| 引用本文: | 刘小勤,顾霄,倪维芳,陶巧凤,郑金琪*.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[J].中国现代应用药学,2024,41(9):1238-1241. |
| LIU Xiaoqin,GU Xiao,NI Weifang,TAO Qiaofeng,ZHENG Jinqi*.Determination of 1-Chloroethyl Cyclohexyl Carbonate in Candesartan Cilexetil Tablets by GC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2024,41(9):1238-1241. |
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| 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 |
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刘小勤1,2, 顾霄1,2, 倪维芳1,2,3, 陶巧凤1,2,3, 郑金琪*1,2,3
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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
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| 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，0.25 μm)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。 |
| 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 |
| DOI：10.13748/j.cnki.issn1007-7693.20224082 |
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| Determination of 1-Chloroethyl Cyclohexyl Carbonate in Candesartan Cilexetil Tablets by GC-MS/MS |
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LIU Xiaoqin1,2, GU Xiao1,2, NI Weifang1,2,3, TAO Qiaofeng1,2,3, ZHENG Jinqi*1,2,3
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1.Zhejiang Institute for Food and Drug Control, Hangzhou 310000, China;2.Key Laboratory for Core Technology of Generic Drug Evaluation National Medical Product Administration, Hangzhou 310000, China;3.Key Laboratory of Drug Contacting Materials Quality Control of Zhejiang Province, Hangzhou 310000, China
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| 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 ℃·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. |
| Key words: candesartan cilexetil tablets 1-chloroethyl cyclohexyl carbonate GC-MS/MS genotoxic impurity |
