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Volume 20, Issue 9
  • ISSN: 1573-4129
  • E-ISSN: 1875-676X

Abstract

Background

Since the International Olympic Committee (IOC) was established, sports doping control analyses have revealed a high rate of positive cases for cannabinoids. Cannabinoids were banned in all sports where they were used in-competition as per the Prohibited List published annually. Further, it was also included in the threshold drug category. Consequently, developing a reliable method for urine Cannabinoids metabolite quantification plays a pivotal role in sports dope testing.

Objectives

This work aimed to develop and validate a reliable, cost-effective, robust gas chromatography-tandem mass spectrometry method for detecting (−)-11-nor-9-Carboxy-Δ9-THC component in human urine samples, in compliance with ICH and WADA guidelines.

Methods

The sample preparation was done by enzymatic hydrolysis for deconjugation, further proceeded with solid phase extraction (SPE), liquid-liquid extraction (LLE), and using an XAD2 column, and N-methyl trimethylsilyl trifluoroacetamide (MSTFA) for derivatization.

Results

The linearity was obtained in a range of 50–300 ng/mL, and the correlation coefficient was found to be higher than 0.99. Throughout the entire validation study, the difference in Retention Time (RT) for the analyte, including the Internal Standard (IS), was shown to be less than 1.0%. The quantification limit (LOQ) was calculated at a level of 50 ng/mL in human urine samples for the 3 most abundant ion transitions. The detection limit (LOD) was established at 4 ng/mL.

Conclusion

The accuracy, precision, linearity, recovery, quantification limit, and selectivity by GC-MS/MS technique were found acceptable and well satisfactory while following the ICH guidelines. The developed method has been proven to be fit for purpose in accordance with the enforced Guidelines of WADA.

© 2024 Bentham Science Publishers
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2024-10-24
2025-03-07

