Screening of 439 Pesticide Residues in Fruits and Vegetables by Gas Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry Based on TOF Accurate Mass Database and Q-TOF Spectrum Library

Abstract

Because of its unique characteristics of accurate mass full-spectrum acquisition, high resolution, and fast acquisition rates, GC-quadrupole-time-of-flight MS (GC-Q-TOF/MS) has become a powerful tool for pesticide residue analysis. In this study, a TOF accurate mass database and Q-TOF spectrum library of 439 pesticides were established, and the parameters of the TOF database were optimized. Through solid-phase extraction (SPE), whereby pesticides are extracted from fruit and vegetable substrates by using 40 mL 1% acetic acid in acetonitrile (v/v), purified by the Carbon/NH2 SPE cartridge, and finally detected by GC-Q-TOF/MS, the rapid analysis of 439 pesticides in fruits and vegetables can be achieved. The methodology verification results show that more than 70 and 91% of pesticides, spiked in fruits and vegetables with concentrations of 10 and 100 μg/kg, respectively, saw recoveries that conform to the European Commission's criterion of between 70 and 120% with RSD ≤20%. Eighty-one percent of pesticides have screening detection limits lower than 10 μg/kg, which makes this a reliable analysis technology for the monitoring of pesticide residues in fruits and vegetables. This technology was further validated for its characteristics of high precision, high speed, and high throughput through successful detection of 9817 samples during 2013-2015.

Current Role of Mass Spectrometry in the Determination of Pesticide Residues in Food

“…In this sense, large-scale multiresidue methods refer to those capable of covering at least 80 analytes [27]. Multiresidue methods for less-polar pesticides can cover the determination of hundreds to thousands of pesticides and metabolites, using either GC-MS methods [28][29][30] or LC-MS methods [31,32].…”

Eliminación de pesticidas organofosforados mediante fotoelectrocatálisis con fotoánodos de WO3

“…En la Figura 4.96 se muestra el cromatograma EIC del fenamifos. El pico asociado a este tiene un valor de m/z de 304.01 y aparece a un tiempo de retención de 12.5 min [140]. En la Figura 4.97 se representa el área obtenida en función de cada concentración de pesticida, así como la recta de calibrado asociada a este pesticida.…”

Screening for More than 1,000 Pesticides and Environmental Contaminants in Cannabis by GC/Q-TOF

“…The procedure is qualitative in nature, but quantification is possible when standards are available. The GC/Q-TOF together with a pesticide PCDL have been used for the detection of pesticides in aquatic environments [15] and in various foods [16, 17], but it has never been used to analyze pesticide residues in cannabis. While this paper describes the analysis of GC-amenable pesticide residues on cannabis, there is a need for a similar broad screening method using high-resolution accurate mass LC/MS because most (but not all) pesticides are LC-amenable.…”