顶空气相色谱法测定阿魏酸哌嗪中有机溶剂残留量

Determination of residual organic solvents in piperazine ferulate by headspace gas chromatography

目的建立顶空气相色谱法测定阿魏酸哌嗪中乙醇、苯、吡啶共3种有机残留溶剂。方法采用顶空气相色谱法,以FID为检测器,使用DB-624（30 m×0.53 mm×3.00μm）毛细管色谱柱,程序升温,以氮气为载气,进样口温度200℃,检测器温度250℃,选择20%的N,N-二甲基甲酰胺为溶剂,配制对照品溶液及供试品溶液。结果 3种有机溶剂完全分离且峰型良好,在所考察的浓度范围内均具有良好的线性关系,相关系数r均〉0.9976,乙醇、苯、吡啶的检测限分别为1.26、0.07、7.86μg·m L-1,精密度RSD均〈5.0%,平均回收率（n=3）分别为98.3%~102.1%、97.5%~99.6%、98.6%~99.8%。结论本方法简便灵敏,结果准确可靠,适用于阿魏酸哌嗪原料药中有机溶剂残留量的检测。

Objective To establish a headspace gas chromatography method for the determination of 3 residual solvents（ethanol, benzene, pyridine） in piperazine ferulate. Methods The headspace gas chromatography method was used, FID detector combined with DB-624 columns（30 m×0.53 mm×3.00 μm）. The injector temperature and detector temperature were set at 200 ℃ and 250 ℃,respectively. The nitrogen was used as carrier gas and the 20% N, N-dimethylformamide was used as the solvent. Results Three solvents were separated completely. Good linear relationships of 3 solvents in each range of concentration were obtained, and all correlation coefficients were higher than 0.9976. The detector limit of ethanol, benzene, pyridine separately was 1.26, 0.07 and 7.86 μg·m L- 1, respectively. The RSD were all less than 5.0%. the average recovery（n = 3） separately were 98.3% ~ 102.1%、97.5% ~ 99.6%、98.6% ~ 99.8%. Conclusion The established method is simple, sensitive and reliable, and can be used for the detection of residual solvents in piperazine ferulate.