NMR test for illegal ingredient DMAA in sports supplements

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  • Published: Jun 20, 2014
  • Author: Steve Down
  • Channels: UV/Vis Spectroscopy / Base Peak / Raman / MRI Spectroscopy / Chemometrics & Informatics / X-ray Spectrometry / Atomic / NMR Knowledge Base / Proteomics / Infrared Spectroscopy

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The illegal supplement 1,3-dimethylamylamine (DMAA) has been at the centre of attention recently as it was banned by the World Anti-Doping Agency and also by European and US food regulatory authorities. The problem from the WADA point of view is its performance-enhancing ability whereas it remains an unapproved food additive and medicinal product.

The persistent drug community have been getting around the ban by selling natural supplements that contain geranium, which is alleged to contain natural DMAA but this is a hotly disputed assertion. Several groups of analytical scientists have found no evidence of DMAA in the plants and claim that the synthetic form must have been added to the supplements.

Mass spectrometry has been one of the key techniques in the search for DMAA but research groups in Germany have recently shown that NMR is also a viable detection technique. Writing in Drug Testing and Analysis, they showed that proton NMR can be used to detect DMAA down to 0.03 g/kg, using the protons within the two methyl groups.

This lower limit is actually higher than that achieved by LC/MS methods but the research team pointed put that it is sufficiently low for pharmacologically relevant studies. Where it gains over both LC/MS and GC/MS is the speed of analysis, partly due to the reduced time spent on sample preparation.

They illustrated the technique by looking for DMAA in 16 sports and dietary supplements of various origins that had been submitted to their lab, a state control facility, for official control purposes. The greatest amounts were found in three products seized at customs points (136-415 g/kg) which did not have labelling information. Of the six remaining positive samples, five had declared DMAA on the label but all contained the chemical at 3.1-3.5 g/kg DMAA.

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