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

刘小勤; 顾霄; 倪维芳; 陶巧凤; 郑金琪

doi:10.13748/j.cnki.issn1007-7693.20224082

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

摘要

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。

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.

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