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<p>A multiresidue method was developed and validated for the simultaneous determination of 25 multiclass pesticides in chicken, buffalo, pig, sheep, and goat meat matrices using a modified QuEChERS extraction coupled with LC–MS/MS analysis. Sample preparation involved acetonitrile extraction followed by dispersive solid-phase cleanup using primary secondary amine and C18 sorbents, together with a freezing-out step at -20&#xa0;°C to minimize lipid-related matrix-derived interferences. Satisfactory matrix-matched calibration linearity was achieved for all analytes over the range of 0.005–0.200&#xa0;mg&#xa0;kg⁻<sup>1</sup>, with coefficients of determination (R<sup>2</sup>) between 0.990 and 0.999. Matrix effects ranged from -17.7% to + 21.4%, indicating moderate signal suppression or enhancement that was effectively compensated by matrix-matched calibration. Mean recoveries across the five matrices ranged from 72.3% to 106.3%, while repeatability (%RSD) and within-laboratory reproducibility (%RSDwR) were generally below 4%, demonstrating satisfactory recovery and precision. Relative ion-ratio deviations at 10&#xa0;μg&#xa0;kg⁻<sup>1</sup> ranged from -11.9% to + 14.3%, remaining within SANTE’s identification criteria. Expanded measurement uncertainty ranged from 1.34% to 5.91%, confirming high confidence in quantitative results. Method performance was further verified through successful performance in a FAPAS proficiency testing scheme (z-score = 1.2). Analysis of 50 meat samples comprising buffalo, pig, chicken, goat, and sheep meat (10 samples from each species), collected from various marketplaces across Hyderabad, India revealed no detection of the target pesticide residues in any of the samples analyzed. The validated method proved suitable for routine monitoring of pesticide residues in animal-derived foods and provides a reliable tool for regulatory surveillance and food safety assessment.</p>

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Method Optimization and Validation for Pesticide Residue Analysis in Meat Matrices by Liquid Chromatography Tandem Mass Spectrometry

  • 期刊论文

  • 发表日期：

    2026年7月29日

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  • Muthukumar Muthupalani,
  • Kalpana S,
  • Jyothsna Yasur,
  • Umamaheswara Rao Chikkulla,
  • Kanchana Kommi,
  • Sukhadeo Baliram Barbuddhe,
  • Kaushik Banerjee

摘要

A multiresidue method was developed and validated for the simultaneous determination of 25 multiclass pesticides in chicken, buffalo, pig, sheep, and goat meat matrices using a modified QuEChERS extraction coupled with LC–MS/MS analysis. Sample preparation involved acetonitrile extraction followed by dispersive solid-phase cleanup using primary secondary amine and C18 sorbents, together with a freezing-out step at -20 °C to minimize lipid-related matrix-derived interferences. Satisfactory matrix-matched calibration linearity was achieved for all analytes over the range of 0.005–0.200 mg kg⁻1, with coefficients of determination (R2) between 0.990 and 0.999. Matrix effects ranged from -17.7% to + 21.4%, indicating moderate signal suppression or enhancement that was effectively compensated by matrix-matched calibration. Mean recoveries across the five matrices ranged from 72.3% to 106.3%, while repeatability (%RSD) and within-laboratory reproducibility (%RSDwR) were generally below 4%, demonstrating satisfactory recovery and precision. Relative ion-ratio deviations at 10 μg kg⁻1 ranged from -11.9% to + 14.3%, remaining within SANTE’s identification criteria. Expanded measurement uncertainty ranged from 1.34% to 5.91%, confirming high confidence in quantitative results. Method performance was further verified through successful performance in a FAPAS proficiency testing scheme (z-score = 1.2). Analysis of 50 meat samples comprising buffalo, pig, chicken, goat, and sheep meat (10 samples from each species), collected from various marketplaces across Hyderabad, India revealed no detection of the target pesticide residues in any of the samples analyzed. The validated method proved suitable for routine monitoring of pesticide residues in animal-derived foods and provides a reliable tool for regulatory surveillance and food safety assessment.