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Quantification of six cannabinoids and metabolites in oral fluid by liquid chromatography-tandem mass spectrometry.
Drug Test Anal 2015; 7(8):684-94DT

Abstract

Δ(9) -Tetrahydrocannabinol (THC) is the most commonly analyzed cannabinoid in oral fluid (OF); however, its metabolite 11-nor-9-carboxy-THC (THCCOOH) offers the advantage of documenting active consumption, as it is not detected in cannabis smoke. Analytical challenges such as low (ng/L) THCCOOH OF concentrations hampered routine OF THCCOOH monitoring. Presence of minor cannabinoids like cannabidiol and cannabinol offer the advantage of identifying recent cannabis intake. Published OF cannabinoids methods have limitations, including few analytes and lengthy derivatization. We developed and validated a sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for THC, its metabolites, 11-hydroxy-THC and THCCOOH quantification, and other natural cannabinoids including tetrahydrocannabivarin (THCV), cannabidiol (CBD), and cannabigerol (CBG) in 1 mL OF collected with the Quantisal device. After solid-phase extraction, chromatography was performed on a Selectra PFPP column with a 0.15% formic acid in water and acetonitrile gradient with a 0.5 mL/min flow rate. All analytes were monitored in positive mode atmospheric pressure chemical ionization (APCI) with multiple reaction monitoring. Limits of quantification were 15 ng/L THCCOOH and 0.2 µg/L for all other analytes. Linear ranges extended to 3750 ng/L THCCOOH, 100 µg/L THC, and 50 µg/L for all other analytes. Inter-day analytical recoveries (bias) and imprecision at low, mid, and high quality control (QC) concentrations were 88.7-107.3% and 2.3-6.7%, respectively (n = 20). Mean extraction efficiencies and matrix effects evaluated at low and high QC were 75.9-86.1% and 8.4-99.4%, respectively. This method will be highly useful for workplace, criminal justice, drug treatment and driving under the influence of cannabis OF testing.

Authors+Show Affiliations

Chemistry and Drug Metabolism, Intramural Research Program, National Institute on Drug Abuse, National Institutes of Health, 251 Bayview Boulevard, Baltimore, MD, 21224, USA. Program in Toxicology, University of Maryland Baltimore, 620 W. Lexington St, Baltimore, MD, 21201, USA.Chemistry and Drug Metabolism, Intramural Research Program, National Institute on Drug Abuse, National Institutes of Health, 251 Bayview Boulevard, Baltimore, MD, 21224, USA.Chemistry and Drug Metabolism, Intramural Research Program, National Institute on Drug Abuse, National Institutes of Health, 251 Bayview Boulevard, Baltimore, MD, 21224, USA.

Pub Type(s)

Journal Article
Research Support, N.I.H., Intramural
Validation Studies

Language

eng

PubMed ID

25428610

Citation

Desrosiers, Nathalie A., et al. "Quantification of Six Cannabinoids and Metabolites in Oral Fluid By Liquid Chromatography-tandem Mass Spectrometry." Drug Testing and Analysis, vol. 7, no. 8, 2015, pp. 684-94.
Desrosiers NA, Scheidweiler KB, Huestis MA. Quantification of six cannabinoids and metabolites in oral fluid by liquid chromatography-tandem mass spectrometry. Drug Test Anal. 2015;7(8):684-94.
Desrosiers, N. A., Scheidweiler, K. B., & Huestis, M. A. (2015). Quantification of six cannabinoids and metabolites in oral fluid by liquid chromatography-tandem mass spectrometry. Drug Testing and Analysis, 7(8), pp. 684-94. doi:10.1002/dta.1753.
Desrosiers NA, Scheidweiler KB, Huestis MA. Quantification of Six Cannabinoids and Metabolites in Oral Fluid By Liquid Chromatography-tandem Mass Spectrometry. Drug Test Anal. 2015;7(8):684-94. PubMed PMID: 25428610.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Quantification of six cannabinoids and metabolites in oral fluid by liquid chromatography-tandem mass spectrometry. AU - Desrosiers,Nathalie A, AU - Scheidweiler,Karl B, AU - Huestis,Marilyn A, Y1 - 2014/11/26/ PY - 2014/08/23/received PY - 2014/10/07/revised PY - 2014/10/24/accepted PY - 2014/11/28/entrez PY - 2014/11/28/pubmed PY - 2016/5/5/medline KW - LC-MS/MS KW - THC KW - THCCOOH KW - cannabinoids KW - oral fluid SP - 684 EP - 94 JF - Drug testing and analysis JO - Drug Test Anal VL - 7 IS - 8 N2 - Δ(9) -Tetrahydrocannabinol (THC) is the most commonly analyzed cannabinoid in oral fluid (OF); however, its metabolite 11-nor-9-carboxy-THC (THCCOOH) offers the advantage of documenting active consumption, as it is not detected in cannabis smoke. Analytical challenges such as low (ng/L) THCCOOH OF concentrations hampered routine OF THCCOOH monitoring. Presence of minor cannabinoids like cannabidiol and cannabinol offer the advantage of identifying recent cannabis intake. Published OF cannabinoids methods have limitations, including few analytes and lengthy derivatization. We developed and validated a sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for THC, its metabolites, 11-hydroxy-THC and THCCOOH quantification, and other natural cannabinoids including tetrahydrocannabivarin (THCV), cannabidiol (CBD), and cannabigerol (CBG) in 1 mL OF collected with the Quantisal device. After solid-phase extraction, chromatography was performed on a Selectra PFPP column with a 0.15% formic acid in water and acetonitrile gradient with a 0.5 mL/min flow rate. All analytes were monitored in positive mode atmospheric pressure chemical ionization (APCI) with multiple reaction monitoring. Limits of quantification were 15 ng/L THCCOOH and 0.2 µg/L for all other analytes. Linear ranges extended to 3750 ng/L THCCOOH, 100 µg/L THC, and 50 µg/L for all other analytes. Inter-day analytical recoveries (bias) and imprecision at low, mid, and high quality control (QC) concentrations were 88.7-107.3% and 2.3-6.7%, respectively (n = 20). Mean extraction efficiencies and matrix effects evaluated at low and high QC were 75.9-86.1% and 8.4-99.4%, respectively. This method will be highly useful for workplace, criminal justice, drug treatment and driving under the influence of cannabis OF testing. SN - 1942-7611 UR - https://www.unboundmedicine.com/medline/citation/25428610/Quantification_of_six_cannabinoids_and_metabolites_in_oral_fluid_by_liquid_chromatography_tandem_mass_spectrometry_ L2 - https://doi.org/10.1002/dta.1753 DB - PRIME DP - Unbound Medicine ER -