PMID- 26342308 OWN - NLM STAT- MEDLINE DCOM- 20161025 LR - 20191210 IS - 1618-2650 (Electronic) IS - 1618-2642 (Linking) VI - 408 IP - 7 DP - 2016 Mar TI - Molecularly imprinted polymer beads for clean-up and preconcentration of beta-lactamase-resistant penicillins in milk. PG - 1843-54 LID - 10.1007/s00216-015-8941-6 [doi] AB - This work describes the development and application of class-selective molecularly imprinted polymers (MIPs) for the analysis of beta-lactamase-resistant penicillins, namely cloxacillin (CLOXA), oxacillin (OXA), and dicloxacillin (DICLOXA), in milk samples. Our method is based on molecularly imprinted solid-phase extraction (MISPE) coupled to high-performance liquid chromatography (HPLC) with diode-array detection (DAD). 2-Biphenylylpenicillin (2BPEN), a surrogate with a close resemblance to beta-lactamase-resistant penicillins in terms of size, shape, hydrophobicity, and functionality, was synthesized and used as the template for the polymer synthesis. A MIP library was prepared and screened to select the optimum functional monomer, N-(2-aminoethyl)methacrylamide, and cross-linker, trimethylolpropane trimethacrylate, that provided the best recognition for the target antibiotics. For the MISPE application, the MIPs were prepared in the form of microspheres, using porous silica beads (40-75 mum) as sacrificial scaffolds. The developed MISPE method enables efficient extraction from aqueous samples and analysis of the antimicrobials, when followed by a selective washing with 2 mL acetonitrile-water (20:80 v/v) and elution with 1 mL 0.05 mol L(-1) tetrabutylammonium in methanol. The analytical method was validated according to EU guideline 2002/657/EC. The limits of quantification (S/N = 10) were in the 5.3-6.3 mug kg(-1) range, well below the maximum residue limits (MRLs) currently established. Inter-day mean recoveries were in the range 99-102 % with RSDs below 9 %, improving on the performance of previously reported MISPE methods for the analysis of CLOXA, OXA, or DICLOXA in milk samples. FAU - Urraca, Javier L AU - Urraca JL AD - Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, 28040, Madrid, Spain. jurracar@quim.ucm.es. AD - CEI Campus Moncloa, UCM-UPM, Avda Complutense s/n, 28040, Madrid, Spain. jurracar@quim.ucm.es. FAU - Chamorro-Mendiluce, Raquel AU - Chamorro-Mendiluce R AD - Department of Organic Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, 28040, Madrid, Spain. FAU - Orellana, Guillermo AU - Orellana G AD - Department of Organic Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, 28040, Madrid, Spain. FAU - Moreno-Bondi, Maria C AU - Moreno-Bondi MC AD - Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, 28040, Madrid, Spain. mcmbondi@quim.ucm.es. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PT - Validation Study DEP - 20150905 PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 RN - 0 (Anti-Bacterial Agents) RN - 0 (Penicillins) RN - 0 (Polymers) RN - COF19H7WBK (Dicloxacillin) RN - EC 3.5.2.6 (beta-Lactamases) RN - O6X5QGC2VB (Cloxacillin) RN - UH95VD7V76 (Oxacillin) SB - IM MH - Animals MH - Anti-Bacterial Agents/*isolation & purification MH - Chromatography, High Pressure Liquid/methods MH - Cloxacillin/isolation & purification MH - Dicloxacillin/isolation & purification MH - Limit of Detection MH - Milk/*chemistry MH - Molecular Imprinting/*methods MH - Oxacillin/isolation & purification MH - Penicillins/*isolation & purification MH - Polymers/*chemistry MH - Solid Phase Extraction/*methods MH - beta-Lactamases/metabolism OTO - NOTNLM OT - MISPE OT - Method validation OT - Milk OT - Molecularly imprinted polymers OT - Penicillin OT - Surrogate template EDAT- 2015/09/08 06:00 MHDA- 2016/10/26 06:00 CRDT- 2015/09/07 06:00 PHST- 2015/06/07 00:00 [received] PHST- 2015/07/25 00:00 [accepted] PHST- 2015/07/21 00:00 [revised] PHST- 2015/09/07 06:00 [entrez] PHST- 2015/09/08 06:00 [pubmed] PHST- 2016/10/26 06:00 [medline] AID - 10.1007/s00216-015-8941-6 [pii] AID - 10.1007/s00216-015-8941-6 [doi] PST - ppublish SO - Anal Bioanal Chem. 2016 Mar;408(7):1843-54. doi: 10.1007/s00216-015-8941-6. Epub 2015 Sep 5.