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J Chromatogr A ; 1451: 15-22, 2016 Jun 17.
Article in English | MEDLINE | ID: mdl-27207577

ABSTRACT

A selective molecularly imprinted polymer synthesized for the selective retention of cocaine (COC) and its metabolites [benzoylecgonine (BZE), ecgonine methyl ester (EME), and cocaethylene (CE)] was used as a solid adsorbent for assessing cocaine abuse by plasma analysis. The MIP beads (50mg) were loaded inside a cone shaped device made of a polypropylene (PP) membrane for micro-solid-phase extraction (µ-SPE). High performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was used for quantifying the analytes after MIP-µ-SPE. The best retention capabilities were reached when loading plasma samples (within the 0.1-5.0mL range), previously adjusted to pH 5.5 by orbital-horizontal shaking (150rpm, 50°C) for 10min. Analyte elution was achieved by subjecting the MIP-µ-SPE device to ultrasound (37kHz, 325W) with 10mL of dichloromethane/2-propanol/ammonium hydroxide (76:20:4) for 8min. After eluate evaporation to dryness and re-dissolution in 100µL of mobile phase, the MIP-µ-SPE method yielded a pre-concentration factor of 50. Precision was assessed by intra-day and inter-day assays, and accuracy (intraday and inter-day analytical recovery, as well as the analysis of a BTMF 1/11-B control serum sample) show that the developed method is highly precise and accurate. In addition, the limits of detection, ranging from 0.061ngmL(-1) for COC to 0.87ngmL(-1) for BZE, were low enough for confirmative conclusions regarding cocaine abuse. The method was used for screening/quantifying cocaine and metabolites in plasma samples from poly-drug abusers.


Subject(s)
Cocaine/blood , Cocaine/metabolism , Molecular Imprinting , Solid Phase Extraction/methods , Chromatography, High Pressure Liquid , Cocaine/analogs & derivatives , Drug Users , Humans , Polymers/chemistry , Porosity , Tandem Mass Spectrometry , Time Factors
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