Acta Agriculturae Zhejiangensis ›› 2024, Vol. 36 ›› Issue (3): 643-650.DOI: 10.3969/j.issn.1004-1524.20230307

• Quality and Safety of Agricultural Products • Previous Articles     Next Articles

Critical control points of ID-LC-MS/MS method for the determination of fipronil-sulfone residues in eggs based on the evaluation of uncertainty

ZHANG Qiaoyan1,2(), FANG Weihuan2, ZHENG Weiran1, WANG Xiajun1, LIU Chaogang3, WANG Qiang1,*()   

  1. 1. Institute of Agro-Product Safety and Nutrition, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China
    2. College of Animal Sciences, Zhejiang University, Hangzhou 310058, China
    3. Institute of Crops and Nuclear Technology Utilization, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China
  • Received:2023-03-10 Online:2024-03-25 Published:2024-04-09

Abstract:

In order to control the accuracy of the detection results, the “Bottom-up” method and a national certified reference material [GBW(E)100779] were used to carry out the measurement uncertainty evaluation on the determination of fipronil-sulfone in egg powder by PAC cartridge-based cleanup and isotope dilution-liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS). The “fish-bone” diagram analysis showed that the main sources of uncertainty components were the sample weighing amount, the volume of internal standard solution added, the concentration of standard working solution and the volume taken. The uncertainty introduced by the addition volume of the internal standard solution was the largest, contributing 68.59% to the uncertainty of the detection results. The uncertainty introduced by the microbalance weighing, which is one in ten thousand, can be neglected. The addition process of the isotope internal standard is a key control point for the ID-LC-MS/MS method, and the reasonable selection of the reference benchmark and the complete extraction of the target substance are prerequisites for accurate measurement. Furthermore, the applicability of the reference material, diluent solvent, and internal standard solution was evaluated using LC-MS/MS method, and the extraction method was optimized based on the national certified reference material [GBW(E)100779]. The research results are beneficial to improving the detection quality and quality control level of egg food safety, and provide new ideas for the design of precise detection quality control schemes.

Key words: measurement uncertainty, egg, fipronil-sulfone, isotope dilution-liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS), quality control, reference material

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