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Reference type: Journal
Authors: Lendoiro E, Castro A, Fernández-Vega H, Cela-Pérez MC, López-Vilariño JM, González-Rodríguez MV, Cruz A, López-Rivadulla M
Article Title: Molecularly imprinted polymer for selective determination of Δ 9-tetrahydrocannabinol and 11-nor-Δ 9-tetrahydrocannabinol carboxylic acid using LC-MS/MS in urine and oral fluid.
Publication date: 2014
Journal: Analytical and Bioanalytical Chemistry
Volume: 406
Issue: (15)
Page numbers: 3589-3597.
DOI: 10.1007/s00216-013-7599-1

Abstract: The use of molecularly imprinted polymers (MIPs) for solid phase extraction (MISPE) allows a rapid and selective extraction compared with traditional methods. Determination of Δ 9-tetrahydrocannabinol (THC) and 11-nor-Δ 9-tetrahydrocannabinol carboxylic acid (THC-COOH) in oral fluid (OF) and urine was performed using homemade MISPEs for sample clean-up and liquid chromatography tandem mass spectrometry (LC-MS/MS). Cylindrical MISPE shaped pills were synthesized using catechin as a mimic template. MISPEs were added to 0.5 mL OF or urine sample and sonicated 30 min for adsorption of analytes. For desorption, the MISPE was transfered to a clean tube, and sonicated for 15 min with 2 mL acetone:acetonitrile (3:1, v/v). The elution solvent was evaporated and reconstituted in mobile phase. Chromatographic separation was performed using a SunFire C18 (2.5 μm; 2.1 x 20 mm) column, and formic acid 0.1 % and acetonitrile as mobile phase, with a total run time of 5 min. The method was fully validated including selectivity (no endogenous or exogenous interferences), linearity (1-500 ng/mL in OF, and 2.5-500 ng/mL in urine), limit of detection (0.75 and 1 ng/mL in OF and urine, respectively), imprecision (%CV <12.3 %), accuracy (98.2-107.0 % of target), extraction recovery (15.9-53.5 %), process efficiency (10.1-46.2 %), and matrix effect (£ 55 %). Analytes were stable for 72 h in the autosampler. Dilution 1:10 was assured in OF, and Quantisal™ matrix effect showed ion suppression (£ 80.4 %). The method was applied to the analysis of 20 OF and 11 urine specimens. This is the first method for determination of THC and THC-COOH in OF using MISPE technology
Template and target information: Δ 9-tetrahydrocannabinol, THC, 11-nor-Δ 9-tetrahydrocannabinol carboxylic acid, THC-COOH
Author keywords: molecularly imprinted polymer, Oral fluid, urine, THC, THC-COOH, LC-MS, MS


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