顶空GC测定盐酸法舒地尔中残留溶剂

Determination of Residual Solvents in Fasudil Hydrochloride by Headspace GC

目的建立盐酸法舒地尔中甲醇、二氯甲烷和乙醇残留量的测定方法。方法采用顶空毛细管气相色谱法,以AgilentHP-INNOWAX毛细管柱(30 m×0.32 mm,0.5μm)为分析柱,柱温为程序升温:起始温度35℃,保持12min,以40℃.min-1升温至200℃,保持5 min;载气为高纯氮气,柱流速1.0 mL.min-1;气化室温度200℃;FID检测器,检测室温度250℃。结果外标法测得甲醇、二氯甲烷和乙醇的平均加样回收率分别为96.21%、77.96%和95.56%。样品中检测到的甲醇、二氯甲烷和乙醇残留量均远在药典规定的限量以下。结论建立的方法能有效控制盐酸法舒地尔原料药中甲醇、二氯甲烷和乙醇的残留量。

OBJECTIVE To develop a headspace gas chromatography method for determining residual organic solvents-methanol,dichloromethane,ethanol in fasudil hydrochloride.METHODS Headspace gas chromatography was added using an Agilent HP-INNOWAX capillary column（30m×0.32 mm,0.5 μm） with temperature programming.The initial column temperature was 35 ℃ maintained for 12 min and then raised（40 ℃·min-1） to 200 ℃ for 5 min with nitrogen gas as carrier and FID as detector.The flow of carrier is 1.0 mL·min-1.The injection port and detector temperature were 200 ℃ and 250 ℃,respectively.RESULTS With external standard method,the average recoveries of methanol,dichloromethane and ethanol were 96.21%,77.96% and 95.56%,respectively.And three solvent residuals in samples were less than the limits of Ch.P.CONCLUSION The method can be used for the determination of residual solvents in fasudil hydrochloride.