Method for preparing Buddledin A

A technique of drunken fish and volume, which is applied in the field of preparation of extracting aspicodin A from plants, and achieves the effects of low energy consumption, low pollution, and the benefit of large-scale production operations.

Inactive Publication Date: 2011-06-15
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 Buendiadine A

Method used

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  • Method for preparing Buddledin A

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Experimental program
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Effect test

Embodiment 1

[0025] Take 10Kg of Buddleia frondosa leaves, add 80L of 60% ethanol and heat to reflux once for 1 hour, take back the liquid, filter, recover the ethanol under reduced pressure and concentrate, and use ethyl acetate-water with a ratio of 10:2 The mixed solvent is subjected to 4-stage countercurrent extraction, the extracts are combined, the solvent is recovered under reduced pressure, added to a D101 macroporous adsorption resin column for adsorption, eluted with 30% ethanol, and the eluate is collected 3 times the volume of the column, and the solvent is recovered under reduced pressure. Add methanol to crystallize, separate the crystals, wash and dry to obtain 45.8 g of colorless platelets of Budhatidine A, which is detected by HPLC with a purity of 94.3%, 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 Buddleia frondosa leaves, add 120L of 80% ethanol, heat and reflux three times, 2 hours each time, combine the reflux liquid, filter, recover the ethanol under reduced pressure and concentrate, and use ethyl acetate with a ratio of 10:2- Carry out 8-stage countercurrent extraction with water mixed solvent, combine the extracts, recover the solvent under reduced pressure, add it to the D102 macroporous adsorption resin column for adsorption, elute with 50% ethanol, collect 8 times the column volume eluate, and recover the solvent under reduced pressure , adding methanol to crystallize, separating the crystals, washing and drying to obtain 51.3g of colorless platelets of Budhafedine A, which was detected by HPLC with a purity of 93.3%, 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 Buddleia frondosa leaves, add 100L of 70% ethanol, heat and reflux twice, each time for 1.5 hours, combine the reflux liquid, filter, recover the ethanol under reduced pressure and concentrate, and use ethyl acetate with a ratio of 10:2- Carry out 6-stage countercurrent extraction with water mixed solvent, combine the extracts, recover the solvent under reduced pressure, add it to the macroporous adsorption resin column for adsorption, elute with 40% ethanol, collect 5 times the column volume eluate, recover the solvent under reduced pressure, add Methanol crystallization, separation and crystallization, washing and drying yielded 46.9g of colorless platelets of Buendadin A, which was detected by HPLC with a purity of 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 method for preparing Buddledin A, which is simple and convenient in operation, low in pollution and low in energy consumption. The method for preparing the Buddledin A comprises the following technological steps of: adding 60 to 80 percent ethanol into Buddleja davidii franch. leaf to perform reflux under heating; merging the reflux solution; filtering; recovering ethanol under reduced pressure and concentrating; performing multi-level countercurrent extraction by using an ethyl acetate-water mixed solvent according to the ratio of ethyl acetate to water of 10:2; merging extract liquid; recovering the solvent under reduced pressure; adding on a macroporous absorption resin column to perform absorption; performing elution by using ethanol; collecting eluent; recovering the solvent under reduced pressure; adding methanol to crystallize; performing fractional crystallization; and washing and drying to obtain the Buddledin A. The Buddledin A prepared by the method has high purity and realizes industrialized amplification easily.

Description

technical field [0001] The present invention relates to a preparation method of Budyudine A, in particular to a preparation method of extracting Budyudine A from plants. Background technique [0002] Buddledin A (Buddledin A), molecular formula: C 17 h 24 o 3 , molecular weight: 276.375, CAS accession number: 62346-20-7. It mainly exists in various plants of the Buddlejaceae family, among which Buddleja davidii Franch. has a higher content in the leaves of the Buddlejaceae plant, and the source of raw materials is abundant. Its molecular formula is as follows: [0003] [0004] Modern studies have shown that Buendardin A has antifungal and fish poisoning activities, and it is also used as a raw material for the synthesis of other active derivatives. [0005] The leaves of Buddleja davidii Franch., a plant of Buddlejaceae, are used as traditional Chinese medicine wine medicinal flowers, which have the functions of dispelling wind and cold, promoting blood circulation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/52C07C69/03
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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