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目的建立一种同位素内标-液相色谱-串联质谱测定水果中11种农药的方法。方法样品用乙腈提取,离心后取上清液旋转蒸发浓缩,经过氨基固相萃取小柱净化后,旋转蒸发至干,流动相溶解样品,用Waters XSelect~HSS T3色谱柱(2.1 mm×50 mm,2.5μm)进行分离,以乙腈和0.2%甲酸溶液作为流动相进行洗脱,内标法测定。结果本研究建立的方法相对标准偏差(RSD)在4.7%~9.4%之间,样品加标回收率在78.6%~107.4%之间,定量限和检出限分别在0.002~2.2和0.000 4~0.66μg/kg。结论本研究建立的分析方法操作简便、结果准确、灵敏度高,可满足实验室对食品中农药残留的检测要求。
Objective To establish a method for the determination of eleven pesticides in fruits by internal standard-liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile, centrifuged and the supernatant was concentrated by rotary evaporation. After purification by Amino-solid phase extraction cartridge, the sample was rotary evaporated to dryness. The mobile phase was dissolved and the sample was separated on a Waters XSelect ~ HSS T3 column (2.1 mm × 50 mm, 2.5 [mu] m), eluting with acetonitrile and 0.2% formic acid as the mobile phase, and determined by internal standard method. Results The relative standard deviations (RSDs) of the method established in this study ranged from 4.7% to 9.4%. The recoveries of spiked samples ranged from 78.6% to 107.4%. The limits of quantitation and detection were 0.002 ~ 2.2 and 0.000 4 ~ 0.66 μg / kg. Conclusion The analytical method established in this study is simple, accurate, sensitive and can meet the laboratory requirements of pesticide residue detection in food.