Rapid determination of broflanilide residues in animal-derived foods by QuEChERS purification combined with UPLC-MS/MS

  • ZHU Li ,
  • DENG Hang ,
  • YUAN Liejiang ,
  • WU Haizhi ,
  • CHEN Yao ,
  • XUE Minmin ,
  • WANG Xiu ,
  • ZHANG Kexin ,
  • LI Ge ,
  • SUN Yiqing ,
  • RAN Dan
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  • 1(Hunan Provincial Institute of Commodity Quality Inspection, Changsha 410007, China)
    2(Yueyang Inspection and Testing Center, Yueyang 410042, China)
    3(Changsha Institute for Food and Drug Control, Changsha 410007, China)

Received date: 2024-04-08

  Revised date: 2024-05-20

  Online published: 2024-10-10

Abstract

In this study, a QuEChERS purification combined with ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was established for the rapid quantification of broflanilide residues in animal-derived food.The samples were extracted and purified using the QuEChERS method, followed by extraction with acetonitrile containing 0.1% formic acid.The extract was subsequently purified using anhydrous magnesium sulfate, C18, and primary secondary amine, followed by centrifugation and membrane filtration prior to analysis.The UPLC-MS/MS method utilized acetonitrile and a 5 mmol/L ammonium acetate solution with 0.1% formic acid as the mobile phase, with a flow rate of 0.300 mL/min for gradient elution.Separation was achieved using an ACQUITY UPLC BEH C18 column, and electrospray ionization in positive ion mode was employed for ionization.The detection was performed in multiple reaction monitoring mode, and quantification was performed using the external standard method with matrix-matched standard curves.The results demonstrated that broflanilide residues displayed excellent linearity within the range of 0.200 to 100 μg/L, with correlation coefficients (R2) all exceeding 0.999. The method’s limits of quantification were 0.5-1.0 μg/kg.When animal-derived food was used as the matrix, at low, medium, and high spiked levels (2.0, 10.0, and 50.0 μg/kg), the average recovery rates for broflanilide residues ranged from 93.9% to 102%, with relative standard deviations ranging from 2.25% to 5.86%.The method is user-friendly, the experimental process is concise, and the detection accuracy is exceptional.It addresses the current gap in detecting broflanilide in animal-derived food, and offers technical support for establishing pesticide residue limits for broflanilide in animal-derived food.

Cite this article

ZHU Li , DENG Hang , YUAN Liejiang , WU Haizhi , CHEN Yao , XUE Minmin , WANG Xiu , ZHANG Kexin , LI Ge , SUN Yiqing , RAN Dan . Rapid determination of broflanilide residues in animal-derived foods by QuEChERS purification combined with UPLC-MS/MS[J]. Food and Fermentation Industries, 2024 , 50(17) : 336 -342 . DOI: 10.13995/j.cnki.11-1802/ts.039475

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