Combined Ultrahigh Pressure Extraction and High-Speed Counter-Current Chromatography for Separation and Purification of Three Glycoside Compounds from Dendrobium officinale Protocorm |
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Authors: | Wei Zhang Yingjie Zhang Jinying Wang Wenjuan Duan Feng Liu |
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Institution: | 1.School of Pharmaceutical Sciences, Shandong Academy of Sciences, Qilu University of Technology, Jinan 250014, China; (W.Z.); (J.W.); (W.D.);2.Shandong Analysis and Test Center, Key Laboratory for Applied Technology of Sophisticated Analytical Instruments of Shandong Province, Shandong Academy of Sciences, Qilu University of Technology, Jinan 250014, China; |
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Abstract: | As an alternative to Dendrobium candidum, protocorm-like bodies (PLBs) of Dendrobium candidum are of great value due to their high yield and low cost. In this work, three glycoside compounds, β-D-glucopyranose 1-(E)-3-(4-hydroxyphenyl)-2-propenoat] (I), β-D-glucopyranose 1-(E)-3-(3, 4-dihydroxyphenyl)-2-propenoat] (II), and 1-O-sinapoyl glucopyranoside (III), were extracted and isolated by ultrahigh pressure extraction (UPE) coupled with high-speed counter-current chromatography (HSCCC) from PLBs of D. officinale. First, the target compounds were optimized and prepared with 50% ethanol solution at a 1:30 (g/mL) solid/liquid ratio in 2 min under 300 MPa by UPE. Then, the crude extract was chromatographed with a silica gel column, and primary separation products were obtained. In addition, the products (150 mg) were separated by HSCCC under the solvent system of MTBE-n-butyl alcohol-acetonitrile-water (5:1:2:6, v/v/v/v), yielding 31.43 mg of compound I, 10.21 mg of compound II, and 24.75 mg of compound III. Their structures were further identified by ESI-MS, 1H NMR, and 13C NMR. The antioxidant results showed that the three compounds expressed moderate effects on the DPPH· scavenging effect. Compound II had the best antioxidant capacity and its IC50 value was 0.0497 mg/mL. |
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Keywords: | ultrahigh pressure extraction (UPE) high-speed counter-current chromatography (HSCCC) PLBs of D officinale glycoside compounds |
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