Analysis of ketamine and norketamine in hair samples using molecularly imprinted solid-phase extraction (MISPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS)

Harun, N., Anderson, R. A. and Cormack, P. A. G. (2010) Analysis of ketamine and norketamine in hair samples using molecularly imprinted solid-phase extraction (MISPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Analytical and Bioanalytical Chemistry, 396(7), pp. 2449-2459. (doi: 10.1007/s00216-009-3404-6)

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Abstract

An anti-ketamine molecularly imprinted polymer (MIP) was synthesized and used as the sorbent in a solid-phase extraction protocol to isolate ketamine and norketamine from human hair extracts prior to LC-MS/MS analysis. Under optimised conditions, the MIP was capable of selectively rebinding ketamine, a licensed anaesthetic that is widely misused as a recreational drug, with an apparent binding capacity of 0.13 mu g ketamine per mg polymer. The limit of detection (LOD) and lower limit of quantification (LLOQ) for both ketamine and norketamine were 0.1 ng/mg hair and 0.2 ng/mg hair, respectively, when 10 mg hair were analysed. The method was linear from 0.1 to 10 ng/mg hair, with correlation coefficients (R-2) of better than 0.99 for both ketamine and norketamine. Recoveries from hair samples spiked with ketamine and norketamine at a concentration of 50 ng/mg were 86% and 88%, respectively. The method showed good intra-and interday precisions (<5%) for both analytes. Minimal matrix effects were observed during the LC-MS/MS analysis of ketamine (ion suppression -6.8%) and norketamine (ion enhancement +0.2%). Results for forensic case samples demonstrated that the method successfully detected ketamine and norketamine concentrations in hair samples with analyte concentrations ranging from 0.2 to 5.7 ng/mg and from 0.1 to 1.2 ng/mg, respectively

Item Type:Articles
Keywords:ABUSE AMPHETAMINES BINDING DIAZEPAM Hair Human Ketamine LC-MS/MS MASS Mass spectrometry MASS-SPECTROMETRY METABOLITES MIPs MS Norketamine OPIATES POLYMERS QUANTIFICATION RECOVERY RISK Scotland SELECTIVITY SPE URINE SAMPLES
Status:Published
Refereed:Yes
Glasgow Author(s) Enlighten ID:Anderson, Dr Robert
Authors: Harun, N., Anderson, R. A., and Cormack, P. A. G.
College/School:College of Medical Veterinary and Life Sciences > School of Medicine, Dentistry & Nursing > Clinical Specialities
Journal Name:Analytical and Bioanalytical Chemistry
ISSN:1618-2642

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