乌苯美司片有关物质测定方法的比较及优化  

Comparison and Optimization of Methods for Determination of Related Substances in Ubenimex Tablets

作　　者：郑金琪 陈翔 付莉娜[3] 郑国钢 

机构地区：[1]浙江省食品药品检验研究院,杭州310004 [2]舟山市食品药品检验所,舟山316021 [3]浙江工业大学药学院,杭州310014

出　　处：《中国药品标准》2014年第4期279-283,共5页Drug Standards of China

摘　　要：目的:优化并建立准确灵敏的乌苯美司片的有关物质检查方法。方法:比较国家标准YBH05722010和YBH07102009中有关物质检查方法在检测波长、配制溶剂、供试品溶液浓度、记录时间和辅料峰是否扣除上存在的差异,优化检查方法:C18柱,以甲醇-0.6%磷酸二氢钠溶液(45∶55)为流动相,柱温40℃,流量1.0 m L·min-1,检测波长220 nm。结果:按照标准YBH05722010中方法检测到的杂质个数和杂质总量均大于按照标准YBH07102009中方法测定的结果。方法优化后乌苯美司峰与辅料峰及各降解产物峰均能良好分离,供试品溶液在24 h内基本稳定,检测限为1.854 ng。结论:优化后方法灵敏度高,专属性强,结果准确,能更好地测定乌苯美司片的有关物质。Objective：To optimize and establish a method for the determination of related substances in Ubenimex tablets .Methods：The detection wavelength , dissolving solvents , concentration of sample solution , recording time and deduction of adjuvant were com-pared between the two government standards of YBH 05722010 and YBH07102009.The optimized RP-HPLC was performed on C 18 col-umn and the mobile phase was methanol-0.6%sodium dihydrogen phosphate solution （45∶55） with a flow rate of 1.0 mL· min-1, the temperature of column was 40 ℃and the detection wavelength was 220 nm.Results：The numbers and total amount of impurities determined according to YBH 05722010 were both more than that determined according to YBH 07102009.In optimized method , Uben-imex peak was completely separated from peaks of adjuvant and degraded impurities , the limit of detection was 1.854 ng and the solu-tion was stable for 24 h.Conclusion：The optimized method is specific , sensitive, accurate and can be used for the determination of related substances of Ubenimex tablets better.

关 键 词：乌苯美司片 有关物质 比较 优化 

分 类 号：R921.2[医药卫生—药学]