Journal of Analytical Chemistry

, Volume 65, Issue 9, pp 951–959 | Cite as

GC-FID optimization and validation for determination of 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyamphetamine and methamphetamine in ecstasy tablets

  • A. Phonchai
  • B. Janchawee
  • S. Prutipanlai
  • S. Thainchaiwattana
Articles

Abstract

A methodology for the determination of 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA) and methamphetamine (MA) in seized tablets using gas chromatography with a flame ionization detector (GC-FID) is described. The chromatographic conditions, i.e. gas flow rates and temperatures for the column, injector and detector were optimized. The optimum chromatographic conditions were as follows: a CP-SIL 24 CB WCOT fused silica capillary column (30 m × 0.32 mm I.D., 0.25 μm film thickness), N2 carrier gas flowing at 2.6 mL/min, injector temperature at 290°C and detector temperature at 300°C. The oven temperature was ramped from 80°C at a rate of 20°C/min to final temperature of 270°C (1 min). All analytes were well separated within 7 min with an analysis time of 10.5 min. Calibration curves were linear over the concentration ranges of 3.125–200 μg/mL for MDMA and 6.25–200 μg/mL for MDA and MA (r > 0.990). The intra- and inter-day precisions for determining all analytes were 2.32–10.38% RSD and 1.15–9.77% RSD, respectively. The intra- and inter-day accuracies ranged from −19.79 to +17.51% DEV and −6.84 to +5.2% DEV, respectively. The lower limits of quantification (LLOQs) were 3.125 μg/mL for MDMA and 6.25 μg/mL for MDA and MA. All analytes were stable at room temperature during 24 h but significant loss occurred after 2-month storage at −20°C. The method was shown to be useful for determining the purity of MDMA in seized tablets.

Preview

Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.

