色谱

色谱 ›› 2017, Vol. 35 ›› Issue (5): 495-501.DOI: 10.3724/SP.J.1123.2016.12016

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法测定蜂蜜中20种全氟烷基化合物

李帅1, 陈辉2, 金铃和2, 彭涛2, 范春林2, 王明林1   

  1. 1. 山东农业大学食品科学与工程学院, 山东 泰安 271018;
    2. 中国检验检疫科学研究院, 北京 100176
  • 收稿日期:2016-12-08 出版日期:2017-05-08 发布日期:2013-08-28
  • 通讯作者: 范春林,E-mail:caiqfcl@163.com;王明林,E-mail:mlwang@163.com.
  • 基金资助:

    国家科技基础性工作专项（2013FY113100）.

Determination of 20 perfluorinated alkyl substances in honey by high performance liquid chromatography- tandem mass spectrometry

LI Shuai1, CHEN Hui2, JIN Linghe2, PENG Tao2, FAN Chunlin2, WANG Minglin1   

  1. 1. College of Food Science and Engineering, Shandong Agricultural University, Tai'an 271018, China;
    2. Chinese Academy of Inspection and Quarantine, Beijing 100176, China
  • Received:2016-12-08 Online:2017-05-08 Published:2013-08-28
  • Supported by:

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

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摘要：

建立了高效液相色谱-串联质谱（HPLC-MS/MS）同时测定蜂蜜中20种全氟烷基化合物（PFASs）含量的分析方法。采用改进的QuEChERS方法对样品进行前处理，用含1.5%（v/v）甲酸的乙腈溶液振荡提取，C18和N-丙基乙二胺（PSA）吸附剂净化，Atlantis T3 C18色谱柱（150 mm×2.1 mm，3μm）分离，以含5 mmol/L乙酸铵的甲醇溶液和5 mmol/L乙酸铵溶液为流动相进行梯度洗脱。在电喷雾离子（ESI）源负离子模式下以多反应监测（MRM）扫描，采用同位素内标法进行定量分析。结果表明，20种PFASs在16 min内即可完成分离，在0.2~10μg/L范围内线性关系良好，相关系数（r）均大于0.99；检出限（LOD，S/N=3）和定量限（LOQ，S/N=10）分别为0.04~0.10μg/kg和0.10~0.20μg/kg。在0.1、0.5、1.0和2.0μg/kg加标水平下，20种PFASs的加标回收率为72.6%~113.0%，RSD为0.4%~15.9%（n=6）。该法快速、高效、准确，适用于蜂蜜样品中20种PFASs的同时检测。

关键词: QuEChERS方法, 蜂蜜, 高效液相色谱-串联质谱, 全氟烷基化合物

Abstract:

A sensitive method for simultaneous determination of 20 perfluorinated alkyl substances (PFASs) in honey was developed by QuEChERS-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The samples were extracted by acetonitrile with 1.5% (v/v) formic acid, and purified by C18 and N-propylethylenediamine (PSA) adsorbents. The separation of the 20 PFASs was performed on an Atlantis T3 C18 column using gradient elution with methanol containing 5 mmol/L ammonium acetate and 5 mmol/L ammonium acetate as mobile phases within 16 min. The PFASs were analyzed under the multiple reaction monitoring (MRM) mode with negative electrospray ionization (ESI-). Under the optimal conditions, the isotope internal standard method was used to quantify the contents of the 20 PFASs. The calibration curves were acquired in the concentration range of 0.2-10 μg/L with correlation coefficients (r) greater than 0.99. The limits of detection (LODs) and limits of quantitation (LOQs) ranged from 0.04 to 0.10 μg/kg and 0.10 to 0.20 μg/kg, respectively. The recoveries of the 20 PFASs spiked in blank honey samples were between 72.6% and 113.0% with relative standard derivations (RSDs) of 0.4%-15.9% (n=6). The developed method is rapid, efficient and accurate, and suitable for the simultaneous analysis of the 20 PFASs in honey samples.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), honey, perfluorinated alkyl substances (PFASs), QuEChERS

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