甘油催化加氢制备1,2-丙二醇液相产物的气相色谱分析

Determination of liquid products from the hydrogenolysis of glycerol to 1,2-propanediol using gas chromatography

采用气相色谱-电子轰击离子源质谱(GC-MS)与比较标准品色谱保留值技术,确定了甘油催化加氢制备1,2-丙二醇液相产物的组成。优化了气相色谱-氢火焰离子法(GC-FID)的色谱条件,使主产物与副产物同时达到最佳分离。以正戊醇为内标物,建立了同时检测甘油催化加氢产物中7种醇类化合物的气相色谱分析方法。在分析方法的线性范围内,各化合物加标回收率均在94.4%～112.6%之间,相对标准偏差(RSD)在1.5%～7.2%之间。反应产物中乙醇、异丙醇、丙醇和丙酮醇的方法最小检出限(LOD)小于0.05μg/g,乙二醇、1,2-丙二醇和甘油的LOD分别为0.21μg/g,0.23μg/g和0.25μg/g,线性相关系数均大于等于0.9957。

A method to determine the liquid products from the hydrogenolysis of glycerol to 1,2-propanediol was studied.The products were identified by using gas chromatography coupled with electron impact ionization mass spectrometric detection（GC-MS） and the comparison of the retention time in chromatography of standard analysis.The analytic conditions of the gas chromatography coupled with a hydrogen flame ionization detector（GC-FID） were optimized to simultaneously achieve the optimal separation of the main products and byproducts.An analytic method for the simultaneous detection of 7 kinds of alcohols in the liquid products from the catalytic hydrogenation of glycerol was established with 1-pentanol as an internal standard.The results showed that in the linear range,the recoveries were between 94.4% and 112.6% with the relative standard deviations（RSD） between 1.5% and 7.2%.The limit of the detections（LOD） of the method for the determination of ethanol,1-propanol,isopropanol and hydroxyacetone were less than 0.05 μg/g,and the LOD for ethylene glycol,1,2-propanediol and gylcerol were 0.21 μg/g,0.23 μg/g and 0.25 μg/g,respectively.The correlation coefficients（R2） of all products were larger than 0.9957.