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Simultaneous quantification of 11 cannabinoids and metabolites in human urine by liquid chromatography tandem mass spectrometry using WAX-S tips.
Anal Bioanal Chem 2016; 408(23):6461-71AB

Abstract

A comprehensive cannabinoid urine quantification method may improve clinical and forensic result interpretation and is necessary to support our clinical research. A liquid chromatography tandem mass spectrometry quantification method for ∆(9)-tetrahydrocannabinol (THC), 11-hydroxy-THC (11-OH-THC), 11-nor-9-carboxy-THC (THCCOOH), ∆(9)-tetrahydrocannabinolic acid (THCAA), cannabinol (CBN), cannabidiol (CBD), cannabigerol (CBG), ∆(9)-tetrahydrocannabivarin (THCV), 11-nor-9-carboxy-THCV (THCVCOOH), THC-glucuronide (THC-gluc), and THCCOOH-glucuronide (THCCOOH-gluc) in urine was developed and validated according to the Scientific Working Group on Toxicology guidelines. Sample preparation consisted of disposable pipette extraction (WAX-S) of 200 μL urine. Separation was achieved on a Kinetex C18 column using gradient elution with flow rate 0.5 mL/min, mobile phase A (10 mM ammonium acetate in water), and mobile phase B (15 % methanol in acetonitrile). Total run time was 14 min. Analytes were monitored in both positive and negative ionization modes by scheduled multiple reaction monitoring. Linear ranges were 0.5-100 μg/L for THC and THCCOOH; 0.5-50 μg/L for 11-OH-THC, CBD, CBN, THCAA, and THC-gluc; 1-100 μg/L for CBG, THCV, and THCVCOOH; and 5-500 μg/L for THCCOOH-gluc (R (2) > 0.99). Analytical biases were 88.3-113.7 %, imprecisions 3.3-14.3 %, extraction efficiencies 42.4-81.5 %, and matrix effect -10 to 32.5 %. We developed and validated a comprehensive, simple, and rapid LC-MS/MS cannabinoid urine method for quantification of 11 cannabinoids and metabolites. This method is being used in a controlled cannabis administration study, investigating urine cannabinoid markers documenting recent cannabis use, chronic frequent smoking, or route of drug administration and potentially improving urine cannabinoid result interpretation.

Authors+Show Affiliations

Chemistry and Drug Metabolism Section, Clinical Pharmacology and Therapeutics Research Branch, Intramural Research Program, National Institute on Drug Abuse, National Institutes of Health, 251 Bayview Boulevard, Baltimore, MD, 21224, USA.Chemistry and Drug Metabolism Section, Clinical Pharmacology and Therapeutics Research Branch, Intramural Research Program, National Institute on Drug Abuse, National Institutes of Health, 251 Bayview Boulevard, Baltimore, MD, 21224, USA. kscheidweiler@intra.nida.nih.gov.Chemistry and Drug Metabolism Section, Clinical Pharmacology and Therapeutics Research Branch, Intramural Research Program, National Institute on Drug Abuse, National Institutes of Health, 251 Bayview Boulevard, Baltimore, MD, 21224, USA.Chemistry and Drug Metabolism Section, Clinical Pharmacology and Therapeutics Research Branch, Intramural Research Program, National Institute on Drug Abuse, National Institutes of Health, 251 Bayview Boulevard, Baltimore, MD, 21224, USA.Chemistry and Drug Metabolism Section, Clinical Pharmacology and Therapeutics Research Branch, Intramural Research Program, National Institute on Drug Abuse, National Institutes of Health, 251 Bayview Boulevard, Baltimore, MD, 21224, USA. University of Maryland School of Medicine, 655 W Baltimore St, Baltimore, MD, 21201, USA.

