GC-MS法测定盐酸右美托咪定中1,2-二氯乙烷的残留量

Determination of Residual 1,2-Dichloroethane in Dexmedetomidine Hydrochloride by GC-MS

目的:建立气相色谱-质谱(GC-MS)法测定盐酸右美托咪定原料药中1,2-二氯乙烷。方法:采用气相色谱-质谱联用法。色谱柱为安捷伦DB-624UI毛细管柱(30 m×0.32 mm,1.8"m),程序升温,在选择离子扫描(SIM)方式下,监测离子m/z62.0,外标法定量。结果:1,2-二氯乙烷在100～400 ng·ml^(-1)范围内线性关系良好(r=0.999 2),定量限为100 ng·ml^(-1),平均回收率为100.3%(RSD=9.4%,n=6)。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1,2-二氯乙烷的残留量测定。

Objective: To establish a GC-MS method for the determination of residual 1,2-dichloroethane in dexmedetomidine hydrochloride. Methods: A GC-MS method was used in the experiment. The analytes were separated on a DB-624 UI capillary column( 30 m × 0. 32 mm,1. 8μm) by programmed heating. The detection was performed by mass spectrometry in a selective ion monitoring mode with m/z 62. 0. The quantification was performed by an external standard method. Results: Good linearity was achieved within the range of 100-400 ng·ml^-1( r = 0. 999 2). The limit of quantification was 100 ng·ml^-1 and the average recovery was 100. 3%( RSD = 9. 4%,n = 6). Conclusion: The established method is useful for the determination of residual 1,2-dichloroethane in dexmedetomidine hydrochloride.