title: Identification and quantification of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid glucuronide (THC-COOH-glu) in hair by ultra-performance liquid chromatography tandem mass spectrometry as a potential hair biomarker of cannabis use.
abstract: We developed and validated an ultra-high-pressure liquid chromatography-tandem mass spectrometry method to identify and quantify 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid glucuronide in hair of cannabis consumers. After hair washing with methyl alcohol and diethyl ether and subsequent addition of amiodarone as internal standard hair samples were treated with 500 μl VMA-T M3 buffer reagent for 1 h at 100 °C. After cooling, 10 μl VMA-T M3 extract were injected into chromatographic system. Chromatographic separation was carried out on a reversed phase column using a linear gradient elution with two solvents: 5 mM ammonium formate pH 3.0 (solvent A) and 0.1% formic acid in acetonitrile (solvent B). The flow rate was kept constant at 0.4 ml/min during the analysis. The separated analytes were detected with a triple quadrupole mass spectrometer operated in multiple reaction monitoring mode via positive electrospray ionization. Linear calibration curves were obtained for 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid glucuronide with correlation coefficients (r(2)) of 0.99 and a limit of quantification of 0.25 pg/mg hair. Analytical recovery was between 79.6% and 100.7% and intra- and inter-assay imprecision and inaccuracy were always lower than 15%. Ultra-high-pressure liquid chromatography-tandem mass spectrometry analysis of 20 different hair samples of cannabis consumers disclosed the presence of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid glucuronide in the range of 0.5-8.6 pg/mg hair. These data provided a good start to consider 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid glucuronide as alternative hair biomarker of cannabis consumption.
authors: Department of Therapeutic Research and Medicines Evaluation, Istituto Superiore di Sanitá, Rome, Italy. Electronic address: simona.pichini@iss.it.
authors: Simona
authors: S
authors: Pichini
authors: Department of Therapeutic Research and Medicines Evaluation, Istituto Superiore di Sanitá, Rome, Italy.
authors: Emilia
authors: E
authors: Marchei
authors: Università Cattolica del Sacro Cuore, Policlinico Agostino Gemelli, Rome, Italy.
authors: Simona
authors: S
authors: Martello
authors: Laboratorio di Sanità Pubblica (LSP), Azienda Provinciale Servizi Sanitari, Trento, Italy.
authors: Massimo
authors: M
authors: Gottardi
authors: Department of Therapeutic Research and Medicines Evaluation, Istituto Superiore di Sanitá, Rome, Italy.
authors: Manuela
authors: M
authors: Pellegrini
authors: Laboratorio di Sanità Pubblica (LSP), Azienda Provinciale Servizi Sanitari, Trento, Italy.
authors: Fiorenza
authors: F
authors: Svaizer
authors: Laboratorio di Sanità Pubblica (LSP), Azienda Provinciale Servizi Sanitari, Trento, Italy.
authors: Andrea
authors: A
authors: Lotti
authors: Università Cattolica del Sacro Cuore, Policlinico Agostino Gemelli, Rome, Italy.
authors: Marcello
authors: M
authors: Chiarotti
authors: Department of Therapeutic Research and Medicines Evaluation, Istituto Superiore di Sanitá, Rome, Italy.
authors: Roberta
authors: R
authors: Pacifici
mesh_terms: D015415:Biomarkers / Q000378:metabolism; D002188:Cannabis / Q000737:chemistry*; D002853:Chromatography, Liquid / Q000379:methods*; D013759:Dronabinol / Q000031:analogs & derivatives* / Q000032:analysis; D006197:Hair / Q000737:chemistry*; D006801:Humans; D015813:Substance Abuse Detection / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D015415:Biomarkers; C016780:11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic acid; D013759:Dronabinol
keywords: 11-Nor-Δ9-tetrahydrocannabinol-9-carboxylic acid glucuronide; Hair testing; Ultra-high-pressure liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS)