改良 QuEChERS-超高效液相色谱-串联质谱法测定水果蔬菜中 36 种农药残留.

[Objective] To establish a method for simultaneous determination of 36 pesticide residues in fruits and vegetables by QuEChERS purification-ultra high performance liquid chromatography-triple quadrupole tandem mass spectrometry. [Method] The sample preparation was treated using the modified QuEChERS method with acetonitrile as the extraction solvent, and after salting out stratification, take 2. 0 mL supernatant, purified with 400 mg anhydrous magnesium sulfate (MgSO4 ), 50 mg ethylenediamine-N-propylsilane (PSA), 50 mg octadecylsilane bonded silica gel (C18 ) and 100 mg of graphitized carbon black (GCB),analyze and detect under multiple reaction monitoring mode (MRM) using Waters Atlantis T3 C18 column (2. 1 mm × 150 mm, 5 μm) as an analytical column, gradient elution and quantification using external standard method. [Result] 36 pesticides had a good linear relationship (r≥0. 991 0) at a mass concentration of 5. 00-200. 38 ng / mL, with the detection limit of 0. 002-0. 003 mg / kg and the quantification limit of 0. 005-0. 010 mg / kg. 36 pesticide standards with concentrations of 2 times, 5 times and 10 times the quantification limit were added to the composite fruit and vegetable juice samples, the average recovery rate was 81. 70%-117. 38%, and the instrument precision RSD was 1. 10%-4. 19%. [Conclusion]The established method has the advantages of simple pretreatment, high sensitivity, good accuracy and strong repeatability, and can be widely used in the analysis and detection of a variety of pesticide residues in fruits and vegetables. [ABSTRACT FROM AUTHOR]