Journal of Analytical Chemistry

, Volume 65, Issue 9, pp 951–959

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

DOI: 10.1134/S106193481009011X

Cite this article as:
Phonchai, A., Janchawee, B., Prutipanlai, S. et al. J Anal Chem (2010) 65: 951. doi:10.1134/S106193481009011X

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.

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

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