气相色谱-质谱法测定乳制品中对苯二甲酸二辛酯  

Determination of Dioctyl Terephthalate in Dairy Products by GC-MS

作　　者：李雪银 黄孟丽 孙小杰 江改青 邢梦珂 LI Xueyin;HUANG Mengli;SUN Xiaojie;JIANG Gaiqing;XING Mengke(Nanjing Testing Institute for Food and Drug Control,Nanjing 210000,China)

机构地区：[1]南京市食品药品监督检验院,江苏南京210000

出　　处：《现代食品》2022年第2期183-186,193,共5页Modern Food

基　　金：国家重点研发计划项目“国际贸易重要食品的安全侦查与风险监控实验室应用示范”(2019YF C1605400)。

摘　　要：本文建立了一种灵敏、准确、快速的气相色谱-质谱法测定乳制品中对苯二甲酸二辛酯含量的定性定量分析方法。考察了提取试剂的类型、提取试剂的用量、超声的时间与温度等对回收率的影响,确定了最佳的前处理方法为:样品经5 mL正己烷25℃超声提取30 min,离心分离取上清液,气相色谱-串联质谱法检测,外标法定量。在此试验条件下,对苯二甲酸二辛酯在0.025~0.50μg·mL^(-1)呈良好的线性关系,线性相关系数(r^(2))不低于0.995,检出限为0.20 mg·kg^(-1),定量限为0.50 mg·kg^(-1)。在0.50μg·kg^(-1)、1.00μg·kg^(-1)、5.00μg·kg^(-1)3个加标水平下的回收率为95.1%~109.5%,相对标准偏差(RSD,n=6)为1.1%~3.2%。结果表明,该方法适用性强,灵敏度高,操作简单,可用于乳制品中对苯二甲酸二辛酯含量的检测,也可应用于其他含乳饮料中塑化剂的提取与检测。In this paper,a sensitive,accurate and rapid gas chromatography-mass spectrometry(GC-MS)method was proposed for the determination of dioctyl terephthalate in dairy products.The effects of the types of extraction reagent,the amount of extraction reagent,ultrasonic time and temperature on the recovery were investigated,and the best pretreatment method was determined.The samples were extracted with 5 mL n-hexane at 25℃for 30 min,and the supernatant was separated by centrifugation.The supernatant was detected by GC-MS and quantified by external standard method.Under these experimental conditions,dioctyl terephthalate showed a good linear relationship in the range of 0.025~0.50μg·mL^(-1),the linear correlation coefficient(r^(2))was not less than 0.995,the detection limit was 0.20 mg·kg^(-1),and the quantitative limit was 0.50 mg·kg^(-1).The recoveries were in the range of 95.1%~109.5%at the spiked levels of 0.50μg·kg^(-1),1.00μg·kg^(-1) and 5.00μg·kg^(-1),and the relative standard deviations(RSD,n=6)were in the range of 1.1%~3.2%.The results show that the method has strong applicability,high sensitivity and simple operation.This method can be used to detect the content of dioctyl terephthalate in dairy products,and can also be used to extract and detect plasticizers in other milk beverages.

关 键 词：气相色谱-质谱法(GC-MS) 乳制品 对苯二甲酸二辛酯 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]