Separation of Dihydro-Isocoumarins and Dihydro-Stilbenoids from Hydrangea macrophylla ssp. serrata by Use of Counter-Current Chromatography |
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Authors: | Johannes Wellmann Beate Hartmann Esther-Corinna Schwarze Silke Hillebrand Stephan I. Brueckner Jakob Ley Gerold Jerz Peter Winterhalter |
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Affiliation: | 1.Institute of Food Chemistry, Technische Universität Braunschweig, Schleinitzstraße 20, 38106 Braunschweig, Germany; (G.J.); (P.W.);2.Symrise AG, Mühlenfeldstraße 1, 37603 Holzminden, Germany; (B.H.); (E.-C.S.); (S.H.); (S.I.B.); (J.L.) |
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Abstract: | Previously, different Hydrangea macrophylla ssp. serrata cultivars were investigated by untargeted LC-MS analysis. From this, a list of tentatively identified and unknown compounds that differ significantly between these cultivars was obtained. Due to the lack of reference compounds, especially for dihydro-isocoumarins, we aimed to isolate and structurally characterise these compounds from the cultivar ‘Yae-no-amacha’ using NMR and LC-MS methods. For purification and isolation, counter-current chromatography was used in combination with reversed-phase preparative HPLC as an orthogonal and enhanced purification workflow. Thirteen dihydro-isocoumarins in combination with other metabolites could be isolated and structurally identified. Particularly interesting was the clarification of dihydrostilbenoid glycosides, which were described for the first time in H. macrophylla ssp. serrata. These results will help us in further studies on the biological interpretation of our data. |
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Keywords: | Hydrangea macrophylla ssp. serrata dihydro-isocoumarins dihydro-stilbenoids cyanogenic glycosides flavonols secoriridoids counter-current chromatography liquid chromatography ion-mobility high-resolution mass spectrometry nuclear magnetic resonance spectroscopy |
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