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 aims were to evaluate the nDATA (non-target data acquisition for target analysis) workflow using ultra high performance liquid chromatography/electrospray ionization quadrupole-Orbitrap mass spectrometry (UHPLC/ESI quadrupole-Orbitrap (Q-Orbitrap)) and semi-quantitate 1094 pesticides in fruits and vegetables.

Methods: Pesticide extracts from fresh produce were prepared using the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) procedure. nDATA was carried out by utilizing UHPLC/ESI Q-Orbitrap full MS scan and variable data independent acquisition (UHPLC/ESI Q-Orbitrap full MS/vDIA MSMS). 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 5 pairs of isobaric pesticides that were not separated by mass resolving power and/or chromatographic separation (retention time difference ΔtR <0.12 min) with the current instrument parameter settings.

Conclusion: The validated nDATA workflow using UHPLC/ESI Q-Orbitrap full MS/vDIA MSMS 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 of pesticides (over 1000). The target analysis using a CDB and a one-point standard calibration affords confidence in semi-quantitative screening results.