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

IF 3 3区农林科学 Q2 FOOD SCIENCE & TECHNOLOGY

Food Analytical Methods Pub Date : 2025-03-26 DOI:10.1007/s12161-025-02786-y

Abderrahim Eddahby, Abdelkarim Chahine, Lahcen Hssaini

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Abstract

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.

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稀释QuEChERS萃取物在LC-MS /MS分析食品中农药中的基质效应

在液相色谱-串联质谱（LC-MS /MS）农药残留分析中，基质效应（MEs）由于共萃取的基质成分导致信号抑制或增强而面临重大挑战。本研究评估了10倍稀释策略在10种食物基质（番茄、豆类、西葫芦、土豆、枣、胡萝卜、黄瓜、茴香、薄荷、苹果）中减轻90种农药微污染的效果。提取液采用改良的QuEChERS工艺制备，稀释后经UPLC-ESI-MS /MS分析。通过比较基质匹配和溶剂型校准曲线的斜率来定量MEs。结果表明，稀释显著降低了大多数基质的ME: 97%的农药在番茄中，92%的农药在西葫芦中，93%的农药在马铃薯中显示出可接受的ME值（±20%）。然而，药效随基质组成和农药性质的不同而不同。亲水农药（例如，乙酰甲胺磷，logP = - 0.85）在富含碳水化合物的基质（例如，枣，- 14% ME）中表现出抑制作用，而亲脂化合物（例如，吡虫蜱，logP = 4.7）在脂质密集的基质（例如，苹果，+ 48.4% ME）中表现出增强作用。25-27%的病例出现持续性MEs，如胡萝卜中的非那米酮（- 15% ME）和茴香中的甲氰菊酯（+ 63% ME），需要基质和分析物特异性干预。虽然稀释被证明对90%以上的病例有效，但对于异常情况，需要采用同位素标记标准等先进方法。这项工作验证了稀释作为常规农药分析的成本效益策略，平衡了食品中的敏感性和法规遵从性。

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来源期刊

Food Analytical Methods 农林科学-食品科技

CiteScore

6.00

自引率

3.40%

发文量

244

审稿时长

3.1 months

期刊介绍： Food Analytical Methods publishes original articles, review articles, and notes on novel and/or state-of-the-art analytical methods or issues to be solved, as well as significant improvements or interesting applications to existing methods. These include analytical technology and methodology for food microbial contaminants, food chemistry and toxicology, food quality, food authenticity and food traceability. The journal covers fundamental and specific aspects of the development, optimization, and practical implementation in routine laboratories, and validation of food analytical methods for the monitoring of food safety and quality.