分子排阻法测定头孢克肟颗粒中的高分子杂质  

Determination of polymer impurities in cefixime granules by molecular-exclusion chromatography method

作　　者：苏燕琼 蔡国伟 高琳 SU Yan-qiong;CAI Guo-wei;GAO Lin(Guangzhou Baiyunshan Pharmaceutical Group Co.,Ltd..Baiyunshan Pharmaceutical Factory,Guangzhou 510515)

机构地区：[1]广州白云山医药集团股份有限公司白云山制药总厂

出　　处：《中南药学》2019年第11期1949-1952,共4页Central South Pharmacy

基　　金：广东省科技计划项目(No.2017B020234005)

摘　　要：目的建立分子排阻色谱法分析头孢克肟颗粒高分子杂质。方法采用TSK gel G2000 SWXL色谱柱(7.8 mm×30 cm×5 mm),流动相为A 0.005 mol·L^-1磷酸盐缓冲液(p H 7.0)[0.005 mol·L^-1磷酸氢二钠溶液和0.005 mol·L^-1磷酸二氢钠溶液(61∶39)]-B乙腈(95∶5),流速为0.8 mL·min^-1,检测波长为288 nm。结果头孢克肟、头孢克肟双母核1、聚合物杂质B、头孢克肟二聚体F在0.02~3.0μg·mL^-1与峰面积线性关系良好(r>0.990),头孢克肟双母核1、聚合物杂质B、头孢克肟二聚体F的校正因子分别为1.11、1.13、1.09,各已知高分子杂质可以主成分自身对照法定量。结论该法能较好地分离头孢克肟与其高分子杂质,且精密度、准确度、重复性均能满足质量控制的要求。Objective To establish a molecular-exclusion chromatography method to determine polymer impurities in cefixime granules.Methods The analytical column was TSK gel G2000 SWXL(7.8 mm×30 cm×5 mm)with mobile phase A of 0.005 mol·L^-1 phosphate buffer(pH 7.0),while mobile phase B of acetonitrile.The flow rate was 0.8 mL·min^-1 and the detection wavelength was 288 nm.Results The calibration curves of cefixime and cefecoxime dimother nucleus 1,polymer impurity B,and cefecoxime dimer F were linearity at 0.02-3.0μg·mL^-1(r>0.990).The correction factors of cefecoxime dimother nucleus 1,polymer impurity B,and cefecoxime dimer F were 1.11,1.13,and 1.09,respectively.Each known polymer impurity was quantified by the main component itself.Conclusion The method can well separate cefixime and its polymer impurities,precisely,accurately,and repeatability can the requirements of quality control.

关 键 词：头孢克肟颗粒 高分子杂质 分子排阻法 校正因子 

分 类 号：R927[医药卫生—药学]