The prevalence of poor-quality dietary supplements worldwide makes determining the composition of active ingredients in marketed dietary supplements a shared interest between marketers, consumers, and researchers alike. Effective techniques are necessary for this type of quality control. Herein, we hypothesize that high-field NMR spectroscopy and positive mode electrospray ionization mass spectrometry (ESI+ MS) can be used to identify biologically active molecules in two commercially-available Epimedium grandiflorum dietary supplements. To guide this analysis, nine prenyl flavonoid glycosides were chosen as standards: baohuoside I, baohuoside V, epimedin A, epimedin A1, epimedin B, epimedin C, icariin, icariside I, and 2”-O-rhamnosylicariside II. Using 1D 1H NMR in tandem with homonuclear correlation spectroscopy (COSY) and ESI+ MS, the identities of the tested standards and the qualitative profiles of the supplements were determined. From here, baohuoside I, icariside I, 2”-O-rhamnosylicariside II, icariin, and epimedin C were observed in one of the tested supplements. The same compounds, in addition to epimedin B and epimedin A1, were identified in the second tested supplement. An unexpected compound, magnoflorine, was also observed in both supplements. These findings support NMR spectroscopy and ESI+ MS as promising tools for the quality control of complex supplements, such as commercial E. grandiflorum. However, further investigation is necessary to refine their usage as quantitative analytical methods.

High-field NMR spectroscopy and mass spectrometry for the quality control of Epimedium grandiflorum dietary supplements

2019 Spring National Meeting

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