建立了以QuEChERS dSPE EMR-Lipid作前处理测定动物源性食品中205种农药及13种代谢物残留量的气相色谱-串联质谱联用方法(GC-MS/MS).分析过程中考察了不同提取溶剂、不同净化方式对目标物回收率的影响,最终确定了样品采用乙腈提取,经Agilent Bond Elut EMR-Lipid增强型脂质去除净化管和Agilent Bond Elut EMR-Lipid Polish反萃管结合净化,多反应监测模式,内标法定量,GC-MS/MS测定分析.结果表明,205种农药及13种代谢物在0.01～0.5 μg/mL质量浓度范围内线性关系良好,线性相关系数(r2)均大于0.995,定量限为0.01 mg/kg;猪肉、猪肝、鸡肉、鸡蛋4种样品基质在0.01、0.02和0.05 mg/kg加标浓度下的平均回收率为60.3％～120.5％,相对标准偏差(n=6)在0.2％～20.4％之间.该方法前处理简单、准确灵敏、回收率好,适合动物源性食品中多农残目标物的同时分析.
Determination of 205 Pesticides and 13 Metabolites Residues in Animal Derived Foods by QuEChERS dSPE EMR-Lipid-GC-MS-MS
A gas chromatography-mass spectrometry(GC-MS-MS)method was developed for the determination of 205 pesticides and 13 metabolites residues in animal derived-food using QuEChERS dSPE EMR-Lipid as pretreatment.During the analysis process,the effects of different extraction solvents and purification methods on the recovery rate of the target substance were investigated.Finally,the sample was extracted with acetonitrile and purified through Agilent Bond Elut EMR-Lipid enhanced lipid removal purification tube and Agilent Bond Elut EMR-Lipid Polish reverse extraction tube.Multiple reaction monitoring modes,internal standard method quantification,and GC-MS-MS quantitative analysis were used.The results showed that there was a good relationship for 205 pesticides and 13 metabolites within the mass concentration range of 0.01-0.5 μg/mL,with linear correlation coefficients(r2)greater than 0.995 and a quantitative limit of 0.01 mg/kg.The average recovery rates of the four sample matrices of pork,pig liver,chicken and egg at 0.01,0.02,and 0.05 mg/kg spiked concentrations were 60.3％-120.5％,with a relative standard deviation(n=6)between 0.2 and 20.4％.This method has simple pretreatment,accuracy,sensitivity and good recovery rate,making it suitable for the simultaneous analysis of multiple agricultural residues in animal derived foods.
QuEChERSdSPE EMR-LipidGas chromatography-tandem mass spectrometryAnimal-derived foodsMulti agricultural residue analysis
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