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
刘小勤 1顾霄 1倪维芳 2陶巧凤 2郑金琪2
作者信息
- 1. 浙江省食品药品检验研究院,杭州 310000;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
- 2. 浙江省食品药品检验研究院,杭州 310000;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;浙江省药品接触材料质量控制研究重点实验室,杭州 310000
- 折叠
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(30m×0.25 mm,0.25 pm)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4.4ng·mL-1,检测限为2.2ng·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.
Abstract
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,0.25 μm).The column temperature was maintained at 80 ℃,then was raised to 300 ℃ at the rate of 20 ℃i-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Key words
candesartan cilexetil tablets/1-chloroethyl cyclohexyl carbonate/GC-MS/MS/genotoxic impurity引用本文复制引用
出版年
2024
NETL
NSTL
万方数据