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Screening of Over 600 Pesticides, Veterinary Drugs, Food-Packaging Contaminants, Mycotoxins, and Other Chemicals in Food by Ultra-High Performance Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry (UHPLC-QTOFMS)

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Abstract

In this article, an accurate mass multiresidue screening method has been developed for the determination of over 630 multiclass food contaminants in different matrices using ultra-high performance liquid chromatography/(quadrupole)-time-of-flight mass spectrometry. The compounds included in the study were 426 pesticides, 117 veterinary drugs, 42 food-packaging contaminants, 21 mycotoxins, 10 perfluorinated compounds, 9 nitrosamines, and 5 sweeteners. The separation was carried out by liquid chromatography using a C18 column (50 mm × 2.1 mm, 1.8 μm particle size). The identification of the targeted species was accomplished using accurate masses of the targeted ions (protonated or deprotonated molecule) along with retention time data and characteristic fragment ion for reliable identification, using specific software for automated data mining and exploitation. The performance of the screening method was validated in terms of linearity, matrix effect, and limits of quantification for three representative food matrices (tomato, orange, and baby food) using a generic sample treatment based on liquid partitioning with acetonitrile (QuEChERS). The overall method performance was satisfactory with limits of quantification lower than 10 μg kg −1 for the 44 % of studied compounds. In some cases (ca. 10–15 % of the pesticides depending on the matrix tested, maximum residue levels were not fulfilled). In orange, 15 % of the compounds displayed LOQs above the maximum residue levels (MRLs) set for the studied pesticides, which can be partially attributed to matrix effects. Moderate signal suppression was observed in the three matrices tested in most cases, being orange the matrix which produced the highest matrix effect and baby food the lowest one.

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Abbreviations

CCL-3:

Contaminant candidate lists

CID:

Collision-induced dissociation

GC-MS/MS:

Gas chromatography/tandem mass spectrometry

HRMS:

High-resolution mass spectrometry

LC-MS/MS:

Liquid chromatography/tandem mass spectrometry

MeOH:

Methanol

QC:

Quality control

QuEChERS:

Quick, easy, cheap, effective, rugged, and safe

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Acknowledgments

The authors acknowledge funding from the Spanish Ministerio de Economía y Competitividad (MINECO) (Ref. CTQ-2009-10897). P.P.-O acknowledges a PhD scholarship from the University of Jaén. F.J.L.-O. acknowledges a FPI Program PhD scholarship from MINECO (Ref. BES-2013-064014). D.M.G. thanks the MINECO for a Juan de la Cierva postdoctoral contract. B.G.L. acknowledges MINECO for her Juan de la Cierva postdoctoral research contract (Ref. JCI-2012-12972). The authors acknowledge Servicios Centrales de Apoyo a la Investigación of the University of Jaen (SCAI-UJAEN).

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Authors and Affiliations

  1. Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Campus Las Lagunillas, Edif. B-3, 23071, Jaén, Spain

    Patricia Pérez-Ortega, Felipe J. Lara-Ortega, David Moreno-González, Juan F. García-Reyes & Antonio Molina-Díaz

  2. Foodomics Laboratory, Bioactivity and Food Analysis Department, Institute of Food Science Research - CIAL (UAM+CSIC), Campus de Cantoblanco, Calle Nicolás Cabrera 9, 28049, Madrid, Spain

    Bienvenida Gilbert-López

  3. Center for Advanced Studies in Olives Grove and Olive Oils (CEAOAO), Science and Technology Park GEOLIT, 23620, Mengíbar, Spain

    Antonio Molina-Díaz

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  1. Patricia Pérez-Ortega
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  2. Felipe J. Lara-Ortega
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  3. Bienvenida Gilbert-López
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  5. Juan F. García-Reyes
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Correspondence to Antonio Molina-Díaz.

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Conflict of Interest

Patricia Pérez-Ortega declares that she has no conflict of interest. Felipe J. Lara-Ortega declares that he has no conflict of interest. Bienvenida Gilbert-López declares that he has no conflict of interest. David Moreno-González declares that he has no conflict of interest. Juan F. García-Reyes declares that he has no conflict of interest. Antonio Molina-Díaz declares that he has no conflict of interest.

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Pérez-Ortega, P., Lara-Ortega, F.J., Gilbert-López, B. et al. Screening of Over 600 Pesticides, Veterinary Drugs, Food-Packaging Contaminants, Mycotoxins, and Other Chemicals in Food by Ultra-High Performance Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry (UHPLC-QTOFMS). Food Anal. Methods 10, 1216–1244 (2017). https://doi.org/10.1007/s12161-016-0678-0

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