山楂叶中127种农药多残留检测分析

Determination and analysis of 127 pesticide residues in hawthorn leaves

目的:建立山楂叶中禁用及常用农药多残留检测方法。方法:以乙腈为溶剂,高速匀浆提取,经氨基石墨化碳小柱净化。方法:气相色谱-串联质谱法和液相色谱-串联质谱法检测。结果:6批山楂叶中农药检出数量达19种,无禁用农药检出。山楂叶提取净化后各待测指标成分线性关系良好,95%以上指标相关系数大于0.995,各待测指标化合物回收率平均值在69.9%~118.2%,符合农药多残留的痕量分析检测要求。结论:该方法有针对性地对山楂叶中127种农药残留进行准确检测,可为基质类似中药材的农药残留检测方法提供借鉴参考。

Objective: To establish a method for the determination of forbidden and commonly used pesticide residues in hawthorn leaf. Methods: The samples were extracted with acetonitrile by high speed homogenater, and purified by solid-phase extraction(SPE) column of envi-carb/NH. Detection was performed by GC-MS/MS analysis and LC-MS/MS analysis. Results: 19 kinds of pesticide were detected in 6 batches of hawthorn leaves, and no forbidden pesticide was detected.After the extraction and purification, the calibration curves of all targets showed good linearity with correlation coefficients of 95% analytes above 0.995, and the average recovery rates were 69.9%-118.2%, which met with the requirements of multi-pesticide trace analysis. Conclusion: This method can be used for accurate detection of 127 kinds of pesticide residues in hawthorn leaves, which provides reference for the detection of pesticide residues in Chinese medicinal materials with similar substrates.