A kind of polyphenol diglycoside compound and its preparation method and application
A technology of diglycoside and compound, applied in the field of polyphenol diglycoside compound and preparation thereof, can solve the problem of less research on polyphenol glycoside compound, and achieve the effects of high product purity, simple operation and high extraction yield
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Embodiment 1
[0025] Example 1 Preparation of polyphenol diglycoside compound
[0026] Take 5kg of the whole plant of Chloranthus spicatus (Thunb.) Makino, dry it, crush it, soak it in methanol (40L) for 2 weeks, suspend the soaking solution in 1L distilled water after concentration (100mL), and add Butanol extraction, the n-butanol extract is concentrated to obtain the extract; use silica gel (100 mesh, 100g) to mix the sample, and carry out normal phase silica gel column chromatography separation (200-300 mesh, 1kg; silica gel column size L 500mm, ), followed by gradient elution with chloroform / methanol with a volume ratio of 9:1, 5:1, 3:1, 1:1, 1:3, 1:9, 5L each time; TLC detected fractions, and collected the elution ratio The 3:1 fractions were combined and recrystallized from methanol.
Embodiment 2
[0027] Example 2 Preparation of polyphenol diglycoside compound
[0028] Take 5kg of Zhulan whole herb, dry, crush, extract with 5L of ethanol under reflux, concentrate the extract, suspend with 1L of distilled water, extract the aqueous suspension with 1L of chloroform, and discard the chloroform layer. The aqueous layer was extracted with 1L n-butanol; the n-butanol was partially concentrated, and the sample was mixed with silica gel (100 mesh, 100 g), and separated by normal phase silica gel column chromatography (200-300 mesh, 1 kg; silica gel column size L 500mm, ), followed by gradient elution with chloroform / methanol with a volume ratio of 9:1, 5:1, 3:1, 1:1, 1:3, 1:9, 5L each time; TLC detected fractions, and collected the elution ratio The 3:1 fractions were combined and recrystallized from methanol.
Embodiment 3
[0029] Example 3 Preparation of polyphenol diglycoside compound
[0030] Take 5kg of Zhulan whole herb, pulverize it, extract with 5L of methanol / ethanol mixture, concentrate the extract, mix the sample with 100g of diatomaceous earth, heat extract with 5L of n-butanol; carry out normal phase silica gel column chromatography (200-300 mesh , 1kg; silica gel column size L 500mm, ), followed by gradient elution with chloroform / methanol mixtures with a volume ratio of 9:1, 5:1, 3:1, 1:1, 1:3, and 1:9, 5 L each time; Fractions with a separation ratio of 3:1 were combined and then recrystallized with acetone / n-hexane (volume ratio 1:1).
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Abstract
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