QuEChERS—气相色谱—质谱联用法测定水果中23种邻苯二甲酸酯  

Determination of 23 Phthalates in Fruits by Gas Chromatography-Mass Spectrometry with QuEChERS

作　　者：朱鲜燕 邓尚贵 周勇 史美佳 祝世军 汪业勇 虞淼 许景景 ZHU Xianyan;ZHU Shanggui;ZHOU Yong(School of Food and Pharmacy of Zhejiang Ocean University,Zhoushan 316022;Zhoushan Institute of Food and Drug Inspection and Testing,Zhoushan 316012,China)

机构地区：[1]浙江海洋大学食品与药学学院,浙江舟山316022 [2]舟山市食品药品检验检测研究院,浙江舟山316012 [3]浙江省海洋地质调查大队,浙江舟山316099 [4]浙江省植保检疫与农药管理总站,浙江杭州310009

出　　处：《浙江海洋大学学报(自然科学版)》2024年第6期487-495,共9页Journal of Zhejiang Ocean University:Natural Science

基　　金：浙江省特支计划杰出人才项目(2021R51006);浙江省市场监督管理局科研计划项目(20200342)

摘　　要：建立了同时测定水果中23种邻苯二甲酸酯(PAEs)的QuEChERS—气相色谱—质谱联用分析方法。样品用乙酸乙酯和乙腈(7:3)复合溶剂提取后,经PSA和Alumina (3:7)填料净化,采用HP-5MS色谱柱程序升温分离,选择多反应监测模式(MRM)进行测定。该方法能有效分离23种邻苯二甲酸酯类化合物,其检出限为1.6~3.7μg·kg^(-1),定量限为3.2~7.4μg·kg^(-1),检测质量浓度线性范围为0~50 ng·mL^(-1),相关系数均大于0.996。23种邻苯二甲酸酯类的加标回收率为70.1%~108.9%,相对标准偏差为0.6%~9.2%。采用该方法对水果中邻苯二甲酸酯类塑化剂进行检测,实际样品中检出DMP、DEP、DIBP、DBP、DHP、DNOP,与GB 5009.271-2016《食品安全国家标准食品中邻苯二甲酸酯的测定》相比,检出值更高,证明该方法可满足水果的邻苯二甲酸酯检测需求。This article establishes a QuEChERS gas chromatography-mass spectrometry method for simultaneous determination of 23 Phthalates(PAEs)in fruits.The sample was extracted using a composite solvent of Ethyl acetate and Acetonitrile(7:3),purified with PSA and Alumina(3:7)packing,and separated using an HP-5MS column with temperature programmed separation.Multiple reaction monitoring mode(MRM)was selected for determination.This method can effectively separate 23 types of Phthalates compounds with a detection limit of 1.6-3.7μg·kg^(-1),with a quantification limit of 3.2-7.4μg·kg^(-1),the linear range of detected mass concentration is 0-50 ng·mL^(-1),and the correlation coefficients are all greater than 0.996.The recovery rates of 23 types of Phthalates were 70.1%-108.9%,with a relative standard deviation of 0.6%-9.2%.This method was used to detect Phthalate plasticizers in fruits,and DMP,DEP,DIBP,DBP,DHP,and DNOP were detected in actual samples.Compared with GB 5009.271-2016"National Food Safety Standard for the Determination of Phthalates in Food",the detection value was higher,proving that this method can meet the detection requirements of phthalates in fruits.

关 键 词：邻苯二甲酸酯 QuEChERS—气相色谱—质谱联用 复合溶剂 水果 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]