PMID- 27816225 OWN - NLM STAT- MEDLINE DCOM- 20170307 LR - 20181202 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1474 DP - 2016 Nov 25 TI - Multiresidue analysis of cephalosporin antibiotics in bovine milk based on molecularly imprinted polymer extraction followed by liquid chromatography-tandem mass spectrometry. PG - 121-129 LID - S0021-9673(16)31454-6 [pii] LID - 10.1016/j.chroma.2016.10.069 [doi] AB - This work reports the preparation of molecularly imprinted polymers (MIPs) selective to cephalosporin (CF) antibiotics, and their application as molecularly imprinted solid-phase extraction (MISPE) sorbents for the determination of these antimicrobials in milk samples. Several functional monomers and cross-linkers have been screened to select the best combination that provides high selectivity for the simultaneous multiresidue extraction of cefthiofur (THIO), cefazolin (AZO), cefquinome (QUI), cephapirin (API), cephalexin (ALE) and cephalonium (ALO) from the samples. The novel MIPs were prepared by a non-covalent imprinting approach in the form of spherical microparticles using the synthetic surrogate molecule sodium 7-(2-biphenylylcarboxamido)-3-methyl-3-cepheme-4-carboxylate, N-3,5-bis(trifluoromethyl)phenyl-N'-4-vinylphenyl urea (VPU) as functional monomer, and divinylbenzene (DVB) as crosslinking agent in a 1:2:20 molar ratio. The optimized MISPE method allowed the extraction of the target antimicrobials from raw cow milk samples using a selective washing with 5mL methanol/2-[4-(2-hydroxyethyl)-1-piperazinyl]ethanesulfonic acid (HEPES) buffer (0.1M, pH 7.5) (2:98, v/v) to remove the non-specifically retained compounds, followed by elution with 1mL of trifluoroacetic acid (TFA) in methanol (0.1:99.9, v/v). The extracts have been analysed by UHPLC-MS/MS and the analytical method has been validated according to EU guideline 2002/657/EC. The limits of quantification (S/N=10) were in the 1.7-12.5mugkg(-1) range, well below the maximum residue limits (MRLs) currently established for the quantified cephalosporins in milk samples. The developed MIP allows mutiresidual determination of the six cephalosporin antibiotics mentioned above, significantly broadening the application to food analysis of MISPE methods. CI - Copyright (c) 2016 Elsevier B.V. All rights reserved. FAU - Baeza, A N AU - Baeza AN AD - Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, E-28040 Madrid, Spain; Institute of Materials Research and Engineering (IMRE), University of Havana, Havana 10400, Cuba. FAU - Urraca, J L AU - Urraca JL AD - Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, E-28040 Madrid, Spain; CEI Campus Moncloa, UCM-UPM, Avda Complutense s/n, E-28040 Madrid, Spain. Electronic address: jurracar@quim.ucm.es. FAU - Chamorro, R AU - Chamorro R AD - Department of Organic Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, E-28040 Madrid, Spain. FAU - Orellana, G AU - Orellana G AD - Department of Organic Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, E-28040 Madrid, Spain. FAU - Castellari, M AU - Castellari M AD - Institute for Food and Agricultural Research and Technology, Food Safety Program, Granja Camps i Armet s/n, Monells 17121, Girona, Spain. FAU - Moreno-Bondi, M C AU - Moreno-Bondi MC AD - Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, E-28040 Madrid, Spain. Electronic address: mcmbondi@quim.ucm.es. LA - eng PT - Journal Article DEP - 20161029 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Anti-Bacterial Agents) RN - 0 (Cephalosporins) RN - 0 (Cross-Linking Reagents) RN - 0 (Polymers) RN - 0 (Solvents) RN - E5R8Z4G708 (Trifluoroacetic Acid) RN - RWW266YE9I (HEPES) RN - Y4S76JWI15 (Methanol) SB - IM MH - Animals MH - Anti-Bacterial Agents/*analysis MH - Cattle MH - Cephalosporins/*analysis MH - Chromatography, High Pressure Liquid MH - Cross-Linking Reagents MH - Drug Residues/*analysis MH - HEPES MH - Methanol MH - Microscopy, Electron, Scanning MH - Milk/*chemistry MH - Molecular Imprinting MH - Polymers MH - Solvents MH - Tandem Mass Spectrometry MH - Trifluoroacetic Acid OTO - NOTNLM OT - Cephalosporins OT - MISPE OT - Milk analysis OT - Molecularly imprinted polymers EDAT- 2016/11/07 06:00 MHDA- 2017/03/08 06:00 CRDT- 2016/11/07 06:00 PHST- 2016/07/14 00:00 [received] PHST- 2016/10/10 00:00 [revised] PHST- 2016/10/27 00:00 [accepted] PHST- 2016/11/07 06:00 [pubmed] PHST- 2017/03/08 06:00 [medline] PHST- 2016/11/07 06:00 [entrez] AID - S0021-9673(16)31454-6 [pii] AID - 10.1016/j.chroma.2016.10.069 [doi] PST - ppublish SO - J Chromatogr A. 2016 Nov 25;1474:121-129. doi: 10.1016/j.chroma.2016.10.069. Epub 2016 Oct 29.