Journal Highlight: Rapid assessment of the illegal presence of 1,3-dimethylamylamine (DMAA) in sports nutrition and dietary supplements using 1H NMR spectroscopy

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  • Published: Oct 6, 2014
  • Author: spectroscopyNOW
  • Channels: NMR Knowledge Base
thumbnail image: Journal Highlight: Rapid assessment of the illegal presence of 1,3-dimethylamylamine (DMAA) in sports nutrition and dietary supplements using <sup>1</sup>H NMR spectroscopy
A proton NMR method was developed and validated for measuring 1,3-dimethylamylamine in sports nutrition and dietary supplements and is recommended for routine use in food testing, customs or doping control laboratories.



Rapid assessment of the illegal presence of 1,3-dimethylamylamine (DMAA) in sports nutrition and dietary supplements using 1H NMR spectroscopy

Drug Testing and Analysis, 2014, 6, 944-948
Yulia B. Monakhova, Maren Ilse, Julia Hengen, Oliver el-Atma, Thomas Kuballa, Matthias Kohl-Himmelseher and Dirk W. Lachenmeier

Abstract: 1,3-Dimethylamylamine (DMAA) is a stimulant that can be found in pre-workout sports nutrition and dietary supplements. This practice is illegal because DMAA is not a safe food ingredient but rather an unapproved medicinal compound due to its pharmacological action. In order to determine the DMAA content in such products, a nuclear magnetic resonance (NMR) spectroscopic method was developed and validated (DMAA was quantified as DMAA-HCl). For quantification, the collective integral from two of the methyl groups of the molecule in the range δ 0.92–0.84 ppm was used. The method was linear over the examined range of 1–21 g/kg (R2 = 0.9937). The recoveries from spiked concentrations (0.1–6 g/kg) ranged between 85% and 105% (96% on average), with a relative standard deviation (RSD) of 1% for an authentic sample. The detection limit was 0.03 g/kg and the quantification limit was 0.08 g/kg (calculated for 75 mg sample weight). The actual DMAA-HCl content in the sample was quantified using calibration curves (external standardization) or 3,5-dinitrobenzoic acid as single-point internal standard. The developed NMR methodology was applied for the analysis of 16 products, from which 9 samples were found positive (the DMAA-HCl concentration varied between 3.1 g/kg and 415 g/kg). The method can be recommended for routine use in food testing, customs or doping control laboratories.

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