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<p>In this study, a highly sensitive ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS) method was developed, optimized, and validated for the determination of more than 400 multiclass pesticides in major fruits, vegetables, herbs, spices, and cereals collected from various Egyptian governorates. Optimal performance—highest signal intensity and lowest matrix suppression—was achieved using 5 mM ammonium formate at pH 4 (aqueous phase) and 5 mM ammonium formate at pH 3 (organic phase). The method was validated across different commodities—according to SANTE guidelines, achieving excellent linearity correlation coefficients (R<sup>2</sup> ≥ 0.99), recoveries within 70–120%, relative standard deviation RSDs &lt; 20%, and a limit of quantification LOQ suitable for regulatory monitoring. The vast majority of analytes complied with SANTE guidelines performance criteria; while a limited number exhibited matrix-dependent deviations in specific commodities, matrix effects varied strongly between commodities, particularly in dry mint and hibiscus. A total of 591 samples collected between 2024 and 2025 were analyzed to assess pesticide prevalence in eight commonly consumed commodities. Of these, 36.2% were residue-free, 63.8% contained at least one detectable pesticide, and 18.4% exceeded Codex Alimentarius maximum residue limits (MRLs). Human health risk assessment, based on estimated daily intake (EDI) and Egyptian food-consumption rates, indicated that all individual HQ values remained below 1.0 across all eight commodities (overall range &lt; 0.01–0.60); the highest EDI recorded was 5.96 × 10<sup>−5</sup>&#xa0;mg/kg bw/day for isoprothiolane in rice (ADI = 0.010&#xa0;mg/kg bw/day; HQ = 0.596), while representative values for other commodities included tetraconazole in apple (EDI = 9.07 × 10⁻⁶ mg/kg bw/day; HQ = 0.227) and haloxyfop in dry mint (EDI = 9.29 × 10⁻⁷ mg/kg bw/day; HQ = 0.143), confirming no chronic dietary risk to Egyptian consumers.</p>

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Comprehensive Development, Optimization, and Application of a Multiresidue UPLC–MS/MS Method for Large-Scale Monitoring of Pesticide Residues and Dietary Risk Assessment in Egyptian Food Commodities

  • 期刊论文

  • 发表日期：

    2026年4月23日

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  • Ahmed Ezzat,
  • Hassan A. El-Gammal,
  • Rasha M. El Nashar

摘要

In this study, a highly sensitive ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS) method was developed, optimized, and validated for the determination of more than 400 multiclass pesticides in major fruits, vegetables, herbs, spices, and cereals collected from various Egyptian governorates. Optimal performance—highest signal intensity and lowest matrix suppression—was achieved using 5 mM ammonium formate at pH 4 (aqueous phase) and 5 mM ammonium formate at pH 3 (organic phase). The method was validated across different commodities—according to SANTE guidelines, achieving excellent linearity correlation coefficients (R2 ≥ 0.99), recoveries within 70–120%, relative standard deviation RSDs < 20%, and a limit of quantification LOQ suitable for regulatory monitoring. The vast majority of analytes complied with SANTE guidelines performance criteria; while a limited number exhibited matrix-dependent deviations in specific commodities, matrix effects varied strongly between commodities, particularly in dry mint and hibiscus. A total of 591 samples collected between 2024 and 2025 were analyzed to assess pesticide prevalence in eight commonly consumed commodities. Of these, 36.2% were residue-free, 63.8% contained at least one detectable pesticide, and 18.4% exceeded Codex Alimentarius maximum residue limits (MRLs). Human health risk assessment, based on estimated daily intake (EDI) and Egyptian food-consumption rates, indicated that all individual HQ values remained below 1.0 across all eight commodities (overall range < 0.01–0.60); the highest EDI recorded was 5.96 × 10−5 mg/kg bw/day for isoprothiolane in rice (ADI = 0.010 mg/kg bw/day; HQ = 0.596), while representative values for other commodities included tetraconazole in apple (EDI = 9.07 × 10⁻⁶ mg/kg bw/day; HQ = 0.227) and haloxyfop in dry mint (EDI = 9.29 × 10⁻⁷ mg/kg bw/day; HQ = 0.143), confirming no chronic dietary risk to Egyptian consumers.