HPLC法在泊沙康唑及其15种异构体杂质拆分中的应用  

Application of High Performance Liquid Chromatography in the Resolution of Posaconazole and Its Fifteen Isomeric Impurities

作　　者：孙井龙 游凤 倪冬胜 单冰冰 赵宜香 SUN Jinglong;YOU Feng;NI Dongsheng;SHAN Bingbing;ZHAO Yixiang(Nanjing Huawe Medicine Technology Group Co.Ltd.,Nanjing 210046)

机构地区：[1]南京华威医药科技集团有限公司,江苏南京210046

出　　处：《中国医药工业杂志》2021年第3期395-399,共5页Chinese Journal of Pharmaceuticals

摘　　要：建立了可同时测定泊沙康唑中15种异构体(14个立体异构体和1个位置异构体)杂质的HPLC法。采用Chiral MD(2)-RH色谱柱(4.6 mm×250 mm,5 μm),流动相为水∶乙腈∶二乙胺(48∶52∶0.1),流速为0.6 ml/min,柱温为30 ℃,检测波长为260 nm。结果显示,14个立体异构体以5个信号出峰,泊沙康唑与15种异构体杂质之间的分离度均符合要求;15种异构体在0.3~12.0 μg/ml内线性关系良好;方法回收率为91.6%~102.7%;检测限为0.09~0.11 μg/ml,定量限为0.28~0.32 μg/ml,均小于0.05%(报告限度)。本方法操作简便,专属性高,可准确测定泊沙康唑原料药及其肠溶片中15种异构体杂质的含量。An HPLC method was established for the determination of fifteen isomers in posaconazole,including fourteen stereoisomers and one regio-isomer.A Chiral MD(2)-RH column(4.6 mm×250 mm,5 μm) was used with the mobile phase of water∶acetonitrile∶diethylamine(48∶52∶0.1).The flow rate was 0.6 ml/min,the column temperature was 30 ℃,and the detection wavelength was 260 nm.The results showed that the fourteen stereoisomers appeared as five peaks and the resolutions between peaks of posaconazole and these fifteen isomeric impurities all met the requirements.Their linear ranges were 0.3-12.0 μg/ml and the recoveries were in the ranges of 91.6%-102.7%.The detection limits for the fifteen impurities were 0.09-0.11 μg/ml,and the quantification limits were 0.28-0.32 μg/ml,both limits were less than 0.05%(reporting limit).This method was simple to operate and had high specificity,which could accurately determine the contents of fifteen isomeric impurities in posaconazole and its enteric-coated tablets.

关 键 词：泊沙康唑 手性拆分 高效液相色谱法 异构体杂质 

分 类 号：R917[医药卫生—药物分析学] O657.7[医药卫生—药学]