title: Water-compatible imprinted pills for sensitive determination of cannabinoids in urine and oral fluid.
abstract: A novel molecularly imprinted solid phase extraction (MISPE) methodology followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) has been developed using cylindrical shaped molecularly imprinted pills for detection of Δ(9)-tetrahydrocannabinol (THC), 11-nor-Δ(9)-tetrahydrocannabinol carboxylic acid (THC-COOH), cannabinol (CBN) and cannabidiol (CBD) in urine and oral fluid (OF). The composition of the molecular imprinted polymer (MIP) was optimized based on the screening results of a non-imprinted polymer library (NIP-library). Thus, acrylamide as functional monomer and ethylene glycol dimethacrylate as cross-linker were selected for the preparation of the MIP, using catechin as a mimic template. MISPE pills were incubated with 0.5 mL urine or OF sample for adsorption of analytes. For desorption, the pills were transferred to a vial with 2 mL of methanol:acetic acid (4:1) and sonicated for 15 min. The elution solvent was evaporated and reconstituted in methanol:formic acid (0.1%) 50:50 to inject in LC-MS/MS. The developed method was linear over the range from 1 to 500 ng mL(-1) in urine and from 0.75 to 500 ng mL(-1) in OF for all four analytes. Intra- and inter-day imprecision were <15%. Extraction recovery was 50-111%, process efficiency 15.4-54.5% and matrix effect ranged from -78.0 to -6.1%. Finally, the optimized and validated method was applied to 4 urine and 5 OF specimens. This is the first method for the determination of THC, THC-COOH, CBN and CBD in urine and OF using MISPE technology.
authors.affiliation: Grupo de Polímeros, Centro de Investigaciones Tecnológicas, Universidad de A Coruña, Campus de Esteiro s/n, 15403 Ferrol, Spain.
authors.forename: M Concepción
authors.initials: MC
authors.lastname: Cela-Pérez
authors.affiliation: Grupo de Polímeros, Centro de Investigaciones Tecnológicas, Universidad de A Coruña, Campus de Esteiro s/n, 15403 Ferrol, Spain.
authors.forename: Ferdia
authors.initials: F
authors.lastname: Bates
authors.affiliation: Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain.
authors.forename: Cristian
authors.initials: C
authors.lastname: Jiménez-Morigosa
authors.affiliation: Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain. Electronic address: elena.lendoiro@usc.es.
authors.forename: Elena
authors.initials: E
authors.lastname: Lendoiro
authors.affiliation: Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain.
authors.forename: Ana
authors.initials: A
authors.lastname: de Castro
authors.affiliation: Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain.
authors.forename: Angelines
authors.initials: A
authors.lastname: Cruz
authors.affiliation: Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain.
authors.forename: Manuel
authors.initials: M
authors.lastname: López-Rivadulla
authors.affiliation: Grupo de Polímeros, Centro de Investigaciones Tecnológicas, Universidad de A Coruña, Campus de Esteiro s/n, 15403 Ferrol, Spain. Electronic address: iquimica@udc.es.
authors.forename: José M
authors.initials: JM
authors.lastname: López-Vilariño
authors.affiliation: Grupo de Polímeros, Centro de Investigaciones Tecnológicas, Universidad de A Coruña, Campus de Esteiro s/n, 15403 Ferrol, Spain.
authors.forename: M Victoria
authors.initials: MV
authors.lastname: González-Rodríguez
mesh_terms: D001826:Body Fluids / Q000737:chemistry*; D002186:Cannabinoids / Q000032:analysis*; D002623:Chemistry Techniques, Analytical / Q000295:instrumentation* / Q000379:methods*; D002853:Chromatography, Liquid; D013759:Dronabinol / Q000032:analysis; D006801:Humans; D008689:Methacrylates / Q000737:chemistry; D011108:Polymers / Q000737:chemistry; D012463:Saliva / Q000737:chemistry; D052616:Solid Phase Extraction; D012997:Solvents / Q000737:chemistry; D053719:Tandem Mass Spectrometry; D014556:Urine / Q000737:chemistry; D014867:Water
chemical_list: D002186:Cannabinoids; D008689:Methacrylates; D011108:Polymers; D012997:Solvents; D014867:Water; C004919:ethylene dimethacrylate; D013759:Dronabinol
keywords: Cannabinoids; LC–MS/MS; MISPE; Oral fluid; Urine; Water-compatible