液相色谱-高分辨质谱快速测定奶粉中氯丙醇酯  

Rapid determination of chloropropanol ester in milk powder by liquid chromatography-high-resolution mass spectrometry

作　　者：周洁 孙骥 余晓玲 于子丰 李双 ZHOU Jie;SUN Ji;YU Xiaoling;YU Zifeng;LI Shuang(Ningbo Zhongsheng Product Testing Company,Ningbo,315040,China;Ningbo Customs Technology Center,Ningbo,315040,China)

机构地区：[1]宁波中盛产品检测有限公司,宁波315040 [2]宁波海关技术中心,宁波315040

出　　处：《环境化学》2022年第7期2458-2460,共3页Environmental Chemistry

摘　　要：通过优化提取和净化过程建立了奶粉中氯丙醇酯的分级提取净化体系,并通过高效液相色谱-四极杆静电场轨道阱高分辨质谱技术(HPLC-Q-Orbitrap-HRMS)对该体系效果进行评价。实验采用在提取出的脂肪中加入内标再进行前处理的做法,第一级采用甲醇振荡提取、C_(18)固相萃取柱净化,可完成对缩水甘油酯和部分氯丙醇单酯的提取和净化工作,第二级采用甲醇提取,二氯甲烷辅助提取,中性氧化铝粉净化,去除油脂干扰的同时,可完成对氯丙醇双酯的提取与净化,通过合并第一、二级提取液,即可实现对奶粉中氯丙醇酯的高通量筛查,方法检出限为0.02 mg·kg^(−1),定量限为0.05 mg·kg^(−1),回收率≥80.6%,标准偏差低于10%,该方法对高蛋白、高脂肪的奶粉基质具有较强的适用性。A system of sequential extraction and purification coupled with UHPLC-Q-Orbitrap-HRMS detection applied to the analysis of chloropropanol ester with very different physicochemical properties in milk powder was established.The experiment added internal labeling to the extracted fat.In the first-stage of extraction,the glycidyl esters and partial chloropropanol monoesters were extracted with methanol and purified effectively by C_(18),in the second-stage of extraction,the chloropropanol diester were mainly extracted with methanol-dichloromethane and purified effectively by Alumina-N.The detection limit was 0.02 mg·kg^(−1),quantification limit was 0.05 mg·kg^(−1),the recoveries more than 80.6%,the standard deviation is less than 10%.The method has strong applicability for high protein,high fat milk powder matrix.

关 键 词：氯丙醇酯 高通量筛查 四极杆/静电场轨道阱高分辨质谱(Q-Orbitrap HRMS) 

分 类 号：O657.63[理学—分析化学] TS252.51[理学—化学]