Determination of Multiclass Pharmaceutical Residues in Milk Using Modified QuEChERS and Liquid-Chromatography-Hybrid Linear Ion Trap/Orbitrap Mass Spectrometry: Comparison of Clean-Up Approaches and Validation Studies

Author:

Koloka Ourania1,Koulama Marioanna1,Hela Dimitra12,Albanis Triantafyllos12,Konstantinou Ioannis12

Affiliation:

1. Department of Chemistry, University of Ioannina, 45110 Ioannina, Greece

2. University Research and Innovation Center, Institute of Environment and Sustainable Development, University of Ioannina, 45110 Ioannina, Greece

Abstract

A multi-residue method was developed to identify and quantify pharmaceutical drug residues in full-fat milk, using a modified QuEChERS extraction procedure and sonication combined with Ultra-High-Performance Liquid Chromatography–High-Resolution Orbitrap Mass Spectrometry (UHPLC-HR-Orbitrap-MS). Sample preparation involves three different QuEChERS extraction procedures and sorbents for the purification step. The optimized modified extraction method, combined with the clean-up approaches using C18 and the EMR-Lipid sorbent, has been validated in terms of linearity, recovery, precision, LOD and LOQ, matrix effects (ME) and expanded uncertainty. The optimized method showed a linearity >0.9903, recoveries within the range 65.1–120.1%, precision (expressed as %RSD) <17.5%, medium (<39.9%) to low (<16.7%) matrix effects and acceptable expanded uncertainty (<33.1%). Finally, the proposed method was applied to representative real samples of milk (by local markets), revealing the existence of one pharmaceutical drug (imidocarb) in one sample.

Funder

Development of research infrastructure for the design, production, development of quality characteristics and safety of agrofoods and functional foods

operational program “Competitiveness, Entrepreneurship and Innovation”

Greece and the European Union

Publisher

MDPI AG

Subject

Chemistry (miscellaneous),Analytical Chemistry,Organic Chemistry,Physical and Theoretical Chemistry,Molecular Medicine,Drug Discovery,Pharmaceutical Science

Reference58 articles.

1. He, Z., and Zhang, H. (2014). Applied Manure and Nutrient Chemistry for Sustainable Agriculture and Environment, Springer.

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3. European Commission (2010). Regulation

4. (EU) No 37/2010 of the Commission of 22 December 2009 on pharmacologically active substances and their classification as regards the maximum residue limits in foodstuffs of animal origin. Off. J. Eur. Union, L15, 1-72.

5. Anthelmintics Residues in Raw Milk. Assessing Intake by a Children Population;Tsiboukis;Pol. J. Vet. Sci.,2013

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