Uncertainty evaluation of the analysis of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol in hair by GC-NCI-MS/MS

GC-NCI-MS/MS를 이용한 모발 중 대마 대사체 분석의 측정불확도 평가

  • Kim, Jin-Young (Drug Analysis Laboratory, Supreme Prosecutors' Office) ;
  • Lee, Jae-Il (Drug Analysis Laboratory, Supreme Prosecutors' Office) ;
  • Cheong, Jae-Chul (Drug Analysis Laboratory, Supreme Prosecutors' Office) ;
  • Suh, Yong-Jun (Drug Analysis Laboratory, Supreme Prosecutors' Office) ;
  • In, Moon-Kyo (Drug Analysis Laboratory, Supreme Prosecutors' Office)
  • Received : 2010.08.17
  • Accepted : 2011.01.25
  • Published : 2011.02.25


We described an estimation of measurement uncertainty in quantitative analysis of 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THC-COOH), the metabolite of ${\Delta}^9$-tetrahydrocannabinol, in hair samples by using the bead-assisted liquid-liquid extraction and gas chromatography-tandem mass spectrometric (GC-NCI-MS/MS) detection. Traceability of measurement was established through the use of reference materials, calibrated volumetric tubes, volume measuring devices, and measuring instruments. The analytical results were compared and the different contributions to the uncertainty were evaluated. Inter-day variation was performed by using statistical analysis of several indicative factors. Measurement uncertainty associated with the analyte in real forensic hair samples were estimated using QC data. The major factor of contribution to combined standard uncertainty was inter-day repeatability, while those associated with preparation of analytical standard and also sample of weight were insignificant considering the degree of contribution. Relative uncertainty of relative extended standard uncertainty divided into the measured concentration of the analyte was 17% in a hair sample. The uncertainty of result evaluation will be invaluable to improve quality of the analysis.


Supported by : 한국연구재단(KRF)


  1. 대검찰청, "2009 마약류범죄백서", 2010.
  2. M. E. Wall, D. R. Brine, G. A. Brine, C. G. Pitt, R. I. Freudenthal and H. D. Christensen, J. Am. Chem. Soc., 92, 3466-3468(1970).
  3. S. Agurell, I. M. Nilsson and M. Widman, In Marihuana Chemistry, 'Biochemistry and Cellular Effects', 141, Springer-Verlag, New York, U.S.A., 1976.
  4. U.S. Department of Heath and Human Servies, 'NIDA Research Monograph 42', 43, National Institute on Drug Abuse, Rockville, MD, U.S.A., 1982.
  5. T. Saito, I. Yamamoto, T. Kusakabe, X. L. Huang, N. Yukawa and S. Takeichi, Forensic Sci. Int., 112, 65-71(2000).
  6. A. P. Mason and A. J. McBay, J. Forensic Sci., 30, 615-631(1985).
  7. K. M. Clauwaert, J. F. Van Bocxlaer, W. E. Lambert and A. P. De Leenheer, Forensic Sci. Int., 110, 157-166(2000).
  8. H. Sachs and P. Kintz, J. Chromatogr. B, 713, 147-161(1998).
  9. M. Rothe, F. Pragst, K. Spiegel, T. Harrach, K. Fischer and J. Kunkel, Forensic Sci. Int., 89, 111-128(1997).
  10. J. Y. Kim and M. K. In, Rapid Commun. Mass Spectrom., 21, 1339-1342(2007).
  11. 한국표준과학연구원, "측정불확도 표현지침", 1998.
  12. Korea Laboratory Accreditation Scheme (KOLAS), "측정결과의 불확도 산정 및 표현을 위한 지침", 2000.
  13. KS Q 4001, "측정결과의 불확도 추정 및 표현을 위한 지침", 2005.
  14. ISO, "Guide to the Expression of Uncertainty in Measurement", ISO, Geneva, Switzerland, 1993.
  15. EURACHEM/CITAC, "Quantifying Uncertainty in Analytical Measurement", 2nd Ed., EURACHEM/CITAC Guide CG 4, 2000.
  16. 한국표준과학연구원, "도전! 측정불확도, 기초에서 중급까지", 2008.