农业投入品中农药隐性成分的精准筛查方法

Accurate screening method of hidden pesticides ingredients in agricultural inputs

目的建立液相色谱-串联质谱法测定农业投入品中在90种农药中高频检出的隐性成分的精准筛查方法。方法样品采用乙腈超声提取、稀释并过膜净化后直接进样分析。采用气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)分析10种有机氯类和拟除虫菊酯类农药,采用液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)分析其他80种非法添加农药成分,采用外标法定量。结果 90种农药的检出限为0.001~0.01μg/mL;在线性范围内,目标物的浓度与峰面积呈良好的线性关系,相关系数大于0.99。利用本方法对天津市内抽检的45个农业投入品进行隐性成分筛查,共筛查出3个样品中含有未标注农药隐性成分。结论该方法检测的农药隐性成分种类多、范围广,具有良好的可靠性和灵敏度,适用于农业投入品中农药隐性成分的快速筛查与分析。

Objective To establish an accurate screening method for the recessive components by high frequency detection in agricultural inputs in 90 pesticide by liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile by ultrasonic, diluted and purified by membrane. Ten organochlorines and pyrethroids were analyzed by gas chromatography-mass spectrometry(GC-MS), and other 80 illegal pesticides were analyzed by liquid chromatography-tandem mass spectrometry(LC-MS/MS). And external standard method was adopted for quantitative analysis. Results The limits of detection of the 90 pesticides were 0.001-0.01 μg/mL. In the linear range, the concentration of the target substance had a good linear relationship with the peak area, and the correlation coefficient were greater than 0.99. This method was applied to screen the hidden pesticides ingredients of 45 agricultural inputs sampled in Tianjin, and a total of 5 samples were found containing unlabeled hidden ingredients. Conclusion This method has many kinds, wide range, good reliability and sensitivity, and is suitable for the rapid screening and analysis of pesticide recessive components in agricultural inputs.