Pub Type(s)

Journal Article
Validation Studies

Language

eng

PubMed ID

27422645

Citation

Andersson, Maria, et al. "Simultaneous Quantification of 11 Cannabinoids and Metabolites in Human Urine By Liquid Chromatography Tandem Mass Spectrometry Using WAX-S Tips." Analytical and Bioanalytical Chemistry, vol. 408, no. 23, 2016, pp. 6461-71.
Andersson M, Scheidweiler KB, Sempio C, et al. Simultaneous quantification of 11 cannabinoids and metabolites in human urine by liquid chromatography tandem mass spectrometry using WAX-S tips. Anal Bioanal Chem. 2016;408(23):6461-71.
Andersson, M., Scheidweiler, K. B., Sempio, C., Barnes, A. J., & Huestis, M. A. (2016). Simultaneous quantification of 11 cannabinoids and metabolites in human urine by liquid chromatography tandem mass spectrometry using WAX-S tips. Analytical and Bioanalytical Chemistry, 408(23), pp. 6461-71. doi:10.1007/s00216-016-9765-8.
Andersson M, et al. Simultaneous Quantification of 11 Cannabinoids and Metabolites in Human Urine By Liquid Chromatography Tandem Mass Spectrometry Using WAX-S Tips. Anal Bioanal Chem. 2016;408(23):6461-71. PubMed PMID: 27422645.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous quantification of 11 cannabinoids and metabolites in human urine by liquid chromatography tandem mass spectrometry using WAX-S tips. AU - Andersson,Maria, AU - Scheidweiler,Karl B, AU - Sempio,Cristina, AU - Barnes,Allan J, AU - Huestis,Marilyn A, Y1 - 2016/07/15/ PY - 2016/03/28/received PY - 2016/07/04/accepted PY - 2016/06/23/revised PY - 2016/7/17/entrez PY - 2016/7/17/pubmed PY - 2018/1/26/medline KW - Cannabinoid KW - DPX KW - LC-MS/MS KW - THC KW - Urine SP - 6461 EP - 71 JF - Analytical and bioanalytical chemistry JO - Anal Bioanal Chem VL - 408 IS - 23 N2 - A comprehensive cannabinoid urine quantification method may improve clinical and forensic result interpretation and is necessary to support our clinical research. A liquid chromatography tandem mass spectrometry quantification method for ∆(9)-tetrahydrocannabinol (THC), 11-hydroxy-THC (11-OH-THC), 11-nor-9-carboxy-THC (THCCOOH), ∆(9)-tetrahydrocannabinolic acid (THCAA), cannabinol (CBN), cannabidiol (CBD), cannabigerol (CBG), ∆(9)-tetrahydrocannabivarin (THCV), 11-nor-9-carboxy-THCV (THCVCOOH), THC-glucuronide (THC-gluc), and THCCOOH-glucuronide (THCCOOH-gluc) in urine was developed and validated according to the Scientific Working Group on Toxicology guidelines. Sample preparation consisted of disposable pipette extraction (WAX-S) of 200 μL urine. Separation was achieved on a Kinetex C18 column using gradient elution with flow rate 0.5 mL/min, mobile phase A (10 mM ammonium acetate in water), and mobile phase B (15 % methanol in acetonitrile). Total run time was 14 min. Analytes were monitored in both positive and negative ionization modes by scheduled multiple reaction monitoring. Linear ranges were 0.5-100 μg/L for THC and THCCOOH; 0.5-50 μg/L for 11-OH-THC, CBD, CBN, THCAA, and THC-gluc; 1-100 μg/L for CBG, THCV, and THCVCOOH; and 5-500 μg/L for THCCOOH-gluc (R (2) > 0.99). Analytical biases were 88.3-113.7 %, imprecisions 3.3-14.3 %, extraction efficiencies 42.4-81.5 %, and matrix effect -10 to 32.5 %. We developed and validated a comprehensive, simple, and rapid LC-MS/MS cannabinoid urine method for quantification of 11 cannabinoids and metabolites. This method is being used in a controlled cannabis administration study, investigating urine cannabinoid markers documenting recent cannabis use, chronic frequent smoking, or route of drug administration and potentially improving urine cannabinoid result interpretation. SN - 1618-2650 UR - https://www.unboundmedicine.com/medline/citation/27422645/Simultaneous_quantification_of_11_cannabinoids_and_metabolites_in_human_urine_by_liquid_chromatography_tandem_mass_spectrometry_using_WAX_S_tips_ L2 - https://dx.doi.org/10.1007/s00216-016-9765-8 DB - PRIME DP - Unbound Medicine ER -