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

关键词:  盐酸法舒地尔  有机溶剂残留量  毛细管气相色谱法  测定

Key words:  fasudil hydrochloride  residual organic solvent  capillary GC  determination

摘要:

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Agilent HP-INNOWAX毛细管柱(30 m´0.32 mm, 0.5 µm)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。

Abstract:

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(30 m´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.