Preparation method of astilbin

A technology for astilbin and extraction is applied in the field of preparation of astilbin to achieve the effects of being beneficial to large-scale production operations, with less pollution and less energy consumption

Inactive Publication Date: 2011-04-20
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, there is no report on the preparation process sui

Method used

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  • Preparation method of astilbin

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Effect test

Embodiment 1

[0025] Take 10Kg of grape pomace (containing pericarp and seeds), add 30L of 70% ethanol and put it into a microwave extraction device for microwave extraction. The extraction power is 300W, extract once for 5 minutes, collect the extract, filter, recover the ethanol under reduced pressure and concentrate , to obtain the extract, carry out 3-stage countercurrent extraction with a mixed solvent of ethyl acetate-water with a ratio of 8:1, the volume ratio of the extract to the total amount of the mixed solvent is 1:3, combine the extract, recover the solvent under reduced pressure, add Adsorbed with H-50 macroporous adsorption resin, eluted with 50% ethanol, collected 3 times the column volume eluate, recovered the solvent under reduced pressure and concentrated, added ethanol to crystallize, separated cleanly, washed and dried to obtain yellow needle crystals- Astilbin 16.8g, detected by HPLC, the purity is 95.3%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical pro...

Embodiment 2

[0027] Take 10Kg of grape pomace (containing pericarp and seeds), add 60L of 90% ethanol and put it into a microwave extraction device for microwave extraction, extraction power 600W, extraction 3 times, 10 minutes each time, collect the extract, filter, and recover ethanol under reduced pressure and concentrated to obtain an extract, which is subjected to 6-stage countercurrent extraction with a mixed solvent of ethyl acetate-water in a ratio of 8:1, the volume ratio of the extract to the total amount of mixed solvent is 1:6, the extracts are combined, and the solvent is recovered under reduced pressure , add CD-180 type macroporous adsorption resin for adsorption, elute with 70% ethanol, collect 8 times the column volume eluate, recover the solvent under reduced pressure and concentrate, add ethanol to crystallize, separate and clean, wash and dry to obtain yellow needles Crystal-astilbin 14.7g, detected by HPLC, the purity is 96.1%, UV, IR, MS, 2 HNMR, 13 The data characte...

Embodiment 3

[0029] Take 10Kg of grape pomace (containing pericarp and seeds), add 50L of 80% ethanol and put it into a microwave extraction device for microwave extraction, extraction power 500W, extraction 2 times, 8 minutes each time, collect the extract, filter, and recover ethanol under reduced pressure and concentrated to obtain an extract, which was subjected to 4-stage countercurrent extraction with a mixed solvent of ethyl acetate-water in a ratio of 8:1, the volume ratio of the extract to the total amount of the mixed solvent was 1:4, the extracts were combined, and the solvent was recovered under reduced pressure , add D101 type macroporous adsorption resin for adsorption, elute with 60% ethanol, collect 5 times the column volume eluate, recover the solvent under reduced pressure and concentrate, add ethanol to crystallize, separate and clean, wash and dry to obtain yellow needle crystals- Astilbin 17.3g, detected by HPLC, the purity is 98.1%, UV, IR, MS, 2 HNMR, 13 The data ch...

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Abstract

The invention relates to a preparation method of astilbin with simple and convenient operation, little pollution and less energy consumption. The process comprises the following steps of: taking trester, adding ethanol to a microwave extraction device and carrying out microwave extraction, collecting extraction liquid, filtering, decompressing, recycling and concentrating ethanol to obtain an extract; carrying out counter-current extraction on a mixed solution of ethyl acetate and water in a ratio of 8 to 1, mixing the extraction liquid, decompressing and recycling the solvent; adding macroporous adsorptive resin for adsorption, eluting with the ethanol, collecting 3-8 times by measuring pin volume of eluent, decompressing, recycling and concentrating the solvent; and adding ethanol for crystallization, cleanly separating, washing and drying. The method of the invention is adopted for preparing astilbin with high product purity and is easy to realize industrial amplification.

Description

technical field [0001] The invention relates to a preparation method of astilbin, in particular to a preparation method of extracting astilbin from plants. Background technique [0002] Astilbin (Astilbin), molecular formula: C 21 h 22 o 11 , molecular weight: 450.398, CAS accession number: 29838-67-3. It exists in various plants of Garciniaceae, Hypericaceae, Walnut, Liliaceae, Morushiaceae, Saxifragaceae, and Grapeaceae, among which the content of grape Vitis vinifera L. is relatively high, and its The sources are plentiful. Its molecular formula is as follows: [0003] [0004] Modern studies have shown that astilbin has various activities such as anti-oxidation, anti-inflammation, inhibition of melanoma, and liver protection, and it is also used as a raw material for the synthesis of other active derivatives. [0005] In the prior art, there is no report on a preparation process suitable for the industrialized mass production of high-purity astilbin. Contents ...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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