GC-MS/MS测定坎地沙坦酯片中基因毒性杂质1-氯乙基环己基碳酸酯  

Determination of 1-Chloroethyl Cyclohexyl Carbonate in Candesartan Cilexetil Tablets by GC-MS/MS

作　　者：刘小勤 顾霄 倪维芳 陶巧凤 郑金琪 LIU Xiaoqin;GU Xiao;NI Weifang;TAO Qiaofeng;ZHENG Jinqi(Zhejiang Institute for Food and Drug Control,Hangzhou 310000,China;Key Laboratory for Core Technology of Generic Drug Evaluation National Medical Product Administration,Hangzhou 310000,China;Key Laboratory of Drug Contacting Materials Quality Control of Zhejiang Province,Hangzhou 310000,China)

机构地区：[1]浙江省食品药品检验研究院,杭州310000 [2]国家药品监督管理局仿制药评价关键技术重点实验室,杭州310000 [3]浙江省药品接触材料质量控制研究重点实验室,杭州310000

出　　处：《中国现代应用药学》2024年第9期1238-1241,共4页Chinese Journal of Modern Applied Pharmacy

摘　　要：目的建立GC-MS/MS分析方法测定坎地沙坦酯片中基因毒性杂质1-氯乙基环己基碳酸酯。方法采用DB-5MS(30 m×0.25 mm,0.25μm)毛细管柱,程序升温,初始温度80℃,以20℃·min^(-1)的速率升至300℃,维持5 min,以氦气为载气,流速1.0 mL·min^(-1),多反应监测模式检测。结果1-氯乙基环己基碳酸酯在4.4~437.8 ng·mL^(-1)内线性关系良好,定量限为4.4 ng·mL^(-1),检测限为2.2 ng·mL^(-1),平均回收率为95.6%(RSD=6.3%,n=9)。结论本法操作简单、灵敏度高、准确性好,适用于坎地沙坦酯片中基因毒性杂质1-氯乙基环己基碳酸酯的检测。OBJECTIVE To establish a GC-MS/MS analytical method for the determination of 1-chloroethyl cyclohexyl carbonate in candesartan cilexetil tablets.METHODS The analytical column was DB-5MS(30 m×0.25 mm,0.25μm).The column temperature was maintained at 80℃,then was raised to 300℃at the rate of 20℃·min^(-1)and was maintained for 5 min.Helium was used as carrier gas,and its flow rate was 1.0 mL·min^(-1).The detection was achieved in multiple reaction monitoring mode.RESULTS The calibration curve of 1-chloroethyl cyclohexyl carbonate had good linearity in the concentration range of 4.4-437.8 ng·mL^(-1).The limits of quantification and detection were 4.4 and 2.2 ng·mL^(-1),respectively.The average recovery was 95.6%(RSD=6.3%,n=9).CONCLUSION This method has satisfactory convenience,good sensitivity and high accuracy,and it is suitable for the determination of 1-chloroethyl cyclohexyl carbonate in candesartan cilexetil tablets.

关 键 词：坎地沙坦酯片 1-氯乙基环己基碳酸酯 气相色谱串联质谱 基因毒性杂质 

分 类 号：R917.101[医药卫生—药物分析学]