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References

  1. MoffadA.C. OsseltonM.D. WiddopB. Clarke’s Analysis of Drugs and Poisons.3rd edLondonPharmaceutical Press1990
     [Google Scholar]
  2. HuestisM.A. 2002Available from: http://137.187.144.24/endnote_pdfs/rm-008540.pdf (accessed on 8-10-2024)
  3. a MoffatA.C. The legalisation of Cannabis for medical use.Sci. Justice J. Forensic Sci. Soc.20024215557
     [Google Scholar]
  4. b BrenneisenR. Determination of the major Δ9-tetrahydrocannabinol metabolite in urine by high-performance liquid chromatography and photodiode array detection.Anal. Chim. Acta198719818318910.1016/S0003‑2670(00)85018‑7
     [Google Scholar]
  5. LendoiroE. de CastroA. VegaH. PérezM.C. VilariñoJ.M. RodríguezM.V. CruzA. RivadullaM. Molecularly imprinted polymer for selective determination of Δ9-tetrahydrocannabinol and 11-nor-Δ9-tetrahydrocannabinol carboxylic acid using LC-MS/MS in urine and oral fluid.Anal. Bioanal. Chem.2014406153589359710.1007/s00216‑013‑7599‑1 24429976
     [Google Scholar]
  6. MontesanoC. SergiM. OdoardiS. SimeoniM.C. CompagnoneD. CuriniR. A μ-SPE procedure for the determination of cannabinoids and their metabolites in urine by LC–MS/MS.J. Pharm. Biomed. Anal.20149116917510.1016/j.jpba.2013.12.035 24469020
     [Google Scholar]
  7. ShannonE. HavillJ. Creating creatinine: How to pass a urine drug test.Nephrol. Open J.2023711310.17140/NPOJ‑7‑126
     [Google Scholar]
  8. ScholzC. MadryM.M. KraemerT. BaumgartnerM.R. LC–MS-MS analysis of Δ9-THC, CBN and CBD in Hair: Investigation of artifacts.J. Anal. Toxicol.202246550451110.1093/jat/bkab056 34041537
     [Google Scholar]
  9. ChildsP.S. McCurdyH.H. Evaluation of a radioimmunoassay (125I) kit for cannabinoid metabolites in urine and whole blood.J. Anal. Toxicol.19848522022310.1093/jat/8.5.220 6503225
     [Google Scholar]
  10. KulkarniU. KulkarniK. PardeshiR. ManeD. High performance thin layer chromatographic detection of cannabis in forensic interest.J. Chem. Pharm. Res.20181011914
     [Google Scholar]
  11. KapurB.M. Drug-testing methods and clinical interpretations of test results.Bull. Narc.1993452115154 7920539
     [Google Scholar]
  12. MeatherallR.C. GarriottJ.C. A sensitive thin-layer chromatographic procedure for the detection of urinary 11-nor-delta 9-tetrahydrocannabinol-9-carboxylic acid.J. Anal. Toxicol.198812313614010.1093/jat/12.3.136 2838684
     [Google Scholar]
  13. ZazoğluS. AnilanmertB. AydinM. CengizS. Fast confirmation for marijuana metabolite: THC-COOH, ultra-fast LC—MS/MS run time, and application to routine samples.Acta Chromatogr.201729225326510.1556/1326.2017.29.2.09
     [Google Scholar]
  14. ParryR.C. NolanL. ShireyR.E. WachobG.D. GischD.J. Pretreatment of urine samples for the analysis of 11-nor-delta 9-tetrahydrocannabinol-9-carboxylic acid using solid-phase extraction.J. Anal. Toxicol.1990141394410.1093/jat/14.1.39 2156110
     [Google Scholar]
  15. FelliM. MartelloS. ChiarottiM. LC–MS–MS method for simultaneous determination of THCCOOH and THCCOOH-glucuronide in urine: Application to workplace confirmation tests.Forensic Sci. Int.20112041-3677310.1016/j.forsciint.2010.05.004 20627630
     [Google Scholar]
  16. WeinmannW. VogtS. GoerkeR. MüllerC. BrombergerA. Simultaneous determination of THC-COOH and THC-COOH-glucuronide in urine samples by LC/MS/MS.Forensic Sci. Int.20001131-338138710.1016/S0379‑0738(00)00210‑3 10978652
     [Google Scholar]
  17. Wahajuddin; Singh, S.P.; Jain, G.K. Determination of lumefantrine in rat plasma by liquid–liquid extraction using LC–MS/MS with electrospray ionization: Assay development, validation and application to a pharmacokinetic study.J. Chromatogr. B Analyt. Technol. Biomed. Life Sci.200987711-121133113910.1016/j.jchromb.2009.02.058 19285925
     [Google Scholar]
  18. Raising the game for clean sport.Available from: https://www.wada-ama.org (accessed on 8-10-2024)
  19. SahuP.L. MauryaA.K. PriyadarshiniS. SiddiquiA.A. SahuK. Measurement uncertainty and validation for quantitation of salbutamol in human urine by gas chromatography-tandem mass spectrometry.J. Chromatogr. Sci.202361760561110.1093/chromsci/bmac079
     [Google Scholar]
  20. BoniniS.A. PremoliM. TambaroS. KumarA. MaccarinelliG. MemoM. MastinuA. Cannabis sativa: A comprehensive ethnopharmacological review of a medicinal plant with a long history.J. Ethnopharmacol.201822730031510.1016/j.jep.2018.09.004 30205181
     [Google Scholar]
  21. RosendoL.M. RosadoT. OliveiraP. SimãoA.Y. MargalhoC. CostaS. PassarinhaL.A. BarrosoM. GallardoE. The determination of cannabinoids in urine samples using microextraction by packed sorbent and gas chromatography-mass spectrometry.Molecules20222717550310.3390/molecules27175503 36080271
     [Google Scholar]
  22. ReberJ.D. KarschnerE.L. SeitherJ.Z. KnittelJ.L. WalterscheidJ.P. Screening and confirmation methods for the qualitative identification of nine phytocannabinoids in urine by LC-MS/MS.Clin. Biochem.202198546210.1016/j.clinbiochem.2021.09.005 34529995
     [Google Scholar]
  23. RumplerM.J. Quantitative analysis of 11-nor-9-carboxy-tetrahydrocannbinol (THC–COOH) in urine by LC–MS/MS following a simple filtration.J. Chromatogr. B Analyt. Technol. Biomed. Life Sci.2014957778310.1016/j.jchromb.2014.02.056 24657414
     [Google Scholar]
  24. SharmaP. RaoV. ChandP.K. MurthyP. Quantification of Δ9-tetrahydrocannabinol in urine as a marker of cannabis abuse.Indian J. Med. Res.20231585&653554110.4103/ijmr.IJMR_3899_20 37929356
     [Google Scholar]
  25. GomesR.L. MeredithW. SnapeC.E. SephtonM.A. Analysis of conjugated steroid androgens: Deconjugation, derivatisation and associated issues.J. Pharm. Biomed. Anal.20094951133114010.1016/j.jpba.2009.01.027 19304432
     [Google Scholar]
/content/journals/cpa/10.2174/0115734129347983241023100539
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Measurement Uncertainty and Validation for Quantification of Marijuana Metabolite: (−)-11-nor-9-Carboxy-Δ9-THC in Human Urine by GC-MS/MS
Current Pharmaceutical Analysis 20, 1056 (2024); https://doi.org/10.2174/0115734129347983241023100539
/content/journals/cpa/10.2174/0115734129347983241023100539
/content/journals/cpa/10.2174/0115734129347983241023100539
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  • Article Type:     Research Article
Keyword(s): (−)-11-nor-9-Carboxy-Δ9-THC; Cannabinoids; doping control; GC-MS/MS; human urine; ICH guidelines; validation; WADA

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