顶空气相色谱法测定盐酸倍他司汀原料药中有机溶剂的残留量

Determination of Residual Organic Solvents in Betahistine Hydrochloride Crude Material by Headspace Gas Chromatography

目的:建立顶空气相色谱法测定盐酸倍他司汀原料药中乙醇、异丙醇、二氯甲烷3种有机溶剂残留量的方法。方法:色谱柱为DB-624石英毛细管柱,柱温70℃,检测器为氢火焰离子化检测器,检测器温度为250℃,进样口温度为180℃,以水为溶剂。结果:乙醇、异丙醇、二氯甲烷的检测浓度的线性范围分别为20～1000(r=1.0000)、20～1000(r=0.9999)、2.4～120(r=0.9998)μg·mL-1;平均回收率为98.6%～99.6%(RSD=0.1%～0.3%);检出限为0.49～1.89μg·mL-1;3批样品中3种有机溶剂残留量均符合《中国药典》要求。结论:本方法简单、准确、灵敏度高、重复性好,可用于该药物中有机溶剂残留量的测定。

OBJECTIVE：To establish a headspace GC method for the determination of residual organic solvents,including alcohol, isopropyl alcohol and dichloromethane in betahistine hydrochloride crude material. METHODS：The residual organic solvents were separated on DB-624 capillary column with a temperature of 70 ℃. FID was used as detector with a temperature of 250 ℃,the inlet temperature was 180 ℃,and water as the solvent. RESULTS：The linear ranges of alcohol, isopropyl alcohol and dichloromethane were 20～100 0（r=1.000 0）,20～100 0（r=0.999 9）,2.4～120 （r=0.999 8） μg·mL-1,respectively.The average recoveries were ranged from 98.6% to 99.6%（RSD=0.1%～0.3%）.The detection limits were 0.49～1.89 μg·mL-1.The residual levels for the three organic solvents in 3 batches samples were all up to the standard stipulated in Chinese Pharmacopeia. CONCLUSION：The method is simple,accurate,sensitive and reproducible,it can be used for the determination of the residual organic solvents in betahistine hydrochloride.