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中国精品科技期刊2020
王莹, 杜思宇, 张红, 张玉慧, 李玲, 王颜红, 李国琛. 改进的QuEChERS-UPLC-MS/MS法测定动物源性食品中13种全氟化合物[J]. 食品工业科技, 2021, 42(1): 239-249. DOI: 10.13386/j.issn1002-0306.2020030192
引用本文: 王莹, 杜思宇, 张红, 张玉慧, 李玲, 王颜红, 李国琛. 改进的QuEChERS-UPLC-MS/MS法测定动物源性食品中13种全氟化合物[J]. 食品工业科技, 2021, 42(1): 239-249. DOI: 10.13386/j.issn1002-0306.2020030192
WANG Ying, DU Si-yu, ZHANG Hong, ZHANG Yu-hui, LI Ling, WANG Yan-hong, LI Guo-chen. Determination of Thirteen PFCs in Animal-derived Food by Improved QuEChERS Extraction Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(1): 239-249. DOI: 10.13386/j.issn1002-0306.2020030192
Citation: WANG Ying, DU Si-yu, ZHANG Hong, ZHANG Yu-hui, LI Ling, WANG Yan-hong, LI Guo-chen. Determination of Thirteen PFCs in Animal-derived Food by Improved QuEChERS Extraction Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(1): 239-249. 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

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

  • 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。

     

    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.

     

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