GC-MS法测定盐酸右美托咪定中氯甲烷和氯乙烷的残留量

Determination of methyl chloride and ethyl chloride in dexmedetomidine hydrochloride by GC-MS

目的建立并验证了气相色谱-质谱(GC-MS)法测定盐酸右美托咪定原料药中的基因毒性杂质氯甲烷和氯乙烷。方法色谱柱为DB-624UI毛细管柱(30 m×0.32 mm,1.8μm),程序升温,在选择离子扫描(SIM)方式下,氯甲烷m/z 50.0,氯乙烷m/z 64.0,外标法定量。结果氯甲烷和氯乙烷在100~1750 ng·m L-1与峰面积线性关系良好,两者定量限均为100 ng·m L-1,回收率均在96.5%~106.7%。结论本研究所建立的GC-MS法能用于盐酸右美托咪定原料药中氯甲烷和氯乙烷的杂质量测定。

Objective To establish a simple and sensitive GC-MS/MS method for determination of the genotoxic impurities methyl chloride and ethyl chloride in dexmedetomidine hydrochloride. Methods The analytes were separated on a DB-624UI capillary column （30 m X 0.32 mm, 1.8 μm） by programmed heating. Detection were performed by mass spectrometry in selective ion monitoring mode with m/z 50.0 for methyl chloride and m/z 64.0 for ethyl chloride. Results Good linearity was achieved in the range of 100 - 1750 ng ·mL-1 for both methyl chloride and ethyl chloride. The limit of quantification was 100 ng · mL-1. The recoveries of methyl chloride and ethyl chloride were between 96.5% and 106.7%. Conclusion It shows that the established method is useful for the determination of methyl chloride and ethyl chloride in dexmedetomidine hydrochloride.