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  • Title: [High-throughput screening of multi-pesticide residues in animal-derived foods by QuEChERS-online gel permeation chromatography-gas chromatography-tandem mass spectrometry].
    Author: Li J, Ju X, Wang YL, Tian QY, Liang XQ, Li HX, Liu YM.
    Journal: Se Pu; 2023 Jul; 41(7):610-621. PubMed ID: 37387282.
    Abstract:
    Improvements in living standards have led to an increase in the consumption of animal-derived foods. Pesticides may be used illegally during animal breeding as well as meat production and processing for pest control and preservation. Pesticides applied to crops may also be enriched in animal tissues through the food chain, thereby increasing the risk of pesticide residue accumulation in muscles and visceral tissues and endangering human health. China has stipulated maximum residue limits for pesticide residues in livestock and poultry meat and their viscera. Many other major developed countries and organizations, including the European Union, Codex Alimentarius Commission, and Japan, have also set maximum residue limits for these residues (0.005-10, 0.004-10, and 0.001-10 mg/kg, respectively). Research on pretreatment technologies for pesticide residue detection in plant-derived foods is widely available, but insufficient attention has been paid to animal-derived foods. Thus, high-throughput detection technologies for pesticide residues in animal-derived foods are limited. The impurities that can interfere with the detection process for plant-derived foods mainly include organic acids, polar pigments, and other small molecular compounds; by contrast, the matrix of animal-derived foods is much more complex. Macromolecular proteins, fats, small molecular amino acids, organic acids, and phospholipids can interfere with the detection of pesticide residues in animal-derived foods. Thus, selecting the appropriate pretreatment and purification technology is of great importance. In this study, the QuEChERS technique was combined with online gel permeation chromatography-gas chromatography-tandem mass spectrometry (GPC-GC-MS/MS) to determine 196 pesticide residues in animal-derived foods. The samples were extracted with acetonitrile, purified using the QuEChERS technique coupled with online GPC, detected by GC-MS/MS, determined in multiple reaction monitoring mode (MRM), and quantified using the external standard method. The effects of the extraction solvent and purification agent type on the extraction efficiency and matrix removal of the method were optimized. The purification effect of online GPC on the sample solution was investigated. The optimal distillate receiving time was obtained by studying the recoveries of the target substances and matrix effects over different distillate receiving periods to achieve the effective introduction of target substances and efficient matrix removal. Further, the advantages of the QuEChERS technique combined with online GPC were evaluated. The matrix effects of 196 pesticides were assessed; ten pesticide residues showed moderate matrix effects, while four pesticide residues showed strong matrix effects. A matrix-matched standard solution was used for quantification. The 196 pesticides showed good linearity in the range of 0.005-0.2 mg/L, with correlation coefficients greater than 0.996. The limits of detection and quantification were 0.002 and 0.005 mg/kg, respectively. The recoveries of 196 pesticides at spiked levels of 0.01, 0.05, and 0.20 mg/kg were 65.3%-126.2%, with relative standard deviations (RSDs) of 0.7%-5.7%. The proposed method is rapid, accurate, and sensitive; thus, it is suitable for the high-throughput screening and detection of multiple pesticide residues in animal-derived foods. 将QuEChERS技术与在线凝胶渗透色谱-气相色谱-串联质谱(GPC-GC-MS/MS)技术结合,建立了动物源性食品中196种农药残留的高通量检测方法。样品经乙腈提取、QuEChERS结合在线GPC净化后,进行GC-MS/MS检测,多反应监测模式(MRM)分析,外标法定量。方法优化了提取溶剂及净化剂类型,实现了目标物的高效提取和基质的有效去除;考察了在线GPC对样品溶液的净化作用。通过研究不同馏分接收时间段内目标物的回收率和基质效应,得出最佳馏分接收时间,实现目标物的有效导入和基质的高效去除,并对QuEChERS-GPC联用技术的优势进行了评价。该方法研究了196种农药的基质效应,其中10种农药表现为中等强度基质效应,4种农药为强基质效应。本研究采用基质匹配标准溶液进行定量,结果表明,196种农药在0.005~0.2 mg/L范围内线性关系良好,相关系数均>0.996,方法的检出限为0.002 mg/kg,定量限为0.005 mg/kg。向猪肉、牛肉、猪肝3种不同脂肪含量基质的空白样品中添加标准溶液,196种农药在3个加标水平下(0.01、0.05、0.20 mg/kg)的平均回收率为65.3%~126.2%,精密度为0.7%~5.7%。本方法快速、准确、灵敏,适用于动物源性食品中多农药残留的高通量筛查与检测。
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