title: Qualitative and quantitative analysis of THC, 11-hydroxy-THC and 11-nor-9-carboxy-THC in whole blood by ultra-performance liquid chromatography/tandem mass spectrometry.
abstract: A qualitative and quantitative analytical method was developed for the simultaneous determination of Δ(9) -tetrahydrocannabinol (THC), 11-hydroxy-Δ(9) -tetrahydrocannabinol (11-OH-THC) and l1-nor-9-carboxy-Δ(9) -tetrahydrocannabinol (THC-COOH) in whole blood. The samples were prepared by solid-phase extraction followed by ultra-performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) analysis using positive ion electrospray ionization and multiple reaction monitoring. The chromatographic separation was performed with an Acquity UPLC® HSS T3 (50 × 2.1 mm i.d., 1.8 µm) reversed-phase column using a methanol/2 mM ammonium formate (formic acid 0.1%) gradient in a total run time of 9.5 min. MS/MS detection was achieved with two precursor-product ion transitions per substance. The method was fully validated, including selectivity and capacity of identification, according to the identification criteria (two transitions per substance, signal-to-noise ratio, relative retention time and ion ratio) without the presence of interferences, limit of detection (0.2 µg/L for THC and 0.5 µg/L for 11-OH-THC and THC-COOH), limit of quantitation (0.5 µg/L for all cannabinoids), recovery (53-115%), carryover, matrix effect (34-43%), linearity (0.5-100 µg/L), intra-assay precision (CV < 10% for the relative peak area ratios and <0.1% for the relative retention time), inter-assay accuracy (mean relative error <10%) and precision (CV <11%). The method has already been successfully used in proficiency tests and subsequently applied to authentic samples in routine forensic analysis.
authors: National Institute of Legal Medicine-South Branch, Rua Manuel Bento de Sousa nº3, 1169-201 Lisbon, Portugal. ssimoes@dlinml.mj.pt
authors: Susana Sadler
authors: SS
authors: Simões
authors: Antonio Castañera
authors: AC
authors: Ajenjo
authors: Mário João
authors: MJ
authors: Dias
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D013759:Dronabinol / Q000031:analogs & derivatives* / Q000097:blood / Q000737:chemistry*; D006801:Humans; D011619:Psychotropic Drugs / Q000097:blood / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D011619:Psychotropic Drugs; C016780:11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic acid; D013759:Dronabinol