Ultrahigh-Performance Liquid Chromatography Electrospray Ionization Q‑Orbitrap Mass Spectrometry for the Analysis of 451 Pesticide Residues in Fruits and Vegetables: Method Development and Validation

• Published in: Journal of agricultural and food chemistry Vol. 62; no. 42; pp. 10375 - 10391
• Main Authors: Wang, Jian, Chow, Willis, Chang, James, Wong, Jon W
• Format: Journal Article
• Language: English
• Published: United States American Chemical Society 22.10.2014; American Chemical Society, Books and Journals Division
• Subjects: Chromatography, High Pressure Liquid - methods; experimental design; Food Contamination - analysis; Fruit - chemistry; fruits; ionization; isotope labeling; mass spectrometry; Mass Spectrometry - methods; pesticide residues; Pesticide Residues - chemistry; pesticides; ultra-performance liquid chromatography; uncertainty; vegetables; Vegetables - chemistry; UHPLC/ESI Q-Orbitrap; quantification; identification; pesticides; high-resolution mass spectrometer; fruits and vegetables; measurement uncertainty
• ISSN: 0021-8561; 1520-5118
• DOI: 10.1021/jf503778c

This paper presents an application of ultrahigh-performance liquid chromatography electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap MS) for the determination of 451 pesticide residues in fruits and vegetables. Pesticides were extracted from samples using the QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure. UHPLC/ESI Q-Orbitrap MS in full MS scan mode acquired full MS data for quantification, and UHPLC/ESI Q-Orbitrap Full MS/dd-MS2 (i.e., data-dependent scan mode) obtained product ion spectra for identification. UHPLC/ESI Q-Orbitrap MS quantification was achieved using matrix-matched standard calibration curves along with the use of isotopically labeled standards or a chemical analogue as internal standards to achieve optimal method accuracy. The method performance characteristics include overall recovery, intermediate precision, and measurement uncertainty evaluated according to a nested experimental design. For the 10 matrices studied, 94.5% of the pesticides in fruits and 90.7% in vegetables had recoveries between 81 and 110%; 99.3% of the pesticides in fruits and 99.1% of the pesticides in vegetables had an intermediate precision of ≤20%; and 97.8% of the pesticides in fruits and 96.4% of the pesticides in vegetables showed measurement uncertainty of ≤50%. Overall, the UHPLC/ESI Q-Orbitrap MS demonstrated acceptable performance for the quantification of pesticide residues in fruits and vegetables. The UHPLC/ESI Q-Orbitrap Full MS/dd-MS2 along with library matching showed great potential for identification and is being investigated further for routine practice.