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Preparation method for frangulin B

A technology for extracting rhamnoside, which is applied in the field of preparation of extracting rhamnoside B from plants, achieves the effects of low energy consumption, low pollution, and favorable large-scale production operations

Inactive Publication Date: 2011-11-23
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-purity rhamnoside B

Method used

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  • Preparation method for frangulin B

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Experimental program
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Effect test

Embodiment 1

[0025] Take 10Kg of buckthorn bark, crush it, add 80L of ethanol with a concentration of 50%, put it into a microwave extraction device for microwave extraction, extraction power 300W, extract once, 3 minutes, combine the extracts, filter, and recover ethanol under reduced pressure And concentrated, carried out 6-stage countercurrent extraction with ethyl acetate-water mixed solvent with a ratio of 3:1, combined the ethyl acetate layer, recovered ethanol under reduced pressure and concentrated, adsorbed by AB-8 type macroporous adsorption resin, 70% ethanol For elution, collect 3 times the column volume eluate, recover ethanol under reduced pressure and concentrate, add acetone to crystallize, separate the crystals, wash and dry to obtain 11.3g of rhamnoside B, which is detected by HPLC with a purity of 95.0% , UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 2

[0027] Take 10Kg of buckthorn bark, crush it, add 120L of ethanol with a concentration of 70%, put it into a microwave extraction device for microwave extraction, extraction power 600W, extract 3 times, each time for 10 minutes, combine the extracts, filter, and decompress Recover ethanol and concentrate, carry out 8-stage countercurrent extraction with ethyl acetate-water mixed solvent with a ratio of 3:1, combine the ethyl acetate layers, recover ethanol under reduced pressure and concentrate, and absorb through HPD-700 macroporous adsorption resin, 80 % ethanol for elution, collect 8 times the amount of column volume eluent, recover ethanol under reduced pressure and concentrate, add acetone to crystallize, separate crystals, wash and dry to obtain 13.3g of Eckhamnosin B, which is detected by HPLC and has a purity of 94.2%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 3

[0029] Take 10Kg of buckthorn bark, crush it, add 100L of ethanol with a concentration of 60%, put it into a microwave extraction device for microwave extraction, extraction power is 500W, extract twice, each time for 8 minutes, combine the extracts, filter, and decompress Recover ethanol and concentrate, carry out 7-stage countercurrent extraction with ethyl acetate-water mixed solvent with a ratio of 3:1, combine the ethyl acetate layers, recover ethanol under reduced pressure and concentrate, and adsorb through H-50 macroporous adsorption resin, 75 % ethanol for elution, collect 5 times the amount of column volume eluate, recover ethanol under reduced pressure and concentrate, add acetone to crystallize, separate crystals, wash and dry to obtain 12.9g of rhamnoside B, detected by HPLC, the purity is 98.3%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

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Abstract

The invention relates to a preparation method for frangulin B, which has the advantages of simple operation, little pollution and low energy consumption. The preparation method comprises the following steps of taking bark of rhamnus frangula for crushing, adding ethanol, putting the mixture into a microwave extracting apparatus for microwave extraction, merging extracts, carrying out filtration, recovering ethanol through pressure reduction, carrying out condensation, carrying out six to eight-stage countercurrent extraction with a mixed solvent of ethyl acetate and water at a ratio of 3:1, merging layers of ethyl acetate, recovering ethanol through pressure reduction, carrying out condensation, carrying out adsorption with macroporous adsorption resin, eluting ethanol, adding acetone for crystallization, separating crystals, and rinsing and drying the crystals so as to obtain frangulin B. The frangulin B prepared in the invention has high purity, and industrial amplification of the method provided in the invention is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of rhamnosin B, in particular to a preparation method of extracting rhamnosin B from plants. Background technique [0002] Rhamnoside B (Frangulin B), molecular formula: C 20 h 18 o 9 , molecular weight: 402.357, CAS accession number: 14101-04-3, mainly exists in various plants of Rhamnaceae. Among them, the Rhamnaceae plant Rhamna Rhamnus frangula The bark of L. is abundant, and its molecular formula is as follows. [0003] [0004] Modern studies have shown that rhamnoside B has anti-tumor and anti-platelet aggregation effects, and it is also used as a raw material for the synthesis of other active derivatives. [0005] Rhamna Rhamnus frangula The bark of L. is used as a green material in traditional Chinese medicine, which can relieve constipation. [0006] In the prior art, there is no report on a preparation process suitable for the industrialized large-scale production of high-purity rhamn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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