同时测定蔬菜中的49种农药残留量的气相色谱/三重四极杆质谱法

Simultaneous determination of 49 kinds of pesticide residues in vegetables by gas chromatography-triple quadrupole tandem mass spectrometry

目的建立一种同时测定蔬菜中49种农药残留量的固相萃取气相色谱一三重四极杆质谱（GC—MS／MS）的方法。方法样品经乙腈提取，43℃水浴中旋转蒸发近干，固相萃取小柱净化，样品液氮吹浓缩后，用气相色谱GC—MS／MS法测定，外标法定量。结果49种农药在36min内完全分离，在0．01—10μg／ml范围内相关系数，。均在0．99以上，加标回收率在71．60％-109．3％之间，相对标准偏差均小于12％，定性检出限为0．001～0．006μg／ml。结论该方法操作简单，准确度和精密度高，适用于各种蔬菜中农药多残留量的检测和确证。

[ Objective] To establish a method for simultaneous determination of 49 kinds of pesticide residues in vegetables by solid phase extraction-gas chromatography-triple quadrupole tandem mass spectrometry （GC/MS/MS）. [ Methods] The samples were ex- tracted with acetonitrile. The extract was warmed with water at 43 ℃, and treated through circumrotate evaporation until it was nearly dry. Then it was cleaned up by solid phase extraction column, and concentrated by nitrogen. The extract was determined by GC/MS/MS, and the external standard method was applied in the quantitative analysis. [ Results]49 kinds of pesticides were sepa- rated completely within 36 minutes. The calibration curves were linear （correlation coefficient r2 〉 0.99） within the range of 0.01-10.0 ug/ml. The recoveries of standard addition were between 71.60% and 109.3%. The relative standard deviations （RSD） of the method were lower than 12%, and the limit of determination （ LOD ） was 0. 001 - 0.006 μg/ml. [ Conclusion ] The method is simple, accurate and sensitive. It is suitable for the detection and confirmation of various pesticides residues in vegetables.