菠菜中13种有机磷农药残留快速检测方法研究

Rapid Analysis of 13 Organophosphorus Residues of Pesticides in Spinach by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

本实验采用高效液相色谱-串联质谱法(HPLC-MS-MS),建立了华东地区叶菜中常用有机磷类农药多残留的快速定量检测方法。实验对各个农药化合物的特征离子对、碰撞电压等参数进行了优化,同时分析了各农药的线性范围和定量限。结果表明13种有机磷类农药在20min内得到良好分离,在0.025～1.0mg/L范围内线性良好,相关系数为0.9986～0.9998;在0.01～0.1mg/kg浓度范围内,平均加标回收率在82.1%～96.3%之间;相对标准偏差为0.5%～8.9%;定量限均小于9.0μg/kg,均显著低于日本肯定列表制度的限量。该方法简便、快速、灵敏度高。

A multiresidue method is described for the determination of 13 pesticides commonly used in leafy-vegetables which customarily used in eastern of China. 5 g of samples are extracted with ethyl acetate, then analyzed by LC-ESI（＋）-MS-MS, without further clean-up steps. The obtained correlation coefficient was ranged from 0.9986 to 0.9998. The average recoveries for the pesticides ranged from 82.1% to 96.3 %, with the relative standard deviations （RSDs） were less than 8.9% for all compounds. The calculated LOQs （ ~ g/kg） were 9.0 μg/kg, lower than the maximum residue limits （MRLs） listed in the positive list. The proposed method is easy, fast and sensitive.