色谱

色谱 ›› 2018, Vol. 36 ›› Issue (7): 634-642.DOI: 10.3724/SP.J.1123.2018.01047

• 研究论文 • 上一篇    下一篇

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

张宪臣1, 张朋杰1, 时成玉1, 华洪波2, 容裕棠1, 卢俊文1, 杨芳1   

  1. 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
  • 收稿日期:2018-01-30 出版日期:2018-07-08 发布日期:2014-06-03
  • 通讯作者: 张宪臣,Tel:0760,88887380,E-mail:zhangxc@zs.gdciq.gov.cn
  • 基金资助:

    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）.

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

ZHANG Xianchen1, ZHANG Pengjie1, SHI Chengyu1, HUA Hongbo2, RONG Yutang1, LU Junwen1, YANG Fang1   

  1. 1. Inspection and Quarantine Technology Center of Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528403, China;
    2. Zhongshan Zhuoya Foreign Language School, Zhongshan 528401, China
  • Received:2018-01-30 Online:2018-07-08 Published:2014-06-03
  • Supported by:

    Science and Technology Plan Project of General Administration of Quality Supervision Inspection and Quarantine(AQSIQ) of China(No. 2015IK052);Social Public Welfare Project of Zhongshan City(No. 2017B1029);Science and Technology Plan Project of Entry-Exit Inspection and Quarantine Bureau of Guangdong(No. 2017GDK24).

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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 MG Ⅱ C18色谱柱（150 mm×2.0 mm，5 μm）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≥ 0.9950；检出限为0.1~1.0 μg/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。

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

Abstract:

An ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q Orbitrap HRMS) method was developed for the rapid determination of 48 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 0.9950. The limits of detection (LODs) ranged from 0.1 to 1.0 μg/kg. The average spiked recoveries of the 48 target compounds were between 71.2% and 108.8%, 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.

Key words: contaminants, food contact plastic products, microwave-assisted extraction, quadrupole/electrostatic field orbitrap high resolution mass spectrometry(Q Orbitrap HRMS), ultra performance liquid chromatography(UPLC)

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