References

  1. 1.
    Gahlinger, P.M., Am. Fam. Physician, 2004, vol. 69, no. 11, p. 2619.Google Scholar
  2. 2.
    National Institute on Drug Abuse. MDMA (Ecstasy). 2006; http://www.nida.nih.gov/infofacts/ecstasy.html
  3. 3.
    Kalant, H., Can. Med. Assoc. J., 2001, vol. 165, no. 7, p. 917.Google Scholar
  4. 4.
    Fleckenstein, A.E., Volz, T.J., Riddle, E.L., Gibb, J.W., and Hanson, G.R., Annu. Rev. Pharmacol. Toxicol., 2007, vol. 47, p. 681.CrossRefGoogle Scholar
  5. 5.
    Office of the Narcotics Control Board. Narcotics Act of B.E. 2522 (1979); http://www1.oncb.go.th/document/Narcotics%20Act%20B.E.2522%20p10-40.pdf
  6. 6.
    Johansen, S.S., and Jornil, J., Scand. J. Clin. Lab. Invest., 2009, vol. 69, no. 1, p. 113.CrossRefGoogle Scholar
  7. 7.
    Kolbrich, E.A., Lowe, R.H., and Huestis, M.A., Clin. Chem., 2008, vol. 54, no. 2, p. 379.CrossRefGoogle Scholar
  8. 8.
    Wu, Y.H., Lin, K.L., Chen, S.C., and Chang, Y.Z., J. Chromatogr. B. Analyt. Technol. Biomed. Life Sci., 2008, vol. 870, no. 2, p. 192.CrossRefGoogle Scholar
  9. 9.
    Brown, S.D., Rhodes, D.J., and Pritchard, B.J., Forensic Sci. Int., 2007, vol. 171, nos. 2–3, p. 142.CrossRefGoogle Scholar
  10. 10.
    Chèze, M., Deveaux, M., Martin, C., Lhermitte, M., and Pépin, G., Forensic Sci. Int., 2007, vol. 170, nos. 2–3, p. 100.CrossRefGoogle Scholar
  11. 11.
    Concheiro, M., de Castro, A., Quintela, O., Cruz, A., and López-Rivadulla, M., Forensic Sci. Int., 2007, vol. 170, nos. 2–3, p. 156.CrossRefGoogle Scholar
  12. 12.
    Concheiro, M., Simões, S.M., Quintela, O., de Castro, A., Dias, M.J., Cruz, A., and López-Rivadulla, M., Forensic Sci. Int., 2007, vol. 171, no. 1, p. 44.CrossRefGoogle Scholar
  13. 13.
    De Martinis, B.S., Barnes, A.J., Scheidweiler, K.B., and Huestis, M.A., J Chromatogr. B. Analyt. Technol. Biomed. Life Sci., 2007, vol. 852, no. 1–2, p. 450.Google Scholar
  14. 14.
    Kim, J.Y., Jung, K.S., Kim, M.K., Lee, J.I., and In, M.K., Rapid Commun. Mass Spectrom., 2007, vol. 21, no. 11, p. 1705.CrossRefGoogle Scholar
  15. 15.
    Martins, L.F., Yegles, M., Samyn, N., Ramaekers, J.G., and Wennig, R., Forensic Sci. Int., 2007, vol. 172, nos. 2–3, p. 150.CrossRefGoogle Scholar
  16. 16.
    Peters, F.T., Samyn, N., Kraemer, T., Riedel, W.J., and Maurer, H.H., Clin. Chem., 2007, vol. 53, no. 4, p. 702.CrossRefGoogle Scholar
  17. 17.
    Cheng, J.Y., Chan, M.F. Chan, T.W., and Hung, M.Y., Forensic Sci. Int., 2006, vol. 162, nos. 1–3, p. 87.CrossRefGoogle Scholar
  18. 18.
    Cheng, W.C., Yau, T.S., Wong, M.K., Chan, L.P., and Mok, V.K., Forensic Sci. Int, 2006, vol. 162, nos. 1–3, p. 95.CrossRefGoogle Scholar
  19. 19.
    Hidvégi, E., Fábián, P., Hideg, Z., and Somogyi, G., Forensic Sci. Int., 2006, vol. 161, nos. 2–3, p. 119.CrossRefGoogle Scholar
  20. 20.
    Jimenez, C., de la Torre, R., Ventura, M., Segura, J., and Ventura, R., J Chromatogr. B. Analyt. Technol. Biomed. Life Sci., 2006, vol. 843, no. 1, p. 84.CrossRefGoogle Scholar
  21. 21.
    Maresová, V., Chadt, J., and Prikryl, L., Neuro Endocrinol. Lett., 2006, vol., 27, suppl. 2, p. 121.Google Scholar
  22. 22.
    Martins, L.F., Yegles, M., Chung, H., and Wennig, R., J. Chromatogr. B. Analyt. Technol. Biomed. Life Sci., 2006, vol. 842, no. 2, p. 98.CrossRefGoogle Scholar
  23. 23.
    Rasmussen, L.B., Olsen, K.H., and Johansen, S.S., J. Chromatogr. B. Analyt. Technol. Biomed. Life Sci., 2006, vol. 842, no. 2, p. 136.CrossRefGoogle Scholar
  24. 24.
    Grob, R.L. and Barry, E.F., Modern Practice of Gas Chromatography, New Jersey: John Wiley & Sons, 2004, p. 97.CrossRefGoogle Scholar
  25. 25.
    United States Food and Drug Administration. Guidance for Industry: Bioanalytical Method Validation. 2001; http://www.fda.gov/cder/guidance/4252fnl.pdf
  26. 26.
    Mitrevski, B. and Zdravkovski, Z., Forensic Sci Int, 2005, vol. 152, nos. 2–3, p. 199.CrossRefGoogle Scholar
  27. 27.
    Kosin, P. and Klew-aom, T., Physical and chemical characterization of ecstasy tablets; http://www.dmsc.moph.go.th/webroot/drug/rd/eDrug.stm
  28. 28.
    Makino, Y., Tanaka, S., Kurobane, S., Nakauchi, M., Terasaki, T., and Ohta, S., J. of Health Science, 2003, vol. 49, no. 2, p. 129.CrossRefGoogle Scholar
  29. 29.
    Teng, S.F., Wu, S.C., Liu, C., Li, J.H., and Chien, C.S., Forensic Sci. Int., 2006, vol. 161, no. 2–3, p. 202.CrossRefGoogle Scholar

Copyright information

© Pleiades Publishing, Ltd. 2010

Authors and Affiliations

  • A. Phonchai
    • 1
  • B. Janchawee
    • 2
  • S. Prutipanlai
    • 2
  • S. Thainchaiwattana
    • 3
  1. 1.Forensic Science Program, Faculty of SciencePrince of Songkla UniversitySongkhlaThailand
  2. 2.Department of Pharmacology, Faculty of SciencePrince of Songkla UniversitySongkhlaThailand
  3. 3.Regional Forensic Science Division 4Muang, SongkhlaThailand

Personalised recommendations