气相色谱法测定盐酸法舒地尔中有机溶剂残留量

目的建立气相色谱法测定盐酸法舒地尔中有机溶剂残留量的方法。方法采用气相色谱法,FID检测器,以毛细管色谱柱SE-54（30 m×0.53 mm,5.0μm）为分析柱。柱温为程序升温,用初始柱温55℃平衡0.5 min,以40℃/min的速度升温至70℃,平衡1 min,以40℃/min的速度升温至180℃,平衡3 min程序升温分别测定甲醇、二氯甲烷。用初始柱温50℃平衡3 min,以20℃/min的速度升温至180℃,平衡3min程序升温测定N,N-二甲基甲酰胺。载气为氮气,进样口温度200℃,检测器温度250℃。结果 3种有机溶剂完全分离,在所考察的浓度范围内具有良好线性关系,3个溶剂相关系数均大于0.999 0,甲醇、二氯甲烷、N,N-二甲基甲酰胺的检测限分别为0.065 7、1.100 0、0.016 6μg/mL,平均回收率分别为99.8%、98.4%、99.1%。结论本试验建立的方法简便灵敏,结果准确可靠,适用于盐酸法舒地尔原料药中有机溶剂残留量的检测。

Determination of the residual organic solvents in Fasudil hydrochloride by GC

Objective To establish a method for determination of residual organic solvents in Fasudil hydrochloride by headspace gas chromatography.Methods The residual solvents was determined by GC.The FID detector was adopted,SE-54 capillary column(30 m×0.53 mm,5.0 μm) was used,the column temperature was programmed temperature,the initial column temperature was 55℃ maintained for 0.5 minutes and then raised(40℃/min) to 70℃ for 1 minute,raised(40℃/min) to 180℃ for 3 minutes for methanol and methylene chloride detection,respectively.The initial column temperature was 50℃ maintained for 3 minutes and then raised(20℃/min) to 180℃ for 3 minutes for N,N-dimethyl formamide detection.The carriergas was nitrogen,the inlet temperature was 200℃ and the detector temperature was 250℃.Results Three kinds of organic solvents methanol,methylene chloride and N,N-dimethyl formamide completely separated,they showed a good linearity within the designed range of concentration,all the correlation coefficients were above 0.999 0.Methanol,methylene chloride and N,N-dimethyl formamide minimum detectable concentrations were 0.065 7,1.100 0,0.016 6 μg/mL,the recovery was 99.8%,98.4%,99.1%.Conclusion The method is accurate and sensitive,it can be used for the determination of the residual organic solvents in Fasudil hydrochloride.