对不同生产企业肾石通颗粒中乙醇残留量的检测

Determination of Ethanol Residual in Shenshitong Granules Produced by Different Manufacturers

目的采用气相色谱法,建立肾石通颗粒中乙醇残留量的检测方法。方法采用色谱柱为DB-624毛细管柱,进样口温度200℃,检测器(FID)温度220℃,程序升温的起始温度为40℃,保持2 min,以3℃/min的速率升至65℃,再以25℃/min的速率升至200℃,保持10 min;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。结果乙醇浓度在0.2~6μL/mL范围内线性关系良好,平均回收率为104.63%(RSD=0.30%,n=9)。不同生产企业的肾石通颗粒中存在乙醇残留的情况。结论气相色谱内标法简便、快速,可用于肾石通颗粒中乙醇残留量的测定,也可为生产企业关注生产工艺过程中乙醇加入量及残留量提供参考。

Objective To establish a method of residual solvent ethanol in shenshitong granules by gas chromatography.Methods The determination of ethanol residues was performed on DB-624 using the flame ionization detector,the temperature of injector and detector was 200℃and 220℃,the column temperature was set as 40℃initially,maintain for 2 min,and increased to 65℃with and increased to 65℃with the rate of 3℃/min,and then ramped up to 200℃with rate of 25℃/min maintaining for 10 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 0.2-6μL/mL.The average recovery was 104.63%(RSD=0.30%,n=9).Conclusion The method is simple and rapid,and can be used for quantitative determination of residual solvent menthol in shenshitong granules,and provide reference for the production enterprises to pay attention to the amount of ethanol added and residual in the production process.