色谱

色谱 ›› 2014, Vol. 32 ›› Issue (7): 723-729.DOI: 10.3724/SP.J.1123.2014.03023

• 研究论文 • 上一篇    下一篇

聚酰胺固相萃取-超高效液相色谱-串联质谱法同时检测饲料中的6种全氟化合物

林钦1,2, 付凤富1, 陈国南1, 郑小严2, 戴明2   

  1. 1. 福州大学食品安全分析与检测教育部重点实验室, 福建 福州 350116;
    2. 福建省产品质量检验研究院, 福建 福州 350002
  • 收稿日期:2014-03-17 修回日期:2014-05-09 出版日期:2014-07-08 发布日期:2014-06-25
  • 通讯作者: 林钦，E-mail：phlqfcii@126.com.
  • 基金资助:

    国家质量监督检验检疫总局科技计划项目（2012QK029）.

Simultaneous determination of six perfluorinated organic compounds in feed by using polyamide solid-phase extraction with ultra performance liquid chromatography-tandem mass spectrometry

LIN Qin1,2, FU Fengfu1, CHEN Guonan1, ZHENG Xiaoyan2, DAI Ming2   

  1. 1. Key Laboratory of Analysis and Detection for Food Safety of Ministry of Education, Fuzhou University, Fuzhou 350116, China;
    2. Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China
  • Received:2014-03-17 Revised:2014-05-09 Online:2014-07-08 Published:2014-06-25

PDF

419

被引次数

18

摘要：

建立了饲料中6种全氟化合物的聚酰胺固相萃取-超高效液相色谱-串联四极杆质谱分析法。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，甲醇淋洗净化，5%（v/v）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（UPLC-MS/MS）检测。分析柱为Acquity BEH C18（100 mm×2.1 mm，1.7 μm）；流动相为5 mmol/L乙酸铵-乙腈梯度洗脱；在最佳实验条件下，采用多反应监测负离子模式测定，同位素内标法定量。该方法对6种全氟化合物的检出限均小于0.1 μg/kg；对6种饲料及原料的加标回收率为94.2%~108.9%，精密度（RSD）为1.8%~8.6%（n=6）；在0.5~25 μg/L范围内均呈良好的线性关系，线性回归系数r>0.995。该方法前处理成本低，效果好，适合复杂基质样品的检测。

关键词: 超高效液相色谱-串联质谱, 聚酰胺固相萃取, 全氟有机化合物, 饲料

Abstract:

A method for the determination of six perfluorinated organic compounds (PFCs) in feed has been developed. It is based on polyamide solid-phase extraction (SPE) together with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted by acidified acetonitrile. The extraction solution was enriched by a polyamide SPE cartridge under acidic condition, and cleaned-up using methanol, eluted by 5%(v/v) ammonia/methanol solvent and determined by UPLC-MS/MS. The UPLC separation was carried out on an Acquity BEH C18 column (100 mm×2.1 mm, 1.7 μm). The mobile phases were 5 mmol/L ammonium acetate and acetonitrile with a gradient elution. Under the optimal conditions, the PFCs were analyzed under multiple reaction monitoring (MRM) mode with negative electrospray ionization. The isotope internal standard method was used to determine the six PFCs, and improve the quantitative accuracy. All of the target compounds exhibited good linearity (r>0.995) over a concentration range of 0.5-25 μg/L. The detection limits of the six PFCs were all smaller than 0.1 μg/kg. The mean recoveries of the six PFCs were in the range of 94.2% to 108.9% with the relative standard deviations (RSDs) of 1.8%-8.6% (n=6). The method for the determination of PFCs in feed is low-cost, favorable effect and suitable for the detection of complex matrix samples.

Key words: feed, perfluorinated organic compounds (PFCs), polyamide solid-phase extraction, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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