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Determination of Fipronil and Four Metabolites in Foodstuffs of Animal Origin Using a Modified QuEChERS Method and GC–NCI–MS/MS

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Abstract

A sensitive, effective, and reliable method for the accurate determination of fipronil and four metabolites (fipronil carboxamide, fipronil sulfone, fipronil sulfide, and fipronil desulfinyl) in foodstuffs of animal origin (egg, milk, beef kidney, beef liver, chicken, and chicken liver) was developed by isotope dilution–gas chromatography–negative chemical ionization–tandem mass spectrometry (GC–NCI–MS/MS). Samples were purified by a modified QuEChERS method. Four isotopically labeled internal standards were added in the sample extraction process to compensate for the matrix effect. The average recoveries were 78.2–107.1% with RSD ≤ 8.5%. The limits of quantification (LOQs) were 0.2 μg kg−1 for fipronil carboxamide and fipronil sulfone and 0.1 μg kg−1 for fipronil, fipronil sulfide, and fipronil desulfinyl. At the same time, the fragmentation mechanism of the five target compounds was analyzed via mass spectral data to help identify the compounds.

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Funding

This work was supported by the Zhejiang Shuren University Basic Scientific Research Special Funds (2020XZ008).

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Authors and Affiliations

  1. College of Biology and Environmental Engineering, Zhejiang Shuren University, Hangzhou, 310015, China

    Chao Han, Caiqin Liu, Nan Wang & Changchun Fu

  2. Comprehensive Technical Service Center of Shaoxing Customs, Shaoxing, 312000, China

    Beizhen Hu

  3. Comprehensive Technical Service Center of Wenzhou Customs, Wenzhou, 325027, China

    Zhou Li

  4. College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou, 325035, China

    Yan Shen

Authors
  1. Chao Han
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  2. Beizhen Hu
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  3. Zhou Li
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  4. Caiqin Liu
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  6. Changchun Fu
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  7. Yan Shen
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Correspondence to Yan Shen.

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Chao Han declares that he has no conflict of interest. Beizhen Hu declares that she has no conflict of interest. Zhou Li declares that he has no conflict of interest. Caiqin Liu declares that she has no conflict of interest. Nan Wang declares that she has no conflict of interest. Changchun Fu declares that she has no conflict of interest. Yan Shen declares that she has no conflict of interest.

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Han, C., Hu, B., Li, Z. et al. Determination of Fipronil and Four Metabolites in Foodstuffs of Animal Origin Using a Modified QuEChERS Method and GC–NCI–MS/MS. Food Anal. Methods 14, 237–249 (2021). https://doi.org/10.1007/s12161-020-01872-7

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  • DOI: https://doi.org/10.1007/s12161-020-01872-7

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