YAKHAK HOEJI (약학회지)

The Pharmaceutical Society of Korea (대한약학회)
권호 표지

Analysis of $\triangle^9$-Tetrahydrocannabinol and 11-nor-9-carboxytetrahydrocannabinol in Hair by Gas Chromatography/Mass Spectrometry

가스크로마토그라피/질량분석기에 의한 모발중 대마성분 분석

  • 양원경 (국립과학수사연구소 마약분석과) ;
  • 한은영 (국립과학수사연구소 마약분석) ;
  • 박용훈 (국립과학수사연구소 마약분석) ;
  • 임미애 (국립과학수사연구소 마약분석) ;
  • 정희선 (국립과학수사연구소 마약분석과)
  • Published : 2004.06.01
Download PDF
⟨ Previous Next ⟩

Abstract

An analytic method was developed for the quantitation of $\Delta$$^{9}-$ tetrahydrocannabinol (THC) and 11-nor-9-carboxy THC (THC-COOH) in human hair. After hair samples were pulverized using Freezer Mill, deuterated internal standards were added and digested in 1 N NaOH at $100^{\circ}C$ water bath for 30 min. Digest solutions were extracted by 5 ml hexane：ethyl acetate (90：10) after acidification with acetic acid. The organic phase was evaporated under N 2 and derivatized by BSTFA (with 1% TMCS) at $85^{\circ}C$ for 45 min. The derivatized solution was separated on HP-5MS column ($30m{\times}0.25mm{\times}0.25mm$) and detected using EI-GC-MS with selective ion monitoring mode. The assay of calibration was ranged from 5 to 100 ng/50 mg hair ($r^2$＞0.99) for THC and THC-COOH. Within and between-run precision were calculated at 6, 30, 60 ng/50 mg hair with coefficients of variation less than 11%. Within and between run accuracies at the same concentrations were$\pm$14% and $\pm$30% of target for both analytes, respectively. Absolute and relative recovery at 10 and 100 ng were 60∼91％. The method was used to detect and quantify THC and THC-COOH in cannabis abuser's hairs (N = 16) and SRM (N=5, THC 1 ng/mg, NIST). We detected THC and THC-COOH in only one hair sample. In SRM, % accuracy was 93% (range 86∼103%) and precision (% CV) was 8.14. We began to set up a quantitative analysis of THC and THC-COOH using EI-GC-MS. Continuously, we need to modify and develop this method in order to apply for identification in cannanbis users' hair.

Keywords

References

  1. Huestis, M. A. : Cannabis Monograph. SOFT Communitiees on Driving Under Influence of Drug, 1 (1994)
  2. Nakahara，Y. : Hair analysis for abused and therapeutic drugs. J. Chromatography B 733, 161 (1999)
  3. Jurado, C., Gimenez, M. P., Menendez, M. and Repetto, M. : Simutaneous quantification of opiates, cocaine and cannabi-noids in hair. Forensic Sci. Inter. 70, 165 (1995) https://doi.org/10.1016/0379-0738(94)01624-E
  4. 유영찬, 정희선, 최화경 : GC/MS 에 의한 한국인의 모발중 methamphetamine 검출. 약학회지 37, 356 (1993)
  5. 김진영, 서승일, 고범준, 이재일, 정재철, 서용준, 인문교 : 가스 크로마토그라피/질량분석기를 이용한 모발중 암페티핀형 각성제의 동시분석. 약학회지 47, 142 (2003)
  6. 박미정, 김은미, 임미애, 정희선 : GC/MS를 이용한 모발중 MDMA의 분석. 약학회지 47, 195 (2003)
  7. Moore, C., Guzaldo, F. and Donahue, T. : The determination of 11-nor-carboxytetrahydrocannabinol (THC-COOH) in hair using negative ion gas chromatography-mass spectrome$\sigma$y and high-volumne injection. J. Anal. Toxicol. 25, 555 (2001)
  8. 최화경, 진원택, 양원경, 한은영, 정희선 : GC/MS에 의한 모발 중 대마성분 분석(I). 국립과학수사연구소연보 31, 297 (1999)
  9. Chiarotti, M. and Costamagna, L. : Analysis of 11-nor-9-carboxy $\{Delta}^9$-tetrahydrocannabinol in biological samples by gas chromatography tandem mass spectrometry (GC/MS-MS). Forensic Sci. Inter. 114, 1 (2000) https://doi.org/10.1016/S0379-0738(00)00248-6
  10. Kintz, P., Cirimele, V. and Mangin, P. : Testing human hair for cannabis II. identification of THC-CCOOH by GC-MS-NCI As a unique proof. J Forensic Sci. 40, 619 (1995)
  11. Baptista, M. J., Monsanto, P. V., Marques, E. G. P., Bermejo, A., Avila, S., Castanheira , A. M., Margalho, C., Barroso, M. and Vieira, D.N. : Hair analysis for $\{Delta}^9$-THC, $\{Delta}^9$-THC-COOH, CBN and CBD, by GC/MS-EI comparison with GC/MS-PCI for $\{Delta}^9$-THC-COOH. Forensic Sci. Inter. 128, 66 (2002) https://doi.org/10.1016/S0379-0738(02)00154-8
  12. Wilkins, D., Haughey, H., Cone, Ed., Huestis, M., Foltz, R. and Rollins, D. : Quantative analysis of THC, 11-OH-THC and THC-COOH in human hair by negative ion chemical ionization mass spectrometry. J Anal. Toxi. 19, 483 (1995)
  13. Nakahara，Y., Takahashi, K. and Kikura, R. : Hair analysis for drug of Abuse. X. Effect of physicochemical properties of drugs on the Incorporation rates into hair. Biol. Pharm. Bull. 18, 1223 (1995)
  14. Cirimele, V., Kintz, P. and Mangin, P. : Testing human hair for cannabis. Forensic Sci. Inter. 70, 175 (1995) https://doi.org/10.1016/0379-0738(94)01615-C
  15. Cirimele, V., Sachs, H., Kintz, P. and Mangin, P. : Testing human hair for cannabis III. rapid screening procedure for the simultaneous identification of $\{Delta}^9$-tetrahydrocannabinol. cannabinol and Cannabidiol, J. Anal. Toxi. 20, 13 (1996)
  16. Musshoff, E, Junker, H. P., Lachenmeire, D. W.,Kroener, L. and Madea, B. : Fully automated determination of cannabinoids in hair samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry. J Anal. Toxi. 26, 1(2002)