Application of ultrahigh-performance liquid chromatography and electrospray ionization quadrupole orbitrap high-resolution mass spectrometry for determination of 166 pesticides in fruits and vegetables.

This paper presents an application of ultrahigh-performance liquid chromatography and electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap) for determination of 166 pesticide residues in fruits and vegetables. Pesticides were extracted from the samples using the QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure. UHPLC/ESI Q-Orbitrap MS (i.e., full MS scan) acquired full MS data for quantification, and UHPLC/ESI Q-Orbitrap dd-MS(2) (i.e., data-dependent scan) obtained product-ion spectra for confirmation. UHPLC/ESI Q-Orbitrap MS quantification was achieved using matrix-matched standard calibration curves with isotopically labeled standards or chemical analogues as internal standards. The method performance characteristics that included overall recovery, intermediate precision, and measurement uncertainty were evaluated according to a nested experimental design. For the matrices studied, about 90.3-91.5% of the pesticides had recoveries between 81 and 110%, 92.1-97.6% had intermediate precision ≤20%, and 89.7-95.2% had measurement uncertainty ≤40%. Confirmation was based on mass accuracy ≤5 ppm and LC retention time tolerance within ±2.5%. Overall, the UHPLC/ESI Q-Orbitrap has demonstrated great performance for quantification and confirmation of pesticide residues in fresh fruits and vegetables.