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Method for preparing compound Phellibamin D from phellinus igniarius medicinal material

A technology for compounds and medicinal materials, applied in the direction of organic chemistry, etc., can solve the problem of unclear spectrum-effect relationship, achieve good enrichment effect, recyclable solvent, and meet the effect of large-scale production

Pending Publication Date: 2022-06-03
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The compound Phellibaumin D is rarely reported, there is no relevant pharmacological activity literature report, and the spectrum-effect relationship is not clear. Therefore, the preparation of this compound is of great significance for the basic research of Phellinus Phellinus and pharmacological activity research;

Method used

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  • Method for preparing compound Phellibamin D from phellinus igniarius medicinal material
  • Method for preparing compound Phellibamin D from phellinus igniarius medicinal material
  • Method for preparing compound Phellibamin D from phellinus igniarius medicinal material

Examples

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Embodiment 1

[0031] Weigh 100 g of Phellinus linteus medicinal materials, add 3L of 70% ethanol aqueous solution, soak for 24 hours; then heat and boil for 8 hours, collect the alcohol extract, and then add 3L of aqueous solution to the solid material and repeat adding water and boiling to collect the alcohol extract to obtain Phellinus linteus The medicinal material alcohol-extracted solution is filtered through a ceramic membrane membrane, the pore size of the ceramic membrane membrane core is 100 nm, and the permeate is concentrated to 20 mg / mL to obtain a ceramic membrane permeation concentrate.

[0032] One-dimensional preparation conditions, chromatographic conditions use C18YE packing (preparative column size: 100 × 250 mm, particle size 30 μm, pore size Mass 1200g, Huapu Xinchuang Technology Co., Ltd.), mobile phase adopts (A) methanol (organic phase)-(B) 0.1% formic acid water (aqueous phase, v / v), gradient elution mode: methanol (mobile phase A) ) The volume concentration was in...

Embodiment 2

[0035] Weigh 100 g of Phellinus linteus, add 2L of 50% ethanol aqueous solution, soak for 36 hours; then heat and boil for 6 hours, collect the alcohol extract, add 2L of 50% ethanol aqueous solution to the solid material again, boil and extract to collect the alcohol extract, and combine to obtain alcohol Extract the liquid, filter it with a ceramic membrane, the pore size of the ceramic membrane core is 100 nm, and the permeate is concentrated to 30 mg / mL.

[0036] One-dimensional preparation conditions, chromatographic conditions use pure water-resistant C18YE silica gel packing (preparative column specifications: 100 × 250 mm, particle size 60 μm, pore size Mass 1200g, Huapu Xinchuang Technology Co., Ltd.), mobile phase adopts (A) ethanol (organic phase)-(B) 0.1% oxalic acid water (aqueous phase, v / v), step isocratic elution method: pure water washing Remove for 20min, ethanol (mobile phase A) volume concentration 55% isocratic (the rest are mobile phase B) elution for 60mi...

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Abstract

The invention provides a method for preparing a compound Phellibaumin D from a phellinus igniarius medicinal material. The method comprises the following steps: extracting the phellinus igniarius medicinal material with ethanol water, performing one-dimensional enrichment by utilizing a pure water-resistant C18YE silica gel filler by adopting a preparative chromatography two-dimensional orthogonal technology to obtain a crude product of the compound Phellibaumin D, and performing preparation purification by utilizing a high-density bonded C18TDE silica gel filler to obtain a purity gt; and 90% of a compound Phellibamin D. The invention also discloses a preparation method of the compound. The method has the advantages of good repeatability in the preparation process, recyclable solvent, high yield, high automation degree and easiness in operation, and can meet the requirements of large-scale production.

Description

technical field [0001] The method relates to the technical field of separation and purification, in particular to a method for preparing the compound Phellibaumin D from Phellinus linteus. Further, the present invention is a method for preparing high-purity compound Phellibaumin D from Phellinus linteus medicinal materials by using two-dimensional liquid chromatography technology, and the purity can reach more than 90%. Background technique [0002] Phellinus linteus is a precious perennial large medicinal fungus, known as "forest gold", which is recorded in "Compendium of Materia Medica". It belongs to the Basidiomycota Laminaria, Non-Pillaceae, Polyporaceae, and there are forty species distributed in my country. It is mainly parasitic on the trunks of mulberry, willow, birch and poplar, among which the wild mulberry Phellinus is the most precious. [0003] Phellinus linteus, as a traditional fungal Chinese medicine in my country, is currently internationally recognized a...

Claims

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Application Information

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IPC IPC(8): C07D309/36
CPCC07D309/36
Inventor 丰加涛梁鑫淼钟正升
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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