Rapid assessment of the illegal presence of 1,3-dimethylamylamine (DMAA) in sports nutrition and dietary supplements using 1H NMR spectroscopy
Deutscher übersetzter Titel: | Schnelle Feststellung des illegalen Vorliegens von 1,3-Dimethylamylamin (DMAA) in Sporternährung und Nahrungsergänzungsmitteln durch 1H-NMR-Spektroskopie |
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Autor: | Monakhova, Yulia B.; Ilse, Maren; Hengen, Julia; el-Atma, Oliver; Kuballa, Thomas; Kohl-Himmelseher, Matthias; Lachenmeier, Dirk W. |
Erschienen in: | Drug testing and analysis |
Veröffentlicht: | 6 (2014), 9/10, S. 944-948, Lit. |
Format: | Literatur (SPOLIT) |
Publikationstyp: | Zeitschriftenartikel |
Medienart: | Gedruckte Ressource Elektronische Ressource (online) |
Sprache: | Englisch |
ISSN: | 1942-7603, 1942-7611 |
DOI: | 10.1002/dta.1677 |
Schlagworte: | |
Online Zugang: | |
Erfassungsnummer: | PU201503002071 |
Quelle: | BISp |
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. Verf.-Referat