不同生产厂家阿魏酸哌嗪片中乙醇残留量的顶空气相色谱法检测

目的:建立阿魏酸哌嗪片中乙醇残留量的气相色谱检测方法。方法:采用色谱柱为聚乙二醇(PEG)毛细管柱(HP-Innowax,30 m×0.32 mm×0.5μm),进样口温度为200℃,检测器(FID)温度为250℃,程序升温的起始温度为40℃,以5℃/min的速率升至100℃,再以100℃/min的速率升至240℃,保持5 min;采用顶空分流进样,分流比为1∶1;顶空瓶平衡温度为85℃,平衡时间为20 min。结果:乙醇浓度处在1.05~527.47μg/mL范围内具有良好的线性关系,相关系数为1.000 0;平均回收率为99.74%,RSD为4.30%;测得4家生产企业阿魏酸哌嗪片中平均含醇量分别为0.02%、0.026%、0.02%和0.452%。结论:本法操作简单,结果准确,可适用于阿魏酸哌嗪片中乙醇残留量的检测。

Determination of Ethanol Residues in Piperazine FerulateTablets Produced by Different Manufacturers by Headspace-Gas Chromatography

Objective: To establish a method for determination of residual amounts of ethanol in piperazine ferulate tablets by headspace-gas chromatography. Methods: The determination of ethanol residues was performed on HP-Innowax capillary chromatographic column(30 m×0.32 mm×0.5 μm)using the flame ionization detector. The temperature of injector and detector was 200 ℃ and 250 ℃. The column temperature was set as 40 ℃ initially, and increased to 100 ℃with the rate of 5 ℃/min and then ramped up to 240 ℃ with the rate of 100 ℃/min maintaining for 5 min. The split ratio was 1: 1. Headspace equilibrium temperature was 85 ℃ and equilibration time was 20 min. Results: The calibration curve of ethanol showed a good linear relationship with the concentration being between 1.05 and 527.47 μg/mL. The average recovery was 99.74% with the RSD of 4.30%. The average ethanol content of piperazine ferulate tablets produced by 4 manufacturers were 0.02%, 0.026%, 0.02% and 0.452%, respectively. Conclusion: The established method could be applied for determination of ethanol residue in piperazine ferulate tablets with simple operation and accurate results.