超高效液相色谱-串联质谱法测定聚氯乙烯食品接触材料中3种柠檬酸酯增塑剂  

Determination of three citrate ester plasticizers in PVC plastic food contact materials by ultra-high performance liquid chromatography-tandem mass spectrometry

作　　者：姚美伊[1] 凌云[1] 邓伟 姚桂红 雍炜[1] 何佩霞 邢仕歌[1] 张峰[1] YAO Meiyi;LING Yun;DENG Wei;YAO Guihong;YONG Wei;HE Peixia;XING Shige;ZHANG Feng(Chinese Academy of Inspection and Quarantine,Key Laboratory of Food Quality and Safety for State Market Regulation,Beijing 100176,China)

机构地区：[1]中国检验检疫科学研究院,国家市场监管重点实验室食品质量与安全,北京100176

出　　处：《中国食品卫生杂志》2023年第7期1000-1005,共6页Chinese Journal of Food Hygiene

基　　金：中央级公益性科研院所基本科研业务费专项(2020JK003)。

摘　　要：目的建立超高效液相色谱-串联质谱法测定聚氯乙烯食品接触材料中3种柠檬酸酯类增塑剂的方法。方法采用正己烷/二氯甲烷(1∶1,V/V)提取,经硅胶固相萃取柱净化,乙腈/乙酸乙酯(1∶4,V/V)洗脱,进入UPLCMS/MS分析,以乙腈和超纯水做流动相,经BEH C18色谱柱(2.1 mm×50 mm,1.7μm)分离,采用ESI源在MRM正离子模式下检测,外标法定量。结果3种化合物在线性范围内决定系数R2>0.996,方法检出限0.1~0.6μg/kg,定量限0.3~2.2μg/kg,回收率为70.3%~103.1%,相对标准偏差为0.9%~9.8%。结论该方法分析快速、灵敏、准确,适用于塑料材料中柠檬酸酯类增塑剂含量的检测,为新型增塑剂的添加使用监管提供方法。Objective To establish an analytical method for determination of three types of citrate ester plasticizers in PVC plastic food contact materials using ultra-high performance liquid chromatography-tandem mass spectrometry.Methods The samples were extracted with n-hexane/dichloromethane(1∶1,V/V),purified via silica gel solid phase extraction column,eluted using acetonitrile/ethyl acetate(1∶4,V/V),added into a UPLC-MS/MS system,separated by BEH C18 column(2.1 mm×50 mm,1.7μm)with acetonitrile and ultrapure water as mobile phase,detected using an ESI source in MRM positive ion mode,and quantified using an external standard.Results The linear relationship of the method was good and the coefficient of determination(R2)was greater than 0.996.The limits of detection were 0.1-0.6μg/kg,and the limits of quantitation were 0.3-2.2μg/kg.The recoveries of the three types of citrate esters plasticizers were 70.3%-103.1%,and the relative standard deviations(RSDs)(n=6)were 0.9%-9.8%.Conclusion The proposed method is highly sensitive,rapid,and highly applicable,and can meet the requirements for the detection of citrate ester plasticizers in plastic materials,which provides a means to supervise the addition of new plasticizers.

关 键 词：食品接触材料 柠檬酸酯增塑剂 聚氯乙烯 超高效液相色谱-串联质谱 

分 类 号：R155[医药卫生—营养与食品卫生学]