Application of nDATA Workflow for Semi-Quantitative Screening of 1094 Pesticide Residues in Fruits and Vegetables Using UHPLC/ESI Q-Orbitrap Full MS/vDIA.

Abstract

Background: Cost-effective multi-residue pesticide methods with a broad detection scope are desired for risk-based monitoring programs.

Objective: The aim was to evaluate the nDATA (non-target Data Acquisition for Target Analysis) workflow using UHPLC/ESI quadrupole-Orbitrap (Q-Orbitrap) mass spectrometry and semi-quantitate 1094 pesticides in fruits and vegetables.

Methods: Pesticide extracts from fresh produce were prepared using the QuEChERS procedure. nDATA was carried out by utilizing UHPLC/ESI Q-Orbitrap Full MS scan and variable data independent acquisition (vDIA). Data were processed using a Compound Database (CDB, 1094 pesticides) and one-point standard calibration with internal standards for semi-quantitation. Data processing criteria were based on retention time (± 0.5 min) and mass accuracy of a precursor ion (± 5 ppm) (RTP by full MS), or retention time (± 0.5 min) and mass accuracy of a precursor ion (± 5 ppm) and that of its fragment ion (± 10 ppm) (RTFI by full MS/vDIA).

Results: RTP found 1010 and 1094 pesticides, while RTFI identified 906 and 1029 pesticides at 10 and 100 μg/kg, respectively. RTF detected all 30 LC-amenable pesticides and RTFI identified 29 of 30 LC-amenable pesticides in eight proficiency testing samples. There were 42 pairs of co-eluting isomeric pesticides and five pairs of isobaric pesticides that were not separated by mass resolving power and/or chromatographic separation (ΔtR < 0.12 min) with the current instrument parameter settings.

Conclusions: The validated nDATA workflow using UHPLC/ESI Q-Orbitrap Full MS/vDIA proved to be a comprehensive detection method for semi-quantitative screening of 1094 pesticides in fruits and vegetables.

Highlights: nDATA combines both non-target data acquisition and target analysis. The non-target data acquisition generates data for retrospective analysis of a large number (over one thousand) of pesticides. The target analysis using a compound database (CDB) and a one-point standard calibration affords confidence in semi-quantitative screening results.