气相色谱法测定甘油中杂质乙二醇与二甘醇的含量

Determination the Content of Ethylene Glycol and Diethylene Glycol in Glycerol Samples Using Gas Chromatography

目的:采用气相色谱(GC)法测定甘油样品中乙二醇与二甘醇的含量。方法:色谱柱为键合6%氰丙基-96%二甲基聚硅氧烷的毛细管柱(DB-624),采用程序升温方式,内标法进行定量。结果:乙二醇、二甘醇检测质量浓度在20.00～160.00 mg.L-1样品峰面积与内标峰面积比值与浓度线性关系良好,乙二醇线性回归方程为YEG=0.004X-0.025(r=0.999 8),平均回收率101.80%,RSD 1.6%;二甘醇线性回归方程为YDEG=0.004 2X-0.045 7(r=0.999 8),平均回收率98.95%,RSD1.9%。结论:方法简单、出峰时间短,可以更好地用于甘油的质量控制。

Objective： A gas chromatographic （GC） method for. ethylene glycol and diethylene glycol determination in glycerol samples was established. Method： 6% cyanopropyl-phenyl and 94% dimethyl polysiloxane capillary column （DB-624） was used. The internal standard method with temperature-programmed mode was used for quantitative analysis. Result： The sample peak area and the internal standard peak area ratio to the concentration of samples for both the ethylene glycol and the diethylene glycol had a good linear relation in the range of 20. 00-160. 00 mg ·L-1. The linear equation of ethylene glycol was YEG = 0. 004X - 0. 025 （ r = 0. 999 8 ）. The average recovery was 101.80% and RSD was 1.6% （n = 9）. The linear equation of diethylene glycol was YDEG = 0. 004 2X -- 0. 045 7 （r=0.999 8）. The average recovery was 98.95% and RSD was 1.9% （n=9） Conclusion： The method has a short peak retention time, which can be used for quality control of the glycerol.