PMID- 20301101 OWN - NLM STAT- MEDLINE DCOM- 20100622 LR - 20151119 IS - 1097-0231 (Electronic) IS - 0951-4198 (Linking) VI - 24 IP - 8 DP - 2010 Apr 30 TI - 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. PG - 1133-41 LID - 10.1002/rcm.4499 [doi] AB - 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. CI - Copyright (c) 2010 John Wiley & Sons, Ltd. FAU - Chebbah, C AU - Chebbah C AD - Doping Control Laboratory, Department of Clinical Biology, Microbiology and Immunology, Ghent University - UGent, Technologiepark 30, B-9052 Zwijnaarde, Belgium. charaf.chebbah@UGent.be FAU - Pozo, O J AU - Pozo OJ FAU - Deventer, K AU - Deventer K FAU - Van Eenoo, P AU - Van Eenoo P FAU - Delbeke, F T AU - Delbeke FT LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - England TA - Rapid Commun Mass Spectrom JT - Rapid communications in mass spectrometry : RCM JID - 8802365 RN - 4TPC9E4A32 (11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic acid) RN - 7J8897W37S (Dronabinol) SB - IM MH - Chromatography, Liquid/*methods MH - *Doping in Sports MH - Dronabinol/*analogs & derivatives/chemistry/urine MH - Humans MH - Linear Models MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Tandem Mass Spectrometry/*methods EDAT- 2010/03/20 06:00 MHDA- 2010/06/23 06:00 CRDT- 2010/03/20 06:00 PHST- 2010/03/20 06:00 [entrez] PHST- 2010/03/20 06:00 [pubmed] PHST- 2010/06/23 06:00 [medline] AID - 10.1002/rcm.4499 [doi] PST - ppublish SO - Rapid Commun Mass Spectrom. 2010 Apr 30;24(8):1133-41. doi: 10.1002/rcm.4499.