Preliminary Study to Develop an Alternative Method for the Non-targeted Determination of Xenobiotics in Food by Means of Ultra High Performance Liquid Chromatography Coupled to High Resolution and Accuracy Mass Spectrometry

Abstract

This preliminary study describes the use of high resolution and accuracy mass spectrometry techniques combined with new generation chemical software products for detecting and identifying contaminants in food commodities. As a first step, the extracts of routine target analysis samples (obtained in our official laboratory responsible for food residues control) were acquired and processed with this method in order to search unknown and non-targeted contaminants in food. In order to verify the feasibility of the presented method, the research has been firstly addressed to untargeted pesticides and their metabolites in stone fruits commodities and tomatoes. The differential analysis carried with Compound Discoverer 2.0 between the investigated unknown sample and the blank matrix sample allowed to remove all the matrix molecular components; Aggregated Computational Toxicology Resource (ACToR) helped to understand and predict chemical interpretation of substances. The acquisition in FullScan-AIF and FullScan-ddMS2 allowed the clear detection and identification of isobaric compounds such as quinalphos and phoxim. In order to verify that the proposed method is suitable to the scope of application, the main points of SANTE/11813/2017 Document have been followed. The results demonstrate that no false positives and no false negatives have been detected from the analysis of samples spiked with 55 pesticides at 0.010 and 0.10 mg kg−1. This preliminary study has been also tested with a Proficiency Test (EUPT-FV-SM08) and, according to EUPT-FV-SM08 Final Report, our laboratory has been included in the 67% (56) that clearly detected over 70% pesticides. Finally, this method has been extended to other matrices and contaminants.

A Quantitative and Confirmatory Method Employing Liquid Chromatography Coupled to Hybrid High-Resolution Mass Spectrometry and QuEChERS for the Determination of Thirty-Seven Growth Promoter Residues in Bovine Urine

“…In this way, the FS-AIF and FS-DIA modes showed not to be appropriate for quantitative analysis. It should be taken into account that these modes might still be applied to screening and untargeted purposes. − A lower resolution power (17,500 FWHM) was selected in the PRM mode in order to increase the number of detected signals for each product ion. However, it should be taken into account that all of the detected ions (precursors and products) have been identified using a mass extraction window of 5 ppm.…”

Nicotinamide Effectively Suppresses Fusarium Head Blight in Wheat Plants

“…Compound discoverer v.3.1 (CD 3.1, Thermo Scientific, San Jose, CA, USA) was used for mass spectrometry data acquisition [53]. The settings were as follows: 5 ppm mass tolerance, 30 signal of intensity tolerance, and 1,000,000 of minimum peak intensity [54]. The annotations of metabolites were generated using ChemSpider (http://www.chemspider.com/) (accessed date: 29 January 2021) database, which consisted of integrating data from the Aracyc, Biocyc, KEGG pathways, mzVault, and mzCloud databases.…”

Alternative method’s results for the non targeted determination of xenobiotics in food by means of high resolution and accuracy mass spectrometry

“…Two hundred grams portions of homogenate samples were weighed out into screw-capped polyethylene plastic bottles, sealed and stored at − 20 °C prior the distribution to the participants. The extraction was carried out as reported by Scarpone et al (2020) with the use of QuEChERS (EN 15662:2008(EN 15662: 2008 without clean-up. The sample extracts were diluted 1:10 in water and injected in LC-MS for the analysis.…”

“…Also in this case, the extraction was carried out as reported by Scarpone et al (2020) with the use of QuEChers (EN 15662:2008(EN 15662: 2008 without clean-up. The sample extracts were diluted 1:10 in water for the LC-MS analysis.…”

“…After these trials, a differential analysis between the blank matrix and the samples was carried out. The blank matrix was not the same of the samples, but as reported in a previous study (Scarpone et al 2020), it is not significant to use the same blank matrix.…”