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A method for simultaneously preparing 7-hydroxyl-4'-methoxyflavan and pterostylbene

A technology of methoxyflavan and pterostilbene, which is applied in the field of simultaneous preparation of 7-hydroxy-4'-methoxyflavan and pterostilbene, achieving the effect of a good material basis

Active Publication Date: 2016-08-31
GUILIN SANJIN PHARMACEUTICALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no method for simultaneously purifying and preparing 7-hydroxy-4'-methoxyflavan and pterostylbene in the prior art. In view of this, the present invention is proposed

Method used

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  • A method for simultaneously preparing 7-hydroxyl-4'-methoxyflavan and pterostylbene
  • A method for simultaneously preparing 7-hydroxyl-4'-methoxyflavan and pterostylbene
  • A method for simultaneously preparing 7-hydroxyl-4'-methoxyflavan and pterostylbene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Get 0.5kg of the resinous wood of Dracaena phoenix leaf, grind it, add 6 times the amount of petroleum ether to extract for 2 days, filter, and use 8 times the amount of chloroform to reflux extract the filter residue for 3 times, recycle the chloroform to obtain the chloroform extract, use 60 Dissolve in % methanol, pass through macroporous resin column chromatography, elute with 60% methanol, each 250ml is a fraction, check and combine by TLC, combine 2-8 fractions, concentrate to dryness, dissolve in 50% methanol, use reversed phase silica gel ( RP-C18) column chromatography, eluting with 50% methanol, each fraction was 100ml, and combined by TLC, 14-18 fractions were combined, concentrated to dryness, methanol-water recrystallization, and 0.54 g of white needle crystals were obtained. It was identified as 7-hydroxy-4'-methoxyflavane (7-hydroxy-4'methoxy-flavane) by spectrum technique, mp: 134-135°C, HPLC98.4%. Fractions 20-27 were combined, concentrated to dryness, ...

Embodiment 2

[0081] 1. The preparation of Dracaena ethanol extract:

[0082] Take Dracaena glabrata, crush it, add ethanol to reflux for extraction twice, filter, recover ethanol, and dry it to obtain the ethanol extract of Dracaena glabrata.

[0083] 2. Separation and purification:

[0084] 1) Take 0.5 kg of ethanol extract of Dracaena glabrata, grind it, add 4 times of petroleum ether to extract for 3 days, filter, and filter the residue for later use;

[0085] 2) The resulting filter residue was refluxed with 10 times the amount of chloroform to extract 3 times, each time for 30 minutes, and the chloroform was recovered to obtain the chloroform extract;

[0086] 3) Dissolve the obtained chloroform extract in 60% methanol, perform macroporous resin column chromatography, and elute with 60% methanol, each 250ml is a fraction, TLC inspection and combination, and 2-8 fractions are combined;

[0087] 4) Concentrate the combined 2-8 fractions to dryness, dissolve with 50% methanol, and use ...

Embodiment 3

[0092] 1. The preparation of Dracaena ethanol extract:

[0093] Take Dracaena glabrata, crush it, add ethanol to reflux for extraction twice, filter, recover ethanol, and dry it to obtain the ethanol extract of Dracaena glabrata.

[0094] 2. Separation and purification:

[0095] 1) Take 0.5kg of the ethanol extract of Dracaena glabrata, grind it, add 8 times petroleum ether to extract for 1 day, filter, and filter the residue for later use;

[0096] 2) The resulting filter residue was refluxed and extracted 3 times with 6 times the amount of chloroform, each time for 30 minutes, and the chloroform was recovered to obtain the chloroform extract;

[0097] 3) Dissolve the obtained chloroform extract in 60% methanol, perform macroporous resin column chromatography, and elute with 60% methanol, each 250ml is a fraction, TLC inspection and combination, and 2-8 fractions are combined;

[0098] 4) Concentrate the combined 2-8 fractions to dryness, dissolve with 50% methanol, and use...

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Abstract

The invention belongs to the field of extraction of traditional Chinese medicines, and in particular relates to a method for simultaneous preparation of 7-hydroxy-4 '-methoxy flavan and pterostilbene. The method includes the steps of: 1) taking dracaena cochinchinensis grease-containing wood or ethanol extract thereof, grinding, adding petroleum ether to extract, filtering to obtain filter residue for standby use; 2) using chloroform for reflux extraction of the obtained filter residue, and recovering the chloroform to obtain chloroform extract; 3) using methanol to dissolve the obtained chloroform extract, performing column chromatography, eluting with methanol with every 250ml being one flow part, and merging 2-8 flow parts; 4) concentrating the merged 2-8 flow parts to dry, dissolving with methanol, using a reverse phase silica gel column for column chromatography, eluting with methanol with every 100ml being one flow part, and respectively merging 14-18 flow parts and 20-27 flow parts; and 5) concentrating the respectively merged 14-18 flow parts and 20-27 flow parts to dry, and respectively recrystallizing to obtain the two compounds of 7-hydroxy-4'-methoxy flavan and pterostilbene. The two compounds of 7-hydroxy-4 '-methoxy flavan and pterostilbene are firstly and simultaneously prepared from dracaena cochinchinensis by the method.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine extraction, and in particular relates to a method for simultaneously preparing 7-hydroxy-4'-methoxyflavan and pterostylbene. Background technique [0002] Dracaena cochinchinensis (Lour.) S.C.Chen] is a plant of the genus Dracaena in the family Liliaceae. The ethanol extract of its lipid-containing wood is called Guangxi blood dragon. It is a new class of traditional Chinese medicine approved by the Ministry of Health. Blood stasis, analgesic pain relief, astringent sores and muscle growth, etc. It is used for bruises, blood stasis pain, stagnation of Qi and blood in women, traumatic bleeding, and abscesses that persist for a long time. [0003] Research on its chemical constituents, "Chemical Constituents and Antifungal Activity of Rhizoma Rhizoma Yunnan" [Wang Jinliang, Li Xingcong, Jiang Dongfu, et al. Chemical constituents and antifungal activities of Rhizoma Rhizoma Yunnan. Yunnan ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/32C07D311/40C07C43/23C07C41/34
CPCC07C41/34C07D311/60C07C43/23
Inventor 邹节明周艳林
Owner GUILIN SANJIN PHARMACEUTICALS CO LTD
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