超声波萃取-高效液相色谱-串联质谱快速检测叶菜中残留农药

Rapid and simultaneous analysis of pesticide residues in leafy-vegetables by solvent ultrasonic extraction-liquid chromatography-electrospray tandem mass spectrometry

使用超声强化萃取-液相色谱-串联质谱（LC-MS-MS）方法对叶菜中常用28种农药建立了快速检测方法。5g样品在40mL混合液（V乙酸乙酯：V石油醚=2：1）中超声强化萃取35min，0．22um膜过滤后直接进行LC-MS-MS检测。在0．1×10^-3～0．2mg／kg范围内线性良好，线性相关系数r〉0．9970，精密度为92．8％～100．3％，加标水平在3．5×10^-3～2．0×10^-2mg／kg时，回收率为83．6％～98．7％，RSD〈4．4％，加标水平在7．6×10^-3～4．0×10^-2mg／kg时，回收率为83．8％～99．6％，RSD〈54．7％；定量限为0．1～5．0ug／kg。本方法快速、简便、灵敏度高，可用于华东地区叶菜中多类多残留的快速检测。

A rapid and simultaneous analysis method is described for the determination of 28 pesticide residues in leafy-vegetables. Samples of 5 g are extracted for 35 min in 40 mL solution with the volume ratio of ethyl acetate to petroleum ether being 2：1 in an ultrasonic bath,filtered with the 0. 22um film,and then analyzed by LC-ESI-MS-MS without further clean-up steps. The obtained correlation coefficient was larger than 0. 997 0 at the test range from 0. 1 × 10^-3 mg/kg to 0. 2 mg/kg, and the precision ranged from 92. 8% to 100. 3%. The average recovery rates of the pesticides ranged from 83.6% to 98. 7% at fortification levels between 3. 5×10^-3 mg/kg and 2. 0×10^-2 mg/kg and 83. 8% to 99. 6% at fortification levels between 7. 6×10^-3 mg/kg and 4. 0×10^-2 mg/kg, with the relative standard deviations （RSDs） being less than 4. 4% and 4. 7%, respectively. The calculated LOQs were 0. 1-5.0 ug/kg. The proposed method is fast and sensitive and can be used for monitoring pesticide residues in normal leafy-vegetables.