Quantitative Screening of Agrochemical Residues in Fruits and Vegetables by Buffered Ethyl Acetate Extraction and LC-MS/MS Analysis

J Agric Food Chem. 2015 May 13;63(18):4449-56. doi: 10.1021/jf505221e. Epub 2015 Feb 10.

Abstract

A buffered ethyl acetate extraction method is proposed for the simultaneous analysis of 296 agrochemicals in a wide range of fruit and vegetable matrices by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The optimized quantity of acetate buffer (1% acetic acid + 0.5 g of sodium acetate per 10 g of sample) adjusted the pH of each test matrix to 5-6, which in turn significantly improved recoveries of acidic and basic compounds. The role of diethylene glycol (used in the evaporation step) on signal suppression of certain compounds was evaluated, and its quantity was optimized to minimize such an effect. The method was validated in grape, mango, drumstick, bitter gourd, capsicum, curry leaf, and okra as per the DG-SANCO/12571/2013 guidelines. Recoveries in the fortification range of 1-40 μg/kg were within 70-120% with associated relative standard deviations below 20% for most of the compounds. The method has potential for regulatory and commercial applications with a generic approach.

Keywords: LC-MS/MS; agrochemical residues; buffered extraction; fruits and vegetables; matrix effect; multiresidue analysis; single-laboratory validation.

Publication types

  • Evaluation Study
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Agrochemicals / chemistry*
  • Agrochemicals / isolation & purification*
  • Chemical Fractionation / methods*
  • Chromatography, High Pressure Liquid / methods*
  • Food Contamination / analysis
  • Fruit / chemistry*
  • Tandem Mass Spectrometry / methods*
  • Vegetables / chemistry*

Substances

  • Agrochemicals