气相色谱法测定甘油中杂质乙二醇与二甘醇的含量

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=0.9998),平均回收率101.80％,RSD 1.6％;二甘醇线性回归方程为YDEG=0.004 2X-0.0457(r =0.9998),平均回收率98.95％,RSD 1.9％.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.

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

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.