Molecularly imprinted polymer for selective determination of Δ9-tetrahydrocannabinol and 11-nor-Δ9-tetrahydrocannabinol carboxylic acid using LC-MS/MS in urine and oral fluid

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作者
E. Lendoiro
A. de Castro
H. Fernández-Vega
M. C. Cela-Pérez
J. M. López-Vilariño
M. V. González-Rodríguez
A. Cruz
M. López-Rivadulla
机构
[1] Universidad de Santiago de Compostela,Servicio de Toxicología, Instituto de Ciencias Forenses
[2] Cienytech,Departamento de I + D
[3] Universidad de A Coruña,Grupo de Polímeros, Centro de Investigaciones Tecnológicas
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Molecularly imprinted polymer; Oral fluid; Urine; THC; THC-COOH; LC-MS/MS;
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摘要
The use of molecularly imprinted polymers (MIPs) for solid phase extraction (MISPE) allows a rapid and selective extraction compared with traditional methods. Determination of Δ9-tetrahydrocannabinol (THC) and 11-nor-Δ9-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 × 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.
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页码:3589 / 3597
页数:8
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