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目的采用双层填料固相萃取柱净化样品,建立气质联用同时测定农产品中49种农药残留的方法。方法干性样品经丙酮提取、新鲜样品经乙腈提取,Carb/NH2固相萃取柱净化,气相色谱质谱选择离子模式测定。结果 49种农药平均回收率为60.1%~117.9%,RSD范围为5%~19.7%,检出限为0.002μg/g~0.45μg/g,定量限为0.004μg/g~0.14μg/g。结论该方法选择性强,准确度好,精密度高,且样品前处理步骤简单,可应用于同时检测农产品中的49种农药残留。
OBJECTIVE To purify samples with double-packed solid-phase extraction column and establish a method for the simultaneous determination of 49 pesticide residues in agricultural products by GC-MS. Methods Dry samples were extracted with acetone, fresh samples were extracted with acetonitrile, cleaned up with Carb / NH2 solid phase extraction column and selected ion mode by gas chromatography-mass spectrometry. Results The average recoveries of 49 pesticides ranged from 60.1% to 117.9% with RSD ranging from 5% to 19.7%. The limits of detection were 0.002μg / g ~ 0.45μg / g with the limits of quantification of 0.004μg / g ~ 0.14μg / g. Conclusion The method is selective, accurate, accurate and simple in sample preparation. It can be applied to the simultaneous determination of 49 pesticide residues in agricultural products.