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<p>This study presents a validated multi-residue analytical method for the simultaneous determination of 170 pesticides in bottled drinking water using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) in both positive and negative electrospray ionization modes. Solid-phase extraction (SPE) with a C18 sorbent was used to concentrate and clean up the samples. Method performance was assessed using procedural calibration over the range of 0.05–0.8&#xa0;µg/L, with correlation coefficients (R²) ≥ 0.99. The limit of quantification (LOQ) was 0.05&#xa0;µg/L for 138 pesticides and 0.1&#xa0;µg/L for 32 pesticides. Precision was generally acceptable, with RSD values below or close to 20% for most analytes, and recoveries were within 70–120% for most analytes. Compared with previously reported UHPLC-MS/MS multi-residue methods, the present method offers several analytical advantages: (i) broader scope with 170 pesticides across 11 chemical classes; (ii) lower LOQs (0.05&#xa0;µg/L) achieved with reduced sample volume (250 mL); (iii) procedural calibration using an internal standard for ESI+ analyses to reduce analytical variability, ESI− analytes were quantified by procedural calibration alone; and (iv) simultaneous sample preparation for both ESI <sup>+</sup> and ESI<sup>-</sup> modes within a single analytical workflow. Analysis of 42 real bottled water samples from Tehran revealed chlorpyrifos in 5 samples, all below the LOQ. This is the first large-scale study in Iran to apply this method across a wide range of pesticide classes, providing a sensitive tool for routine surveillance and compliance with national and international regulatory limits.</p>

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Monitoring of multi-class pesticides in bottled drinking water using UHPLC–MS/MS-ESI method

  • 期刊论文

  • 发表日期：

    2026年7月21日

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  • Mehdi Elmi,
  • Bahram Daraei,
  • Amin Mousavi Khaneghah,
  • Sima Tahmouzi,
  • Maryam Amirahmadi

摘要

This study presents a validated multi-residue analytical method for the simultaneous determination of 170 pesticides in bottled drinking water using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) in both positive and negative electrospray ionization modes. Solid-phase extraction (SPE) with a C18 sorbent was used to concentrate and clean up the samples. Method performance was assessed using procedural calibration over the range of 0.05–0.8 µg/L, with correlation coefficients (R²) ≥ 0.99. The limit of quantification (LOQ) was 0.05 µg/L for 138 pesticides and 0.1 µg/L for 32 pesticides. Precision was generally acceptable, with RSD values below or close to 20% for most analytes, and recoveries were within 70–120% for most analytes. Compared with previously reported UHPLC-MS/MS multi-residue methods, the present method offers several analytical advantages: (i) broader scope with 170 pesticides across 11 chemical classes; (ii) lower LOQs (0.05 µg/L) achieved with reduced sample volume (250 mL); (iii) procedural calibration using an internal standard for ESI+ analyses to reduce analytical variability, ESI− analytes were quantified by procedural calibration alone; and (iv) simultaneous sample preparation for both ESI + and ESI- modes within a single analytical workflow. Analysis of 42 real bottled water samples from Tehran revealed chlorpyrifos in 5 samples, all below the LOQ. This is the first large-scale study in Iran to apply this method across a wide range of pesticide classes, providing a sensitive tool for routine surveillance and compliance with national and international regulatory limits.