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<p>Consumption of food containing residues of nitrofuran metabolites may pose potential risks to human health. Although many countries have prohibited the use of nitrofurans as veterinary drugs, their illegal application persists. The detection of nitrofuran (NF) metabolites is essential for ensuring food safety. In this study, we designed and synthesized a pair of novel isotope-coded derivatization (ICD) reagents, 2-(4-formylphenyl)-1-phenyl-1H-naphtho[1,2-d]imidazole (d<sub>0</sub>-PPIB) and 2-(4-formylphenyl)-1-(pentadeuteriophenyl)-1H-naphtho[1,2-d]imidazole (d<sub>5</sub>-PPIB), using phenyl as the isotope-coded group. With the aid of the ICD reagents, a sensitive and accurate method for determination of NFs using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was established. The instrumental analysis time is remarkably short, with the four target analytes separated within just 4&#xa0;min. The derivatization process was efficiently completed in only 15&#xa0;min using microwave-assisted techniques, substantially reducing the overall experimental duration. The method achieved excellent sensitivity, with detection limits ranging from&#xa0;0.011 to 0.019&#xa0;μg/L, and the measurement error ranged from −2.2 to 3.5%. The intra- and inter-day precision was consistently high, with relative standard deviations (RSDs) below&#xa0;5%.&#xa0;This ICD-based strategy effectively mitigates matrix effects while reducing costs and improving accuracy. Using one pair of ICD reagents (d<sub>0</sub>/d<sub>5</sub>-PPIB), multiple analytes are concurrently derivatized to generate their isotope-labeled internal standards, markedly decreasing commercial stable isotope-labeled (SIL) internal standard consumption. The method was successfully applied to quantify NF metabolites in three food samples.</p> Graphical abstract <p></p>

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A sensitive and accurate method for determination of nitrofurans metabolites in food samples by ultra-high performance liquid chromatography-tandem mass spectrometry with a pair of facile isotope-coded derivatization reagents

  • 期刊论文

  • 发表日期：

    2026年7月30日

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  • Xuedi Qi,
  • Zenghui Xu,
  • Zhongyin Ji,
  • Xiaojian Kong,
  • Zhiwei Sun

摘要

Consumption of food containing residues of nitrofuran metabolites may pose potential risks to human health. Although many countries have prohibited the use of nitrofurans as veterinary drugs, their illegal application persists. The detection of nitrofuran (NF) metabolites is essential for ensuring food safety. In this study, we designed and synthesized a pair of novel isotope-coded derivatization (ICD) reagents, 2-(4-formylphenyl)-1-phenyl-1H-naphtho[1,2-d]imidazole (d0-PPIB) and 2-(4-formylphenyl)-1-(pentadeuteriophenyl)-1H-naphtho[1,2-d]imidazole (d5-PPIB), using phenyl as the isotope-coded group. With the aid of the ICD reagents, a sensitive and accurate method for determination of NFs using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was established. The instrumental analysis time is remarkably short, with the four target analytes separated within just 4 min. The derivatization process was efficiently completed in only 15 min using microwave-assisted techniques, substantially reducing the overall experimental duration. The method achieved excellent sensitivity, with detection limits ranging from 0.011 to 0.019 μg/L, and the measurement error ranged from −2.2 to 3.5%. The intra- and inter-day precision was consistently high, with relative standard deviations (RSDs) below 5%. This ICD-based strategy effectively mitigates matrix effects while reducing costs and improving accuracy. Using one pair of ICD reagents (d0/d5-PPIB), multiple analytes are concurrently derivatized to generate their isotope-labeled internal standards, markedly decreasing commercial stable isotope-labeled (SIL) internal standard consumption. The method was successfully applied to quantify NF metabolites in three food samples.

Graphical abstract