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<p>Matrix effects (MEs) in liquid chromatography-tandem mass spectrometry (LC–MS/MS) analysis of pesticide residues pose significant challenges due to signal suppression or enhancement caused by co-extracted matrix components. This study evaluates the efficacy of a 10-fold dilution strategy to mitigate MEs for 90 pesticides across 10 food matrices (tomato, bean, zucchini, potato, dates, carrot, cucumber, fennel, mint, apple). Extracts were prepared using a modified QuEChERS protocol, diluted, and analyzed via UPLC-ESI–MS/MS. MEs were quantified by comparing slopes of matrix-matched and solvent-based calibration curves. Results demonstrated that dilution significantly reduced MEs in most matrices: 97% of pesticides in tomato, 92% in zucchini, and 93% in potato exhibited acceptable ME values (± 20%). However, efficacy varied with matrix composition and pesticide properties. Hydrophilic pesticides (e.g., acephate, logP =  − 0.85) showed suppression in carbohydrate-rich matrices (e.g., dates, − 14% ME), while lipophilic compounds (e.g., chlorpyrifos, logP = 4.7) displayed enhancement in lipid-dense matrices (e.g., apple, + 48.4% ME). Persistent MEs occurred in 25–27% of cases, such as fenamidone in carrot (− 15% ME) and fenpropathrin in fennel (+ 63% ME), necessitating matrix- and analyte-specific interventions. While dilution proved effective for more than 90% of cases, outliers necessitate advanced methods like isotope-labeled standards. This work validates dilution as a cost-effective strategy for routine pesticide analysis, balancing sensitivity with regulatory compliance in food.</p>

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Assessing Matrix Effects in LC–MS/MS Analysis of Pesticides in Food Using Diluted QuEChERS Extracts

  • 期刊论文

  • 发表日期：

    2025年3月26日

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  • Abderrahim Eddahby,
  • Abdelkarim Chahine,
  • Lahcen Hssaini

摘要

Matrix effects (MEs) in liquid chromatography-tandem mass spectrometry (LC–MS/MS) analysis of pesticide residues pose significant challenges due to signal suppression or enhancement caused by co-extracted matrix components. This study evaluates the efficacy of a 10-fold dilution strategy to mitigate MEs for 90 pesticides across 10 food matrices (tomato, bean, zucchini, potato, dates, carrot, cucumber, fennel, mint, apple). Extracts were prepared using a modified QuEChERS protocol, diluted, and analyzed via UPLC-ESI–MS/MS. MEs were quantified by comparing slopes of matrix-matched and solvent-based calibration curves. Results demonstrated that dilution significantly reduced MEs in most matrices: 97% of pesticides in tomato, 92% in zucchini, and 93% in potato exhibited acceptable ME values (± 20%). However, efficacy varied with matrix composition and pesticide properties. Hydrophilic pesticides (e.g., acephate, logP =  − 0.85) showed suppression in carbohydrate-rich matrices (e.g., dates, − 14% ME), while lipophilic compounds (e.g., chlorpyrifos, logP = 4.7) displayed enhancement in lipid-dense matrices (e.g., apple, + 48.4% ME). Persistent MEs occurred in 25–27% of cases, such as fenamidone in carrot (− 15% ME) and fenpropathrin in fennel (+ 63% ME), necessitating matrix- and analyte-specific interventions. While dilution proved effective for more than 90% of cases, outliers necessitate advanced methods like isotope-labeled standards. This work validates dilution as a cost-effective strategy for routine pesticide analysis, balancing sensitivity with regulatory compliance in food.