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目的确定盐酸法舒地尔中乙醇和二氯甲烷残留量的检测方法。方法使用Agilent DB-1701毛细管柱(30 m×0.32 mm,0.25μm),柱温为程序升温:起始温度40℃,保持5 min,以39℃/min升温至200℃,保持15min;以高纯氮气为载气,柱流速为3.0 ml/min;气化室温度160℃;FID检测器,检测室温度280℃。结果外标法测得乙醇和二氯甲烷的平均回收率分别为90.7%和91.5%,样品中检测到的乙醇和二氯甲烷均满足药典规定。结论该方法准确、可靠、重现性好,可作为有效控制盐酸法舒地尔原料药中乙醇和二氯甲烷残留量的方法。
Objective To determine the method for the determination of ethanol and methylene chloride residues in fasudil hydrochloride. Methods The temperature of the column was programmed with an Agilent DB-1701 capillary column (30 m × 0.32 mm, 0.25 μm). The temperature was programmed at 40 ° C for 5 min. The temperature was raised to 200 ° C at 39 ° C / min for 15 min. Pure nitrogen as carrier gas, the column flow rate of 3.0 ml / min; gasification chamber temperature of 160 ℃; FID detector, detection chamber temperature 280 ℃. Results The average recoveries of ethanol and dichloromethane measured by the external standard method were 90.7% and 91.5%, respectively. Both ethanol and dichloromethane detected in the samples met the requirements of the Pharmacopoeia. Conclusion The method is accurate, reliable and reproducible. It can be used as a method to effectively control the residues of ethanol and dichloromethane in fasudil hydrochloride.