PMID- 26526910 OWN - NLM STAT- MEDLINE DCOM- 20160708 LR - 20151103 IS - 1873-4324 (Electronic) IS - 0003-2670 (Linking) VI - 898 DP - 2015 Oct 22 TI - Porous membrane-protected molecularly imprinted polymer micro-solid-phase extraction for analysis of urinary cocaine and its metabolites using liquid chromatography - Tandem mass spectrometry. PG - 50-9 LID - S0003-2670(15)01236-2 [pii] LID - 10.1016/j.aca.2015.10.002 [doi] AB - Porous membrane-protected micro-solid phase extraction (mu-SPE) using a molecularly imprinted polymer (MIP) as an adsorbent has been proposed as an integrated extraction-cleanup procedure for isolating cocaine (COC) and its metabolites [benzoylecgonine (BZE), ecgonine methyl ester (EME), and cocaethylene (CE)] from human urine. MIP beads have been synthesized using COC as a template molecule, ethylene dimethacrylate (EDMA) as a functional monomer, divinylbenzene (DVB) as a cross-linker, and 2,2'-azobisisobutyronitrile (AIBN) as an initiator. High performance liquid chromatography - tandem mass spectrometry (HPLC-MS/MS) has been used for quantifying the analytes after MIP-mu-SPE. Variables such as urine pH, adsorption temperature and time, mechanical (orbital-horizontal) stirring; and composition of the eluting solution and eluting time, were evaluated. The proposed method was shown to be precise and accurate [relative standard deviations (RSDs) of intra- and inter-day tests ranging from 3 to 8% and from 2 to 10%, respectively]; and analytical recoveries in the range of 89-100%). In addition, excellent accuracy was also verified after analyzing a FDT +25% control material for BZE. The detection limits were in the range of 0.16-1.7 ng L(-1), low enough for confirmative conclusions regarding cocaine abuse. The method was finally applied for screening/quantifying cocaine and metabolites in urine samples from poly-drug abusers. CI - Copyright (c) 2015 Elsevier B.V. All rights reserved. FAU - Sanchez-Gonzalez, Juan AU - Sanchez-Gonzalez J AD - Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n, 15782, Santiago de Compostela, Spain. FAU - Tabernero, Maria Jesus AU - Tabernero MJ AD - Department of Pathologic Anatomy and Forensic Sciences, Faculty of Medicine, University of Santiago de Compostela, Rua de San Francisco, s/n, 15782, Santiago de Compostela, Spain. FAU - Bermejo, Ana Maria AU - Bermejo AM AD - Department of Pathologic Anatomy and Forensic Sciences, Faculty of Medicine, University of Santiago de Compostela, Rua de San Francisco, s/n, 15782, Santiago de Compostela, Spain. FAU - Bermejo-Barrera, Pilar AU - Bermejo-Barrera P AD - Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n, 15782, Santiago de Compostela, Spain. FAU - Moreda-Pineiro, Antonio AU - Moreda-Pineiro A AD - Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n, 15782, Santiago de Compostela, Spain. Electronic address: antonio.moreda@usc.es. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20151021 PL - Netherlands TA - Anal Chim Acta JT - Analytica chimica acta JID - 0370534 RN - 0 (Polymers) RN - I5Y540LHVR (Cocaine) SB - IM MH - Chromatography, Liquid/*methods MH - Cocaine/*urine MH - Humans MH - Microscopy, Electron, Scanning MH - *Molecular Imprinting MH - Polymers/*chemistry MH - Porosity MH - Reproducibility of Results MH - Solid Phase Microextraction/*methods MH - Tandem Mass Spectrometry/*methods OTO - NOTNLM OT - Cocaine OT - High performance liquid chromatography tandem mass spectrometry OT - Human urine OT - Micro-solid phase extraction OT - Molecularly imprinted polymer OT - Porous membrane-protected EDAT- 2015/11/04 06:00 MHDA- 2016/07/09 06:00 CRDT- 2015/11/04 06:00 PHST- 2015/07/31 00:00 [received] PHST- 2015/09/30 00:00 [revised] PHST- 2015/10/07 00:00 [accepted] PHST- 2015/11/04 06:00 [entrez] PHST- 2015/11/04 06:00 [pubmed] PHST- 2016/07/09 06:00 [medline] AID - S0003-2670(15)01236-2 [pii] AID - 10.1016/j.aca.2015.10.002 [doi] PST - ppublish SO - Anal Chim Acta. 2015 Oct 22;898:50-9. doi: 10.1016/j.aca.2015.10.002. Epub 2015 Oct 21.