阿卡波糖固体制剂有关物质测定及未知杂质结构鉴定  

Determination of Related Substances of Acarbose Solid Preparations and Impurity Identification

作　　者：彭飞城 李昌亮 石笑弋 高慧如 李帅 刘雁鸣 兰文 易必新 PENG Fei-cheng;LI Chang-liang;SHI Xiao-yi;GAO Hui-ru;LI Shuai;LIU Yan-ming;LAN Wen;YI Bi-xin(Hunan Institute for Drug Control and Testing,Hunan Changsha 410001;NMPA Key Laboratory for Pharmaceutical Excipients Engineering Technology Reasearch,Hunan Changsha 410001;Hunan Drug Inspection Center,Hunan Changsha 410001,China)

机构地区：[1]湖南省药品检验检测研究院,湖南长沙410001 [2]国家药品监督管理局药用辅料工程技术研究重点实验室,湖南长沙410001 [3]湖南省药品审核查验中心,湖南长沙410001

出　　处：《广州化工》2024年第15期76-79,90,共5页GuangZhou Chemical Industry

基　　金：2021年国家药品抽验计划(No.国药监药管[2021]1号);湖南省2024部门联合基金项目(No:2024JJ8177)。

摘　　要：建立阿卡波糖固体制剂有关物质的测定方法,对未知杂质[相对保留时间(relative retention time,RRT) 0.75]进行结构鉴定。采用HPLC法进行有关物质测定,使用氨基柱(150 mm×4.6 mm,3μm),流动相采用磷酸盐缓冲液(取磷酸二氢钾2.13 g与磷酸氢二钠二水合物0.77 g,加水至1 000 mL,调节pH值至6.4)-乙腈(22∶78);检测波长为210 nm;流速为2.2~2.5 mL/min;柱温45℃。采用2DLC-QTOF/MS方法,对RRT 0.75杂质做结构鉴定。通过改进实验条件,提高了杂质Ⅰ、杂质Ⅲ峰与阿卡波糖峰的分离度;通过方法学验证,确定该方法的专属性好、灵敏度高,准确性好。RRT0.75杂质鉴定为阿卡波糖的同分异构体。建立的方法能准确测定阿卡波糖固体制剂中的有关物质,可为本品的工艺优化和质量控制提供参考依据。To develop a method for related substances of Acarbose Solid preparations,and identify the structure of impurity whose relative retention time(RRT) was 0.75,the related substances were determined by HPLC,which was performed on amino column(150 mm×4.6 mm,3 μm),the moblie phase was phosphate buffer(took 2.13 g of potassium dihydrogen phosphate and 0.77 g of disodium hydrogen phosphate dihydrate,and added water to 1 000 mL,and then adjusted pH to 6.4)-acetonitrile(22∶78) at the flow rate of 2.2~2.5 mL/min,the detection wavelength was 210 nm,and the column temperature was 45 ℃.2DLC-Q-TOF/MS was used to identify the structure of impurity(RRT 0.75).By improving the experimental conditions,the separation degree between impurity Ⅰ,impurity Ⅲ and acarbose was improved.The methodological test confirmed that the method had good specificity,high sensitivity,good accuracy.The impurity(RRT 0.75) was supposed to be the isomer of acarbose.The established HPLC method can determine the related substances in acarbose solid preparations accurately,which can provide references for the process optimization and quality control of acarbose solid preparations.

关 键 词：阿卡波糖固体制剂 高效液相色谱法 有关物质 结构鉴定 

分 类 号：R917[医药卫生—药物分析学]