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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 gas chromatography-tandem mass spectrometry (GC-MS / MS) method for simultaneous analysis of 109 pesticide residues in pork. Methods The samples were extracted by fast solvent extraction and purified by gel permeation chromatography (GC-MS). The internal standard epoxy heptachlor was added and analyzed by multi-reaction monitoring mode (MRM) with GC-MS / MS. Results The results showed that 109 pesticides had a good linearity in the concentration range of 10 ~ 500μg / L with the correlation coefficient (r ~ 2) greater than 0.99. The limit of detection (S / N = 3) for each pesticide was 0.09-1.57 μg / kg and the limit of quantification (S / N = 10) for each pesticide ranged from 0.31 to 4.78 μg / The recoveries ranged from 68.3% to 112.8% with the relative standard deviations (RSDs) less than 14.2% at 3 levels (n = 6). Conclusion The method is accurate and reliable with high sensitivity and can be used for simultaneous detection of 109 pesticide residues in pork.