食品科学 ›› 2013, Vol. 34 ›› Issue (10): 241-245.

• 分析检测 • 上一篇    下一篇

聚酰胺固相萃取法在动物源食品中全氟辛酸和全氟辛烷磺酸检测中的应用研究

林钦   

  1. 福建省产品质量检验研究院,福建 福州 350002
  • 收稿日期:2012-01-31 修回日期:2013-03-27 出版日期:2013-05-25 发布日期:2013-05-07
  • 通讯作者: 林钦 E-mail:phlqfcii@126.com
  • 基金资助:

    福建省质量技术监督局科技研究项目

Determination of Perfluorooctanoic Acid and Perfluorooctane Sulphonic Acid in Foods of Animal Origin Using Polyamide Solid-Phase Extraction

LIN Qin   

  1. Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China
  • Received:2012-01-31 Revised:2013-03-27 Online:2013-05-25 Published:2013-05-07

摘要:

建立动物源食品中全氟辛酸(PFOA)和全氟辛烷磺酸(PFOS)的聚酰胺固相萃取法。样品采用酸化乙腈提取,在酸性条件下用聚酰胺固相萃取小柱富集、净化,5%氨水-甲醇溶液洗脱后采用超高效液相色谱-串联四极杆质谱检测。PFOA和PFOS在1~60ng/mL质量浓度范围内均呈良好的线性关系,r=0.9999。精密度在0.8%~6.2%之间(n=5);两种待测组分的检测限均为0.2μg/kg;对6种动物源食品的加标回收率在93.3%~102.8%之间。

关键词: 超高效液相色谱-串联四极杆质谱仪, 动物源食品, 全氟辛酸, 全氟辛烷磺酸, 聚酰胺固相萃取

Abstract:

A method for the extraction of perfluorooctanoic acid (PFOA) and perfluorooctane sulphonic acid (PFOS) in
foods of animal origin using polyamide solid-phase extraction (SPE) was developed. Samples were extracted with acidified
acetonitrile, cleaned up and enriched on a polyamide SPE cartridge under acidic conditions through elution with 5%
ammonia-methanol and determined by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/
MS). The calibration curves for PFOA and PEOS exhibited good linearity (r = 0.9999) in the concentration range of 1 to 60
ng/mL, and the detection limit of the developed method was 0.2 μg/kg for both compounds and the average recovery rates
were in the range of 93.3% to 102.8% with relative standard deviations (RSD) of 0.8% to 6.2%.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), animal-origin food, perfluorooctanoic acid (PFOA), perfluorooctane sulphonic acid (PFOS), polyamide solid-phase extraction

中图分类号: