色谱

色谱 ›› 2016, Vol. 34 ›› Issue (7): 708-714.DOI: 10.3724/SP.J.1123.2016.01012

• 特别策划:出入境检验检疫系统专栏(2016) • 上一篇    下一篇

固相萃取-液相色谱-串联质谱法测定食品包装材料中16种全氟烷基类化合物

何建丽1,2, 彭涛1, 谢洁1,3, 胡雪艳1, 常巧英1, 陈辉1, 范春林1, 李存2   

  1. 1. 中国检验检疫科学研究院, 北京 100176;
    2. 天津农学院动物科学与动物医学学院, 天津 300384;
    3. 中国农业大学动物医学院, 北京 100193
  • 收稿日期:2016-01-10 出版日期:2016-07-08 发布日期:2013-02-05
  • 通讯作者: 彭涛, 李存
  • 基金资助:

    国家科技基础性工作专项(2013FY113100).

Determination of 16 perfluorinated alkyl substances in food packaging materials by solid phase extraction-liquid chromatography-tandem mass spectrometry

HE Jianli1,2, PENG Tao1, XIE Jie1,3, HU Xueyan1, CHANG Qiaoying1, CHEN Hui1, FAN Chunlin1, LI Cun2   

  1. 1. Chinese Academy of Inspection & Quarantine, Beijing 100176, China;
    2. College of Animal Science and Veterinary Medicine, Tianjin Agricultural University, Tianjin 300384, China;
    3. College of Veterinary Medicine, China Agricultural University, Beijing 100193, China
  • Received:2016-01-10 Online:2016-07-08 Published:2013-02-05
  • Supported by:

    National Special Technology Base Work (No. 2013FY113100).

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摘要：

建立了使用固相萃取-液相色谱-串联质谱(SPE-LC-MS/MS)同时检测食品包装材料中16种全氟烷基类化合物(PFAS)的方法。分别对样品前处理方法、质谱条件等进行了比较和优化,样品用甲醇超声提取,经Oasis WAX固相萃取小柱净化后,用Atlantis T3 C18色谱柱分离,以乙腈和5 mmol/L乙酸铵溶液为流动相进行梯度洗脱,多反应监测(MRM)负离子模式扫描,同位素内标法和外标法结合定量。16种PFAS在0.5~20.0 μg/L范围内线性关系良好,相关系数(r2)均大于0.99。加标回收率为68.6%~109.2%,RSD为2.5%~18.1%(n=6)。检出限为0.2~0.5 μg/kg,定量限为0.5~1.0 μg/kg。该方法简便、快速、准确,可用于食品包装材料样品中PFAS的检测。

关键词: 包装材料, 固相萃取, 全氟烷基类化合物, 液相色谱-串联质谱

Abstract:

A method for the simultaneous determination of 16 perfluorinated alkyl substances (PFAS) in food packaging materials by solid phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) was developed. Comparison and optimization of the sample pretreatment methods, mass spectrometry and other conditions were carried out. The samples were ultrasonically extracted with methanol, followed by clean-up using an Oasis WAX SPE column. The analytes were separated on a reversed phase Atlantis T3 C18 column and eluted gradiently with acetonitrile and 5 mmol/L ammonium acetate. The analytes were quantified using isotope internal standard and isotope external standard calibration curve method. The linear calibration curves were obtained in the range of 0.5-20.0 μg/L with the linear relative coefficients more than 0.99. The recoveries were in the range of 68.6%-109.2% and the relative standard deviations (RSDs) were ranged from 2.5% to 18.1% (n=6). The limits of detection (LODs) and the limits of quantification (LOQs) for the PFAS were 0.2-0.5 μg/kg and 0.5-1.0 μg/kg, respectively. This method is simple, rapid, accurate and can be used in the determination of PFAS in food packaging materials.

Key words: food packaging materials, liquid chromatography-tandem mass spectrometry (LC-MS/MS), perfluorinated alkyl substances (PFAS), solid phase extraction (SPE)

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