Tags

Type your tag names separated by a space and hit enter

Direct quantification of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid in urine by liquid chromatography/tandem mass spectrometry in relation to doping control analysis.
Rapid Commun Mass Spectrom. 2010 Apr 30; 24(8):1133-41.RC

Abstract

An accurate and precise method for the quantification of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid (THCA) in urine by liquid chromatography/tandem mass spectrometry (LC/MS/MS) for doping analysis purposes has been developed. The method involves the use of only 200 microL of urine and the use of D(9)-THCA as internal standard. No extraction procedure is used. The urine samples are hydrolysed using sodium hydroxide and diluted with a mixture of methanol/glacial acetic acid (1:1). Chromatographic separation is achieved using a C8 column with gradient elution. All MS and MS/MS parameters were optimised in both positive and negative electrospray ionisation modes. For the identification and the quantification of THCA three product ions are monitored in both ionisation modes. The method is linear over the studied range (5-40 ng/mL), with satisfactory intra-and inter-assay precision, and the relative standard deviations (RSDs) are lower than 15%. Good accuracy is achieved with bias less than 10% at all levels tested. No significant matrix effects are observed. The selectivity and specificity are satisfactory, and no interferences are detected. The LC/MS/MS method was applied for the analysis of 48 real urine samples previously analysed with a routine gas chromatography/mass spectrometry (GC/MS) method. A good correlation between the two methods was obtained (r(2) > 0.98) with a slope close to 1.

Authors+Show Affiliations

Doping Control Laboratory, Department of Clinical Biology, Microbiology and Immunology, Ghent University - UGent, Technologiepark 30, B-9052 Zwijnaarde, Belgium. charaf.chebbah@UGent.beNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

20301101

Citation

Chebbah, C, et al. "Direct Quantification of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic Acid in Urine By Liquid Chromatography/tandem Mass Spectrometry in Relation to Doping Control Analysis." Rapid Communications in Mass Spectrometry : RCM, vol. 24, no. 8, 2010, pp. 1133-41.
Chebbah C, Pozo OJ, Deventer K, et al. Direct quantification of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid in urine by liquid chromatography/tandem mass spectrometry in relation to doping control analysis. Rapid Commun Mass Spectrom. 2010;24(8):1133-41.
Chebbah, C., Pozo, O. J., Deventer, K., Van Eenoo, P., & Delbeke, F. T. (2010). Direct quantification of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid in urine by liquid chromatography/tandem mass spectrometry in relation to doping control analysis. Rapid Communications in Mass Spectrometry : RCM, 24(8), 1133-41. https://doi.org/10.1002/rcm.4499
Chebbah C, et al. Direct Quantification of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic Acid in Urine By Liquid Chromatography/tandem Mass Spectrometry in Relation to Doping Control Analysis. Rapid Commun Mass Spectrom. 2010 Apr 30;24(8):1133-41. PubMed PMID: 20301101.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Direct quantification of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid in urine by liquid chromatography/tandem mass spectrometry in relation to doping control analysis. AU - Chebbah,C, AU - Pozo,O J, AU - Deventer,K, AU - Van Eenoo,P, AU - Delbeke,F T, PY - 2010/3/20/entrez PY - 2010/3/20/pubmed PY - 2010/6/23/medline SP - 1133 EP - 41 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 24 IS - 8 N2 - An accurate and precise method for the quantification of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid (THCA) in urine by liquid chromatography/tandem mass spectrometry (LC/MS/MS) for doping analysis purposes has been developed. The method involves the use of only 200 microL of urine and the use of D(9)-THCA as internal standard. No extraction procedure is used. The urine samples are hydrolysed using sodium hydroxide and diluted with a mixture of methanol/glacial acetic acid (1:1). Chromatographic separation is achieved using a C8 column with gradient elution. All MS and MS/MS parameters were optimised in both positive and negative electrospray ionisation modes. For the identification and the quantification of THCA three product ions are monitored in both ionisation modes. The method is linear over the studied range (5-40 ng/mL), with satisfactory intra-and inter-assay precision, and the relative standard deviations (RSDs) are lower than 15%. Good accuracy is achieved with bias less than 10% at all levels tested. No significant matrix effects are observed. The selectivity and specificity are satisfactory, and no interferences are detected. The LC/MS/MS method was applied for the analysis of 48 real urine samples previously analysed with a routine gas chromatography/mass spectrometry (GC/MS) method. A good correlation between the two methods was obtained (r(2) > 0.98) with a slope close to 1. SN - 1097-0231 UR - https://www.unboundmedicine.com/medline/citation/20301101/Direct_quantification_of_11_nor_Delta_9__tetrahydrocannabinol_9_carboxylic_acid_in_urine_by_liquid_chromatography/tandem_mass_spectrometry_in_relation_to_doping_control_analysis_ L2 - https://doi.org/10.1002/rcm.4499 DB - PRIME DP - Unbound Medicine ER -