GC-MS/MS法测定复方二甲双胍格列吡嗪胶囊中N-亚硝基二甲胺与N-亚硝基二乙胺  

Determination of N-nitrosodimethylamine and N-nitrosodiethylamine in compound metformin hydrochloride and glipizide capsules by GC-MS/MS

作　　者：岳青阳 张耀文 徐万魁 YUE Qing-yang;ZHANG Yao-wen;XU Wan-kui(Liaoning Inspection,Examination and Certification Centre,Shenyang 110036;Liaoning Institute for Drug Control/NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drug,Shenyang 110036)

机构地区：[1]辽宁省检验检测认证中心,沈阳110036 [2]辽宁省药品检验检测院/国家药品监督管理局化学药品质量研究与评价重点实验室,沈阳110036

出　　处：《中南药学》2023年第10期2720-2723,共4页Central South Pharmacy

基　　金：辽宁省自然科学基金项目(No.2020-MS-073)。

摘　　要：目的建立复方二甲双胍格列吡嗪胶囊中N-亚硝基二甲胺(NDMA)与N-亚硝基二乙胺(NDEA)的检测方法。方法色谱柱为Agilent VF-WAXms,载气为氦气,流速为1.2 mL·min^(-1),进样口温度250℃,柱温为程序升温。电子轰击电离方式,离子源温度:230℃;定量测定采用MRM模式。以8批复方盐酸二甲双胍格列吡嗪胶囊为测定对象,测定其NDMA和NDEA含量。结果NDMA、NDEA及相邻色谱峰之间的分离良好,分别在0.1966~39.32 ng·mL^(-1)(r=0.9990)和0.1870~37.41 ng·mL^(-1)(r=0.9995)内与峰面积线性关系良好,检测限分别为0.0983 ng·mL^(-1)和0.0935 ng·mL^(-1),加样回收率分别为82.3%和85.4%。结论该法分离效果好、操作简便、灵敏度高,可同时检测复方二甲双胍格列吡嗪胶囊中NDMA和NDEA的含量。Objective To establish a specific method to determine N-nitrosodimethylamine(NDMA)and N-nitrosodiethylamine(NDEA)in compound metformin hydrochloride and glipizide capsules.Methods The separation was performed on an Agilent VF-WAXms column in a temperature rising program.The carrier gas was helium with the flow rate of 1.2 mL·min^(-1).The inlet temperature was 250℃.The sample was ionized by electron ionization with multi reaction monitoring data acquisition mode.NDMA and NDEA were detected in 8 batches of compound metformin hydrochloride and glipizide capsules following based on the conditions.Results NDMA,NDEA and adjacent chromatographic peaks were separated well and showed good linearity at 0.1966~39.32 ng·mL^(-1)(r=0.9990)and 0.1870~37.41 ng·mL^(-1)(r=0.9995),respectively.The limit of detection was 0.0983 ng·mL^(-1) and 0.0935 ng·mL^(-1).The sample recoveries were 82.3%and 85.4%.Conclusion The method separaties well,convenient and sensitive,which can be used in the simultaneous determination of NDMA and NDEA in compound metformin hydrochloride and glipizide capsules.

关 键 词：GC-MS/MS N-亚硝基二甲胺 N-亚硝基二乙胺 复方二甲双胍格列吡嗪胶囊 

分 类 号：R927[医药卫生—药学]