2D and 3D DOSY 1H NMR, a useful tool for analysis of complex mixtures: application to herbal drugs or dietary supplements for erectile dysfunction.

Stéphane Balayssac (1) , Saleh Trefi (1) , Véronique Gilard (1) , Myriam Malet-Martino (1) , Robert Martino (1) , Marc-André Delsuc (2)

1 SPCMIB - Synthèse et Physico-Chimie de Molécules d'Intérêt Biologique
2 IGBMC - Institut de Génétique et de Biologie Moléculaire et Cellulaire

Seventeen herbal dietary supplements, marketed as natural substances for the enhancement of sexual function, were analyzed by diffusion ordered spectroscopy (DOSY) (1)H NMR. The method allowed a global analysis of the samples with detection of both active and inactive ingredients present in these complex matrixes. Eight formulations contained compounds related to the synthetic phosphodiesterase-5 inhibitors. Sildenafil, tadalafil, vardenafil, hydroxyhomosildenafil, thiosildenafil, and the newly identified adulterant thiomethisosildenafil were detected. Quantification of these active ingredients was carried out by HPLC or NMR. In addition to these actives, about 30 compounds or excipients were characterized. This study ended up with a three-dimensional DOSY-COSY (1)H NMR experiment on a herbal formulation which provided both virtual separation and structural information.

Stéphane Balayssac, Saleh Trefi, Véronique Gilard, Myriam Malet-Martino, Robert Martino, et al.. 2D and 3D DOSY 1H NMR, a useful tool for analysis of complex mixtures: application to herbal drugs or dietary supplements for erectile dysfunction.. Journal of Pharmaceutical and Biomedical Analysis, 2009, 50 (4), pp.602-12. ⟨10.1016/j.jpba.2008.10.034⟩. ⟨inserm-00420792⟩