02ng、0.37ng、1.20ng,定量限分别为20.10ng、1.23ng、4.01ng,平均回收率为100.4%、100.2%、98.7%。结论该方法灵敏、准确、专属性强、重复性好,可用于替尼泊苷原料药的质量控制。Objective To establish an HPLC method for the determination of related substances(lig P,TCA,DMEP)in teniposide.Methods HPLC was used.The chromatographic column was phenomenex Luna phenyl hexyl(250×4.6mm,5μm),mobile phase A:acetonitrile acetate buffer(20:80);mobile phase B:acetonitrile acetate buffer(60:40),gradient elution,detection wavelength:284 nm;column temperature:30℃,flow rate:1.0ml/min.Results Lig P,TCA,DMEP were completely separated from the man components.In the range of 0.2μg/ml-20μg/ml,the linear ranges of Lig P,TCA and DMEP were 1,0.999 and 1,respectively.The limits of detection were 4.02ng,0.37ng and 1.20ng,and the limits of quantification were 20.10ng,1.23ng and 4.01ng,respectively.The average recoveries were 100.4%,100.2%and 98.7%,respectively.Conclusion the method is sensitive,accurate,specific and reproducible,and can be used for the quality control of teniposide.

关 键 词：替尼泊苷原料药 高效液相色谱法 梯度洗脱 有关物质 

分 类 号：R28[医药卫生—中药学]