분석과학 (Analytical Science and Technology)

  • 제22권3호
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  • Pages.210-218
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  • 2009
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  • 1225-0163(pISSN)
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  • 2288-8985(eISSN)
한국분석과학회 (The Korean Society of Analytical Sciences)
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GC-MS/MS를 이용한 모발 중 암페타민 유도체 및 노르케타민 동시분석

Simultaneous determination of amphetamine derivatives and norketamine in hair by GC-MS/MS

  • Kim, Jin Young (Drug Analysis Laboratory, Supreme Prosecutors' Office) ;
  • Shin, Soon Ho (Drug Analysis Laboratory, Supreme Prosecutors' Office) ;
  • Ko, Beom Jun (Drug Analysis Laboratory, Supreme Prosecutors' Office) ;
  • Chung, Jae Cheol (Drug Analysis Laboratory, Supreme Prosecutors' Office) ;
  • Suh, Yong Jun (Drug Analysis Laboratory, Supreme Prosecutors' Office) ;
  • In, Moon Kyo (Drug Analysis Laboratory, Supreme Prosecutors' Office)
  • 투고 : 2009.04.26
  • 심사 : 2009.05.18
  • 발행 : 2009.06.25
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초록

GC-MS/MS를 이용하여 모발 중 암페타민계 마약류 4종과 노르케타민의 동시 분석법을 확립하였으며 결과의 신뢰도를 높이기 위해 분석법 검정을 실시하였다. 모발 시료의 전처리 과정은 증류수와 아세톤을 이용하여 세척, 자동분쇄기를 이용한 세절, 메탄올 용매를 이용한 추출 및 배양 그리고 HFBA로 유도체화하는 단계를 거쳐 GC-MS/MS를 이용하여 분석하였다. 그 결과 모든 분석물질에 대해 정량범위 내에서 우수한 직선성을 나타내었으며, 실제 마약 복용자의 모발감정에 이용될 수 있는 충분한 감도와 선택성, 정밀도와 정확도를 확인하였다. 검정곡선의 결정계수($r^2$)는 0.998 이상을 나타내었고 검출 한계는 0.007 ng/mg 이하였으며 회수율은 75.9-100.9%이었다. 일내 (intra-day) 및 일간 (inter-day) 정확도는 -2.6-17.0%의 범위를 나타내었으며 정밀도는 10.7%이하로 모두 기준값(20% 이하)이내의 값을 나타내었다. 확립된 분석법을 마약 복용자의 모발에 적용한 결과 메스암페타민의 농도 분포는 0.97-19.30 ng/mg이었으며 암페타민은 0.14-2.56 ng/mg이었다.

A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed and validated for simultaneous determination of amphetamine derivatives and norketamine in human hair. Preparation of hair involves external decontamination, mechanical pulverization, incubation and extraction prior to instrumental analysis. The samples were derivatized using heptafluorobutyric anhydride, and analyzed by GC-MS/MS. The linear ranges were 0.05-20.0 ng/mg for the analytes except for 3,4-methylenedioxyamphetamine, with good coefficients of determination ($r^2$ >0.998). The intra-day and inter-day precisions were within 10.7% and 8.5%, respectively. The intra-day and inter-day accuracies were between -1.6 and 17.0% and -2.6 and 10.5%, respectively. The limits of detections for each analyte were lower than 0.007 ng/mg, while recoveries were 75.9-100.9%. When the method was applied to hair samples obtained from suspected drug abusers, the concentrations in hair samples were 0.97-19.30 ng/mg for methamphetamine and 0.14-2.56 ng/mg for amphetamine.

