气相色谱-串联质谱法同时分析葡萄基质中 196种农药残留

Simultaneous analysis of 196 pesticide residues in grape matrix using gas chromatography-tandem mass spectrometry

中文关键词:  葡萄  农药残留  气相色谱-串联质谱法

英文关键词:196 pesticide residues  grape  GC-MS/MS

中文摘要:

      目的 建立同时分析葡萄基质中196种农药残留的气相色谱-串联质谱(GC-MS/MS)方法。方法 葡萄样品经乙腈提取, QuEChERS方法净化, 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, 38 min内即可完成196种农药的分离, 内标法定量。结果 196种农药在10~1000 μg/L的浓度范围内线性关系良好, 相关系数(r2)大于0.99, 各农药的检出限(S/N=3)为0.1~2.5 μg/kg, 各农药的定量限(S/N=10)为0.3~8.3 μg/kg, 在10.0 μg/kg和50.0 μg/kg 2个水平的添加浓度下, 回收率在60.5%~126.2%之间, 相对标准偏差0.2%~16.1%(n=6)。结论 该方法准确可靠, 灵敏度高, 可用于葡萄基质中196种农药残留的同时检测。

英文摘要:

      To analyze 196 pesticides in grape matrix using gas chromatography- tandem mass spectrometry (GC-MS/MS). Methods The grape samples were extracted by acetonitrile and purified by QuEChERS extraction package. The treated samples with internal standard substance (heptachlor-endo-epoxide) were then subjected to GC-MS/MS using multiple reaction monitor (MRM) acquisition mode. The 196 pesticide residues could be analyzed in 38 minutes and quantification was performed using internal standard calibration. Results The linear relation between peak area ratio and concentration ratio of 196 pesticides and internal standard substance were good from 10 ng/mL to 1000 ng/mL (r2>0.99). The limits of detection (S/N=3) and quantitation (S/N=10) of 196 pesticides in the spiked blank grape sample were 0.1~2.5 μg/kg and 0.3 ~8.3 μg/kg, respectively. The recoveries at levels of 10.0 μg/kg and 50.0 μg/kg were ranged from 60.5% to 126.2%. The relative standard deviations (%RSD, n=6) were 0.2%~16.1%. Conclusion The established method is sensitive and repeatable, and reliable for simultaneous analysis of 196 pesticides in grape matrix.