快速溶剂萃取-凝胶渗透色谱净化-气相色谱-串联质谱分析猪肉中109种农药残留

Determination of 109 pesticide residues in pork using accelerated solvent extraction-gel permeation chromatography purification followed by gas chromatography-tandem mass spectrometry

目的建立一种同时分析猪肉中109种农药残留的气相色谱-串联质谱(GC-MS/MS)方法。方法样品经快速溶剂萃取仪提取,凝胶渗透色谱仪净化,加入内标环氧七氯,采用GC-MS/MS在多反应监测模式(MRM)下分析,内标法定量。结果 109种农药在10~500μg/L的浓度范围内线性关系良好,相关系数(r^2)大于0.99。各农药的检出限(S/N=3)为0.09~1.57μg/kg,各农药的定量限(S/N=10)为0.31~4.78μg/kg,在10.0、20.0和50.0μg/kg 3个水平的添加浓度下,回收率在68.3%~112.8%之间,相对标准偏差小于14.2%(n=6)。结论该方法准确可靠、灵敏度高,可用于猪肉中109种农药残留的同时检测。

Objective To establish a method for the simultaneous determination of 109 pesticides in pork by gas chromatography-tandem mass spectrometry（GC-MS/MS）. Methods The pork samples were extracted by accelerated solvent extraction and cleaned up by gel permeation chromatography. The treated samples with internal standard substance（heptachlor-epoxide） were then subjected to GC-MS/MS under multiple reaction monitor（MRM） acquisition mode. The quantification was performed by using internal standard calibration. Results The linear relation between peak area ratio and concentration ratio of 109 pesticides were good from 10 μg/L to 500 μg/L（r^2〉0.99）. The limits of detection（S/N=3） and quantitation（S/N=10） of 109 pesticides in the spiked blank pork sample were 0.09-1.57 μg/kg and 0.31-4.78 μg/kg, respectively. The recoveries at levels of 10.0, 20.0 and 50.0 μg/kg were ranged from 68.3% to 112.8%. The relative standard deviations（RSDs） were less than 14.2%（n=6）. Conclusion The established method is sensitive and repeatable, and reliable for the simultaneous determination of 109 pesticides in pork.