氢溴酸高乌甲素中有机溶剂残留量HL-GC 检测方法的建立

目的：建立测定氢溴酸高乌甲素中4种有机溶剂残留量的顶空毛细管气相色谱方法。方法采用DB-624毛细管柱（30 m ×0.53 mm,3μm）,程序升温,起始柱温40℃,维持7 min,以25℃·min-1的速率升至200℃,维持1 min；进样口温度：200℃；FID 检测器,检测器温度：250℃；进样方式：顶空进样,平衡温度：80℃,平衡时间：30 min；载气为N2；以DMF为溶剂对氢溴酸高乌甲素中乙醇、乙酸乙酯、三氯甲烷和苯的残留量进行测定。结果4种有机溶剂分离度良好,乙醇、乙酸乙酯、三氯甲烷和苯浓度分别在129.2-1033μg·mL-1（r=0.999）、120.5-964.2μg·mL-1（r=0.999）、3.32-26.5μg·mL-1（r=0.998）、0.14-1.13μg·mL-1（r=0.997）范围内线性关系良好；平均回收率（n=9）分别为97.4%、97.4%、96.8%、98.1%,RSD 分别为1.3%、2.0%、1.7%、3.1%。结论本文建立的顶空毛细管气相色谱法,经方法学验证可用于氢溴酸高乌甲素中有机溶剂残留量的测定,可作为该药质量标准修订的参考。

Establishment of HS-GC Method for Determination of Residual Solvents in Lappaconite Hydrobrom

Objective To establish a headspace gas chromatography method for determination of four residual solvents in lappaconite hydrobrom.Methods The residual solvents in lappaconite hydrobrom were separated on the DB-624 column （30 m × 0.53 mm,3μm）with an FID detector.The injector temperature and the detector temperature were set at 200 ℃and 250 ℃.The initial temperature was 40 ℃and kept for 7 min, the temperature was then raised to 200 ℃ at the rate of 25 ℃· min-1 and lasted 1 min.The containers of headspace injector were in equilibrium for 30 min at 80 ℃.The DMF was used as the solvent to determine the four residual solvents in lappaconite hydrobrom.Results Four residual solvents were completely separated. Good linearities of the four solvents were obtained within the range of 129.2-1033μg·mL-1 （r=0.999）, 120.5-964· 2 μg.mL-1 （r=0.999）,3.32-26.5 μg · mL-1 （r=0.998）,0.14-1.13μg· mL-1 （r=0.997）.The average recoveries （n=9 ）of ethanol,ethyl acetate,chloroform,benzene were 97.4%, 97.4%,96.8%,98.1% and the RSDs were 1.3%,2.0%,1.7%,3.1%,respectively.Conclusion The established method was in accordance with the requirements of the methodology validation which can be used for the determination of four residual solvents in lappaconite hydrobrom,and can provide a reference for the drug quality standard revision.