改进的QuEChERS-UPLC-MS/MS法测定动物源性食品中13种全氟化合物

王莹; 杜思宇; 张红; 张玉慧; 李玲; 王颜红; 李国琛

doi:10.13386/j.issn1002-0306.2020030192

改进的QuEChERS-UPLC-MS/MS法测定动物源性食品中13种全氟化合物

1. 中国科学院, 沈阳应用生态研究所, 辽宁沈阳 110016;
2. 农业农村部农产品质量安全环境因子风险评估实验室(北京), 北京 100029

基金项目:

国家重点研发计划项目（2016YFD0401201）；特色农产品产地溯源方法开发及应用（2018SG-Y-07）。

详细信息

作者简介:
王莹(1979-),女,硕士,高级工程师,研究方向:农产品检测与安全评价,E-mail:wangy@iae.ac.cn。

通讯作者:
王颜红(1963-),女,硕士,研究员,研究方向:农产品安全与环境质量,E-mail:wangyh@iae.ac.cn

李国琛(1983-),女,博士,副研究员,研究方向:农产品安全与环境质量,E-mail:ligc@iae.ac.cn。

中图分类号: TS207.3
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出版历程
- 收稿日期: 2020-03-15
- 网络出版日期: 2021-01-07
- 刊出日期: 2020-12-31

Determination of Thirteen PFCs in Animal-derived Food by Improved QuEChERS Extraction Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

1. Institute of Applied Ecology, Chinese Academy of Sciences, Shenyang 110016, China;
2. Risk Assessment Laboratory on Environmental Factors of Agricultural Products Safety and Quality(Beijing), Ministry of Agriculture and Rural Affairs, Beijing 100029, China

摘要

摘要: 建立了超高效液相色谱-串联质谱法检测动物源性食品（肝脏、肾脏、肌肉）中13种全氟化合物的分析方法。样品经0.2%盐酸-乙腈振荡提取，N-丙基乙二胺（PSA）、十八烷基键合硅胶（C₁₈）和石墨化炭黑（GCB）3种吸附剂分散固相萃取净化，以2.5 mmol/L乙酸铵甲醇溶液-2.5 mmol/L乙酸铵水溶液为流动相，经Waters Atlantis T3色谱柱分离，电喷雾负离子扫描方式，多反应监测模式检测，同位素内标法定量。13种化合物在0.05~10 ng/mL范围内线性关系良好。方法检出限为0.02~0.05 μg/kg，定量限为0.06~0.15 μg/kg。在0.2、1、2 μg/kg三个添加浓度水平，13种全氟化合物平均回收率为62.3%~119.3%，相对标准偏差为3.5%~19.9%。该方法快速简单、准确度好、灵敏度高，适用于动物源性食品中13种全氟化合物的检测需求。
- 全氟化合物 /
- 液相色谱-串联质谱 /
- QuEChERS /
- 动物源性食品
Abstract: A method of ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-ESI-MS/MS)combined with improved QuEChERS was established for the determination of 13 perfluorinated compounds(PFCs)in animal-derived food. The samples were extracted with 0.2% hydrochloric acid acetonitrile and cleaned up with a sorbent mixture of N-propylethylenediamine(PSA),octadecyl bonded silica gel(C₁₈)and graphitized carbon black(GCB). The PFCs were separated by an Atlantis T3 reversed-phase column using gradient elution with a mixed solution of 2.5 mmol/L ammonium acetate methanol and 2.5 mmol/L ammonium acetate,and detected by electrospray ionization in negative mode using the multiple reaction monitoring(MRM)mode. The samples were quantified using isotope internal standard.The calibration curves of 13 PFCs were linear in the concentration range of 0.05~10 ng/mL. The limits of detection(LODs)were between 0.02 and 0.05 μg/kg,and the limits of quantitation(LOQs)were between 0.06 and 0.15 μg/kg. At the spiked levels of 0.2,1 and 2 μg/kg,the average recoveries were in the range of 62.3%~119.3%,with relative standard deviations(RSDs)of 3.5%~19.9%. With its simplicity,accuracy and high sensitivity,this method is suitable for the identification and quantification of 13 PFCs in animal-derived food.
- perfluorinated compounds(PFCs) /
- ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) /
- QuEChERS /
- animal-derived food

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