增强型脂质去除分散固相萃取净化-气相色谱-串联质谱法测定动物性食品中146种农药残留

Determination of 146 kinds of pesticide residues in animal derived food by enhanced matrix removal-lipid dispersion solid phase extraction purification coupled with gas chromatography-tandem mass spectrometry

中文关键词:  动物性食品  脂质去除分散固相萃取  气相色谱-串联质谱法  农药残留

英文关键词:animal derived foods  enhanced matrix removal-lipid dispersion solid phase extraction  gas chromatography-tandem mass spectrometry  pesticide residues

中文摘要:

      目的 建立一种基于增强型脂质去除分散固相萃取(enhanced matrix removal-lipid dispersion solid phase extraction, dSPE EMR-Lipid)净化技术结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)测定动物性食品中146种农药残留量的分析方法。方法 在5 g样品中加入2 mL超纯水, 经乙腈提取, 冷冻10 min, QuEChERS-EN-盐包除水分离, 采用dSPE EMR-Lipid净化技术, GC-MS/MS动态多反应监测(dynamic multi-reaction monitoring, DMRM)模式监测, 基质匹配标准曲线法定量分析。结果 146种化合物在5~320 μg/L范围内线性关系良好, 相关系数均大于0.9939, 方法的检出限为0.04~10.91 μg/kg, 定量限为0.11~32.72 μg/kg。146种化合物在0.01、0.02和0.10 mg/kg 3个不同加标水平下的平均回收率范围在61.3%~119.3%之间, 相对标准偏差为0.15%~16.02%。结论 该方法操作简便快速, 灵敏准确, 能够满足多种农药残留量的同时检测需求, 适用于动物性食品中多种农药残留的定量筛查。

英文摘要:

      Objective To establish an analytical method for the determination of 146 kinds of pesticide residues in animal derived foods by enhanced matrix removal-lipid dispersion solid phase extraction (dSPE EMR-Lipid) and purification technology coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The 5 g sample were added to 2 mL ultrapure water, extracted with acetonitrile, freezed for 10 min, separated with QuEChERS EN-extraction package, cleaned-up with dSPE EMR-Lipid, then was detected by GC-MS/MS in dynamic multi-reaction monitoring (DMRM) mode. The analytes were quantified by matrix-matched standard curve method. Results The results showed that 146 kinds of pesticides had good linearities in the concentration of 5–320 μg/L, the linear correlation coefficient of the compounds were greater than 0.9939, and the limits of detection of the method were 0.04–10.91 μg/kg, the limits of quantification were 0.11–32.72 μg/kg. The average recoveries of 146 kinds of pesticides at the spiked level of 0.01, 0.02 and 0.10 mg/kg ranged from 61.3% to 119.3%, relative standard deviations were 0.15%–16.02%. Conclusion The method is simple in pre-treatment, convenient in operation, rapid, sensitive and accurate in detection, can meet the simultaneous detection requirements for multiple pesticide residues. It is suitable for preliminary screening and quantitative detection of multiple pesticide residues in animal derived food.