Determination of Selected Priority Pesticides in High Water Fruits and Vegetables by Modified QuEChERS and GC-ECD with GC-MS/MS Confirmation

Abstract

A modified quick, easy, cheap, efficient, rugged and safe (QuEChERS) method coupled to gas chromatography with electron capture detector (GC-ECD) was developed for simultaneous determination of selected electronegative pesticides in fruits and vegetables with high water content. The chosen compounds are commonly detected in fruit and vegetable crops, and some of their metabolites have even been found in human urine. In addition, some of them are known or suspected carcinogens according to the International Agency for Research of Cancer. Extraction and clean up parameters were optimized, thus the original QuEChERS method was modified to decrease solvent usage, in accordance with ‘green chemistry’ principles. The proposed methodology was validated in terms of selectivity, specificity, linearity, precision and accuracy. The obtained limits of detection (LODs) for all investigated pesticides ranged from 5.6 µg·kg−1 to 15 µg·kg−1 and limits of quantification (LOQs) from 17 µg·kg−1 to 45 µg·kg−1. The obtained data demonstrated the good reproducibility and stability of the procedure in the tested concentration range up to 10 mg·kg−1, with relative standard deviations (RSDs) lower than 10%. Recoveries for spiked pear samples at LOQ level for each pesticide were from 90% to 107% with RSDs lower than 9.6%. The suitability of the developed procedure was tested on various fruit and vegetable samples available on the market at different seasons. The proposed methodology is applicable for detection and monitoring of selected pesticides not only in fruits and vegetables with high water content, but also in samples containing large amounts of pigments and dyes.