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.