키워드

참고문헌

  1. C. E. Cook, A. R. Jeffcoat, M. Perez-Reyes, B. M. Sadler, R. D. Voyksner, J. A. Hill, W. R. White and S. McDonald, Eur. J. Pharmacol., 183, 456-457 (1990) https://doi.org/10.1016/0014-2999(90)93345-Q
  2. H. H. Maurer, J. Bickeboeller-Friedrich, T. Kraemer and F. T. Peters, Toxicol. Lett., 112-113, 133-142(2000)
  3. A. C. Parrott, Psychopharmacology, 173(3-4), 234-241(2004) https://doi.org/10.1007/s00213-003-1712-7
  4. J. Y. Kim, M. K. In and J. H. Kim, Rapid Commun. Mass Spectrom., 20, 3159-3162(2006) https://doi.org/10.1002/rcm.2682
  5. Supreme Prosecutors' Office, Drug Trend Report, Seoul, Korea, 12, 16-18(2005)
  6. K. Kulsudjarit, Ann. N. Y. Acad. Sci., 1025, 446-457(2004) https://doi.org/10.1196/annals.1316.055
  7. F. Musshoff and B. Madea, Ther. Drug Monit., 28(2), 155-163(2006) https://doi.org/10.1097/01.ftd.0000197091.07807.22
  8. T. Saito, I. Yamamoto, T. Kusakabe, X. L. Huang, N. Yukawa and S. Takeichi, Forensic Sci. Int., 112(1), 65-71(2000) https://doi.org/10.1016/S0379-0738(00)00165-1
  9. V. A. Boumba, K. S. Ziavrou and T Vougiouklakis, Int. J. Toxicol., 25(3), 143-163(2006) https://doi.org/10.1080/10915810600683028
  10. J. Y. Kim, S. I. Suh, B. J. Ko, J. I. Lee, J. C. Jeong, Y. J. Suh and M. K. In, Yakhak Hoeji, 47(3), 142-147(2003)
  11. G. Frison, L. Tedeschi, D. Favretto, A. Reheman and S. D. Ferrara, Rapid Commun. Mass Spectrom., 19(7), 919-927(2005) https://doi.org/10.1002/rcm.1873
  12. H. Miyaguchi, Y. T. Iwata, T. Kanamori, K. Tsujikawa, K. Kuwayama and H. Inoue, J. Chromatogr. A, 1216(18), 4063-4070(2009) https://doi.org/10.1016/j.chroma.2009.02.093
  13. Y. Nakahara, Forensic Sci. Int., 70 135-153(1995) https://doi.org/10.1016/0379-0738(94)01627-H
  14. J. Y. Kim, K. S. Jung, M. K. Kim, J. I. Lee and M. K. In, Rapid Commun. Mass Spectrom., 21(11), 1705- 1720(2007) https://doi.org/10.1002/rcm.3010
  15. J. V. Goodpaster, J. J. Bishop and B. A. Benner, Jr., J. Forensic Sci., 48(2), 1-8(2003)
  16. Y. Nakahara and R. Kikura, Forensic Sci. Int., 84, 165- 177(1997) https://doi.org/10.1016/S0379-0738(96)02060-9
  17. Y. H. Wu, K. L. Lin, S. C. Chen and Y. Z. Chang, Rapid Commun. Mass Spectrom., 22(6), 887-897(2008) https://doi.org/10.1002/rcm.3409
  18. J. Y. Kim, S. I. Suh, M. K. In and B. C. Chung, J. Anal. Toxicol., 29(5), 370-375(2005) https://doi.org/10.1093/jat/29.5.370
  19. R. Kronstrand, I. Nystr$\ddot{o}$m, J. Strandberg and H. Druid, Forensic Sci. Int., 145(2-3), 183-190(2004) https://doi.org/10.1016/j.forsciint.2004.04.034
  20. R. Stanaszek and W. Piekoszewski, J. Anal. Toxicol., 28, 77-85(2004) https://doi.org/10.1093/jat/28.2.77
  21. H. Miyaguchi, M. Kakuta, Y. T. Iwata, H. Matsuda, H, Tazawa, H. Kimura and H. Inoue, J. Chromatogr. A, 1163(1), 43-48(2007) https://doi.org/10.1016/j.chroma.2007.06.017
  22. E. Han, E. Miller, J. Lee, Y. Park, M. Lim and H. Chung, J. Anal. Toxicol., 30, 380-385(2006) https://doi.org/10.1093/jat/30.6.380
  23. H. P. Eser, L. P$\ddot{o}$tsch, G. Skopp and M. R. Moeller, Forensic Sci. Int., 84(1-3), 271-279(1997) https://doi.org/10.1016/S0379-0738(96)02071-3
  24. J. Segura, R. Ventura and C. Jurado, J. Chromatogr. B, 713, 61-90(1998) https://doi.org/10.1016/S0378-4347(98)00089-9
  25. R. Bruce and W Maynard, Anal. Chem., 41(7), 977-979(1969) https://doi.org/10.1021/ac60276a003
  26. Forensic Toxicology Laboratory Guidelines 2006 Version, Society of Forensic Toxicologists (SOFT)/American Academy of Forensic Sciences (AAFS). Available: http://www.soft-tox.org/docs/Guidelines%202006%20 Final.pdf