硅胶柱色谱法去除天然维生素E中塑化剂研究  

Removal of phthalic acid esters(PAEs) from natural V_E by silica gel column chromatography

作　　者：王义永[1] 代志凯[1] 张莉华[1] 缪飞[1] 李祥清[1] 

机构地区：[1]浙江医药股份有限公司新昌制药厂,浙江新昌312500

出　　处：《中国油脂》2016年第4期83-86,共4页China Oils and Fats

摘　　要：天然VE是以植物油的脱臭馏出物为原料,经过酯化、分子蒸馏、萃取及色谱分离等提取而得。由于受环境、包装、加工过程等污染,植物油的脱臭馏出物中容易富集邻苯二甲酸酯类(PAEs)塑化剂。通过考察天然VE提取过程中塑化剂含量的变化规律,利用塑化剂与天然VE极性差异,采用硅胶柱色谱法去除天然VE中的塑化剂。结果表明:天然VE原料经过酯化-蒸馏后低沸点的塑化剂主要富集于脂肪酸甲酯中,而部分高沸点的塑化剂仍然残留于天然VE中;真空蒸馏后得到的天然VE上硅胶柱色谱分离,在硅胶色谱柱高径比10∶1、载样量15%、3 BV环己烷洗脱、1.5 BV20%乙酸乙酯-环己烷及1 BV乙酸乙酯的洗脱条件下,可以有效去除天然VE产品中的PAEs塑化剂,天然VE含量显著提高,达到80.5%,平均收率为85.7%。With vegetable oil deodorizer distillate as raw material,natural V_E was prepared by esterification,molecular distillation,extraction and chromatographic separation methods. Due to the pollution of environment,packaging and processing,phthalic acid esters（ PAEs） plasticizer was easily enriched in vegetable oil deodorizer distillate. The changing rule of plasticizer content in natural V_E extraction process was studied. Based on the polar differences between plasticizer and natural V_E ,plasticizer was removed from natural V_E by silica gel column chromatography method. The results showed that low- boiling plasticizer was mainly enriched in fatty acid methyl ester,while part of the high- boiling plasticizer was still remained in natural V_E after natural V_E raw material was treated by esterification- distillation. Natural V_E prepared by vacuum distillation was separated by silica gel column chromatography. Under the elution conditions of ratio of height to diameter of silica gel chromatographic column 1 ∶ 10,sample loading amount 15% and respective elution volume of cyclohexane,20% ethyl acetate- cyclohexane and ethyl acetate 3,1. 5 BV and 1 BV,PAEs plasticizer could be removed effectively from natural V_E ,especially the content of natural V_E increased significantly,up to 80. 52%,and the average yield was 85. 7%.

关 键 词：天然VE 邻苯二甲酸酯类 塑化剂 去除 硅胶柱色谱 

分 类 号：O652.6[理学—分析化学] TQ466.5[理学—化学]