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Accurate identification and quantification of 11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic acid in urine drug testing: evaluation of a direct high efficiency liquid chromatographic-mass spectrometric method.
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Aug 01; 871(1):101-8.JC

Abstract

A direct liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method for measurement of urinary Delta(9)-tetrahydrocannabinol carboxylic acid (THCA) was developed. The method involved dilution of the urine sample with water containing (2)H(9)-deuterated analogue as internal standard, hydrolysis with ammonia, reversed phase chromatography using a Waters ultra-performance liquid chromatography (UPLC) equipment with gradient elution, negative electrospray ionization, and monitoring of two product ions in selected reaction monitoring mode. The measuring range was 2-1000 ng/mL for THCA, and the intra- and inter-assay imprecision, expressed as the coefficient of variation, was below 5%. Influence from urine matrix on ionization efficiency was noted in infusion experiments, but was compensated for by the internal standard. Comparison with established gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry methods in authentic patient samples demonstrated accuracy in both qualitative and quantitative results. A small difference in mean ratios (~15%) may be explained by the use of different hydrolysis procedures between methods. In conclusion, the high efficiency LC-MS/MS method was capable of accurately identify and quantify THCA in urine with a capacity of 14 samples per hour.

Authors+Show Affiliations

Department of Medicine, Division of Clinical Pharmacology, Karolinska Institute and University Hospital, Stockholm, Sweden.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Comparative Study
Evaluation Study
Journal Article
Validation Study

Language

eng

PubMed ID

18620911

Citation

Stephanson, Nikolai, et al. "Accurate Identification and Quantification of 11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic Acid in Urine Drug Testing: Evaluation of a Direct High Efficiency Liquid Chromatographic-mass Spectrometric Method." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 871, no. 1, 2008, pp. 101-8.
Stephanson N, Josefsson M, Kronstrand R, et al. Accurate identification and quantification of 11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic acid in urine drug testing: evaluation of a direct high efficiency liquid chromatographic-mass spectrometric method. J Chromatogr B Analyt Technol Biomed Life Sci. 2008;871(1):101-8.
Stephanson, N., Josefsson, M., Kronstrand, R., & Beck, O. (2008). Accurate identification and quantification of 11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic acid in urine drug testing: evaluation of a direct high efficiency liquid chromatographic-mass spectrometric method. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 871(1), 101-8. https://doi.org/10.1016/j.jchromb.2008.06.047
Stephanson N, et al. Accurate Identification and Quantification of 11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic Acid in Urine Drug Testing: Evaluation of a Direct High Efficiency Liquid Chromatographic-mass Spectrometric Method. J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Aug 1;871(1):101-8. PubMed PMID: 18620911.
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TY - JOUR T1 - Accurate identification and quantification of 11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic acid in urine drug testing: evaluation of a direct high efficiency liquid chromatographic-mass spectrometric method. AU - Stephanson,Nikolai, AU - Josefsson,Martin, AU - Kronstrand,Robert, AU - Beck,Olof, Y1 - 2008/07/03/ PY - 2008/01/18/received PY - 2008/06/17/revised PY - 2008/06/26/accepted PY - 2008/7/16/pubmed PY - 2008/10/7/medline PY - 2008/7/16/entrez SP - 101 EP - 8 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 871 IS - 1 N2 - A direct liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method for measurement of urinary Delta(9)-tetrahydrocannabinol carboxylic acid (THCA) was developed. The method involved dilution of the urine sample with water containing (2)H(9)-deuterated analogue as internal standard, hydrolysis with ammonia, reversed phase chromatography using a Waters ultra-performance liquid chromatography (UPLC) equipment with gradient elution, negative electrospray ionization, and monitoring of two product ions in selected reaction monitoring mode. The measuring range was 2-1000 ng/mL for THCA, and the intra- and inter-assay imprecision, expressed as the coefficient of variation, was below 5%. Influence from urine matrix on ionization efficiency was noted in infusion experiments, but was compensated for by the internal standard. Comparison with established gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry methods in authentic patient samples demonstrated accuracy in both qualitative and quantitative results. A small difference in mean ratios (~15%) may be explained by the use of different hydrolysis procedures between methods. In conclusion, the high efficiency LC-MS/MS method was capable of accurately identify and quantify THCA in urine with a capacity of 14 samples per hour. SN - 1570-0232 UR - https://www.unboundmedicine.com/medline/citation/18620911/Accurate_identification_and_quantification_of_11_nor_delta_9__tetrahydrocannabinol_9_carboxylic_acid_in_urine_drug_testing:_evaluation_of_a_direct_high_efficiency_liquid_chromatographic_mass_spectrometric_method_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(08)00485-6 DB - PRIME DP - Unbound Medicine ER -