Organic impurities, stable isotopes, or both

a comparison of instrumental and pattern recognition techniques for the profiling of 3,4- methylenedioxymethamphetamine

Hilary A. S. Buchanan, William J. Kerr, Wolfram Meier-Augenstein, Niamh Nic Daéid (Lead / Corresponding author)

Research output: Contribution to journalArticle

7 Citations (Scopus)

Abstract

In this study, we precisely synthesised 61 3,4- methylenedioxymethamphetamine hydrochloride (MDMA.HCl) samples. The synthetic route, reaction conditions, and batch of starting material used were carefully controlled in order to facilitate the assessment of the sample linkage abilities of: (1) GCMS organic impurity profiling using different sets of target impurities recommended from the published literature, and (2) stable isotope ratio mass spectrometry (IRMS) for dC, dN, dH, and dO-values. For GCMS analysis, we utilised the extraction parameters, instrumental conditions, and data analysis techniques recently published. In addition to this, we analysed all MDMA.HCl samples by IRMS for their C, N, H, and O isotopic composition. The resulting data sets were subjected to hierarchical cluster analysis, principal component analysis, and discriminant analysis to identify which type of measurement (i.e. GCMS, IRMS, or both), which set of target impurities for GCMS, and which data pre-treatment method offers meaningful discrimination of the samples according to batch of starting material used, synthetic route used, or both. For our data set, discriminant analysis using a combination of the IRMS data and GCMS data ('Van Deursen' impurities pre-treated with the fourth root method) provided the most accurate discrimination of the MDMA.HCl samples. Principal component analysis had the second highest success rate, and hierarchical cluster analysis had only limited success at producing meaningful discrimination of the samples into their known groupings.
Original languageEnglish
Pages (from-to)2279-2288
Number of pages10
JournalAnalytical Methods
Volume3
Issue number10
DOIs
Publication statusPublished - 1 Oct 2011

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N-Methyl-3,4-methylenedioxyamphetamine
Isotopes
Pattern recognition
Mass spectrometry
Impurities
Cluster analysis
Discriminant analysis
Principal component analysis
Parameter extraction
Chemical analysis

Keywords

  • stable isotopes, organic impurity profiling, Physical and theoretical chemistry, Engineering(all), Chemical Engineering(all), Analytical Chemistry

Cite this

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title = "Organic impurities, stable isotopes, or both: a comparison of instrumental and pattern recognition techniques for the profiling of 3,4- methylenedioxymethamphetamine",
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Organic impurities, stable isotopes, or both : a comparison of instrumental and pattern recognition techniques for the profiling of 3,4- methylenedioxymethamphetamine. / Buchanan, Hilary A. S.; Kerr, William J.; Meier-Augenstein, Wolfram; Nic Daéid, Niamh (Lead / Corresponding author).

In: Analytical Methods, Vol. 3, No. 10, 01.10.2011, p. 2279-2288.

Research output: Contribution to journalArticle

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T2 - a comparison of instrumental and pattern recognition techniques for the profiling of 3,4- methylenedioxymethamphetamine

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