微波辅助萃取-超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速测定食品接触塑料制品中48种污染物残留  

Rapid determination of 48 contaminant residues in food contact plastic products by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry coupled with microwave-assisted extraction

作　　者：张宪臣 张朋杰 时成玉 华洪波 容裕棠 卢俊文 杨芳 ZHANG Xianchen1 , ZHANG Pengjie1, SHI Chengyu1, HUA Hongbo2, RONG Yutang, LU Junwen1, YANG Fang1(1. fnspection and Quarantine Technology Center of Zhongshan Entry-Exit fnspection and Quarantine Bureau, Zhongshan 528403, China; 2. Zhongshan Zhuoya Foreign Language School, Zhongshan 528401, Chin)

机构地区：[1]中山出入境检验检疫局检验检疫技术中心,广东中山528403 [2]中山市卓雅外语学校,广东中山528401

出　　处：《色谱》2018年第7期634-642,共9页Chinese Journal of Chromatography

基　　金：国家质检总局科技计划项目(2015IK052);中山市社会公益重大项目(2017B1029);广东检验检疫局科技计划项目(2017GDK24)~~

摘　　要：利用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法(UPLC-Q Orbitrap HRMS)的同时定性定量功能,建立了食品接触塑料制品中48种污染物残留的检测方法。用甲醇提取目标化合物,经微波辅助萃取,采用CAPCELL PAK MGⅡC18色谱柱(150 mm×2.0 mm,5μm)分离,以0.04%(v/v)甲酸甲醇溶液和含0.04%(v/v)甲酸与20 mmol/L(v/v)乙酸铵的水溶液为流动相进行梯度洗脱,在加热电喷雾电离(HESI)源、全扫描/实时二级质谱(Full MS/dd-MS2)监测模式下进行检测。结果表明,48种目标化合物在各自范围内线性关系良好,相关系数(r)均≥0.995 0;检出限为0.1~1.0μg/kg;平均加标回收率为71.2%~108.8%,相对标准偏差为2.2%~11.8%(n=6)。该法具有操作简单快捷、灵敏度高等优点。An ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry（UPLC-Q Orbitrap HRMS） method was developed for the rapid determination of48 contaminant residues in food plastic packaging materials. The samples were extracted with methanol using microwave-assisted extraction. The separation of the 48 contaminants was performed on a CAPCELL PAK MG Ⅱ C18 column（150 mm×2. 0 mm,5 μm） with gradient elution. Methanol（containing 0. 04%（v/v） formic acid） and water（containing 0. 04%（v/v） formic acid and 20 mmol/L ammonium acetate）were used as mobile phases. The compounds were detected under the full scan/date dependent-MS/MS（Full MS/dd-MS2） mode with a heated electrospray ionization（HESI） source. The calibration curves were linear with correlation coefficients no less than 0. 995 0. The limits of detection（LODs） ranged from0. 1 to 1. 0 μg/kg. The average spiked recoveries of the 48 target compounds were between 71. 2% and108. 8%,with relative standard derivations（RSDs） ranging from 2. 2% to 11. 8%（n = 6）. Compared to previous methods,this method has advantages of simpler sample preparation and higher sensitivity.

关 键 词：超高效液相色谱 四极杆/静电场轨道阱高分辨质谱 微波辅助萃取 污染物 食品接触塑料制品 

分 类 号：O658[理学—分析化学]