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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 establish a method for the determination of methanol, dichloromethane and ethanol residues in fasudil hydrochloride. Methods Headspace capillary gas chromatography with Agilent HP-INNOWAX capillary column (30 m × 0.32 mm, 0.5μm) as the analytical column, the column temperature for the program temperature: the initial temperature of 35 ℃, holding 12min, 40 ℃ .min- 1 heated to 200 ℃ for 5 min; carrier gas was high purity nitrogen, the column flow rate 1.0 mL.min-1; gasification chamber temperature 200 ℃; FID detector, detection room temperature 250 ℃. Results The average recoveries of methanol, dichloromethane and ethanol measured by external standard method were 96.21%, 77.96% and 95.56%, respectively. Methanol, dichloromethane and ethanol residues detected in the sample are far below the limits set by the Pharmacopoeia. Conclusion The established method can effectively control the residues of methanol, dichloromethane and ethanol in the fasudil hydrochloride drug substance.