凝胶渗透色谱净化-高效液相色谱法测定油脂食品中的邻苯二甲酸酯类增塑剂  

Determination of phthalate plasticizers in foods by high performance liquid chromatography with gel permeation chromatographic clean-up

作　　者：张春雨 王辉[2] 张晓辉 马忠强 邓宛梅 胡克 丁明玉[2] 

机构地区：[1]北京莱伯泰科有限公司,北京101312 [2]清华大学化学系,北京100084

出　　处：《色谱》2011年第12期1236-1239,共4页Chinese Journal of Chromatography

基　　金：国家自然科学基金项目(No.21075074)

摘　　要：建立了油脂食品(方便面、油炸糕点、沙琪玛、食用油等)中5种主要邻苯二甲酸酯类增塑剂的凝胶渗透色谱(GPC)净化-高效液相色谱(HPLC)分析方法。食品样品用石油醚超声提取,经GPC净化后,采用反相HPLC进行分析。所用的分离柱为Labtech C18(250 mm×4.6 mm,5μm),以乙腈和水为流动相,梯度洗脱。方法的相关系数皆在0.997以上,目标物的检出限(信噪比为3计)为3.25～13.4μg/L。在50 mg/L添加水平时,目标物的加标回收率为70.4%～113.6%,相对标准偏差为0.3%～5.8%(n=3)。该方法简便、快捷、实用,可用于油脂食品中邻苯二甲酸酯类增塑剂的分析测定。A method of gel permeation chromatography-high performance liquid chromatography（GPC-HPLC） was established for the simultaneous determination of 5 main phthalate plasticizers in foods（edible oil,instant noodles,fried pastries,Saqima,etc.）.The samples were extracted with petroleum ether in an ultrasonator,purified by a GPC column,and analyzed by HPLC.The chromatographic separation was achieved on a Labtech-C18 column（250 mm×4.6 mm,5 μm） using acetonitrile and water mixture as the mobile phases in a gradient elution mode.The developed method exhibited a linear correlation coefficient of more than 0.997 and the detection limits of 3.25-13.4 μg/L.The spike recoveries were between 70.4% and 113.6% with the relative standard deviations（RSDs,n=3） of 0.3%-5.8% at the spiked level of 50 mg/L.This method is simple,rapid and practical,and can be used for the simultaneous determination of PAEs in grease food samples.

关 键 词：凝胶渗透色谱 高效液相色谱 邻苯二甲酸酯 增塑剂 油脂食品 

分 类 号：O658[理学—分析化学]