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Method for preparing hyperin from Dogbane leaves

A technology for the preparation of hyperin and liquid phase, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., to achieve the effects of low production cost, low energy consumption, and high extraction efficiency

Inactive Publication Date: 2013-10-09
JIANGSU PROVINCIAL HOSPITAL OF TCM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, there are many methods for separating and purifying flavonoids, mainly chromatography, but there are great differences in the types and structures of flavonoids contained in different plants, so there are differences in chemical properties, and general extraction and purification methods are used in the extraction and purification process. method, the purity of the obtained flavonoids is not high, if to reach very high purity, its separation efficiency is lower, and the cost is higher; At present, there are few reports on the method for extracting and purifying high-purity hyperin from Apocynum leaf, and The chemical composition in hemp leaves is complex, especially the properties of hyperin and isoquercitrin contained in apocynum leaves are similar, so it is very difficult to extract and separate, and the unique chemical structure type of hyperin is due to its strong activity. Very useful, so in order to make full use of Apocynum leaf resources and meet market demand, it is necessary to develop a set of preparation methods with high extraction and purification efficiency, low cost, and high purity of hyperin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (2) get the Apocynum apocynum leaf extract that step (1) obtains and add ethanol to make the concentration of ethanol reach 80%, leave standstill, precipitate, filter out solution, concentrate, obtain the alcohol precipitation solution of Apocynum apocynum leaf extract and stand-by;

[0034] (3) Get the D101 type macroporous resin column on the Apocynum leaf alcohol precipitation liquid that step (2) obtains, first wash 5 ~ 10 column volumes with water, then use 10% ethanol to elute 1 ~ 3 column volumes, and then use 60% ethanol was eluted for 3 to 5 column volumes, detected by thin-layer chromatography, and 60% ethanol was collected for elution, and the solvent was recovered under reduced pressure at 60°C, concentrated to obtain the crude extract of Apocynum apocynum leaves, and set aside;

[0035] (4) get the hyperin crude extract obtained in step (3) and extract 10 times with water-saturated n-butanol, combine the extracts, reclaim the solvent under reduced pressure, ...

Embodiment 2

[0039] (2) get the Apocynum apocynum leaf extract that step (1) obtains and add ethanol to make the concentration of ethanol reach 85%, leave standstill, precipitate, filter out solution, concentrate, obtain the alcohol precipitation solution of Apocynum apocynum leaf extract and stand-by;

[0040] (3) AB-8 type macroporous resin column on AB-8 type macroporous resin column on the Apocynum leaf alcohol precipitation liquid that step (2) obtains, first wash 5~10 column volumes with water, then use 20% ethanol to elute 1~3 column volumes, Then eluted with 55% ethanol for 3~5 column volumes, detected by thin-layer chromatography, collected 55% ethanol for elution, recovered the solvent under reduced pressure at 60°C, concentrated, and obtained the crude extract of Apocynum apocynum leaves, which was set aside;

[0041] (4) The hyperin crude extract obtained in step (3) is adjusted to pH=3 with dilute hydrochloric acid, then extracted 8 times with ethyl acetate, the extracts are co...

Embodiment 3

[0045] (2) get the Apocynum apocynum leaf extract that step (1) obtains and add ethanol to make the concentration of ethanol reach 75%, leave standstill, precipitate, filter out solution, concentrate, obtain the alcohol precipitation solution of Apocynum apocynum leaf extract and stand-by;

[0046] (3) Get the HPD100 type macroporous resin column on the Apocynum leaf alcohol precipitation liquid that step (2) obtains, first wash 5 ~ 10 column volumes with water, then use 10% ethanol to elute 1 ~ 3 column volumes, and then use Elute with 50-70% ethanol for 3-5 column volumes, detect by thin-layer chromatography, collect and elute with 60% ethanol, recover the solvent under reduced pressure at 60°C, concentrate, and obtain the crude extract of Apocynum apocynum leaves, which is set aside;

[0047] (4) Take the hyperin crude extract obtained in step (3), adjust the pH=3 with dilute hydrochloric acid, then extract 10 times with water-saturated n-butanol, combine the extracts, recov...

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Abstract

The invention discloses a method for preparing hyperin from Dogbane leaves, which comprises the following steps: firstly. determining the optimum extraction temperature, a separation material and the concentration of an eluting agent; secondly, regulating the pH value, and extracting with a solvent having high hyperin dissolving and extracting power, thus obtaining a liquid extract; thirdly, heating at 80-85 DEG C under reflux of ethanol or methanol, and extracting; and finally, standing and crystallizing at a preferable cooling temperature, thus effectively separating the hyperin and isoquercitrin which are two flavonoid glycoside components having similar properties. In the invention, the hyperin is further purified by preparing a liquid phase; and a moving phase is examined and determined by methodology, and is subjected to targeted and efficient separation and purification based on the absorption wavelength of the hyperin, thus obtaining the hyperin having purity up to 90-99%. Thehyperin conforms to the requirements for Class A active pharmaceutical ingredients.

Description

technical field [0001] The invention relates to a method for preparing raw materials from Chinese herbal medicines, in particular to a method for preparing high-purity hyperin from extracting and separating leaves of Apocynum apocynum. Background technique [0002] Apocynum leaf is the dried leaf of Apocynum apocynum, which mainly contains flavonoids, tannins, low molecular organic acids, long-chain fatty acid esters, alcohols, steroids and other ingredients. "Compendium of Materia Medica" records that it has the effects of calming palpitations, stopping dizziness, relieving asthma and relieving cough, strengthening the heart and diuresis. Modern studies have shown that apocynum leaves have various pharmacological effects such as lowering blood pressure, lowering blood fat, antidepressant, sedative, and diuretic. [0003] Hyperin (quercetin-3-O-β-D-galactopyranoside) and isoquercitrin are flavonoid glycosides in Apocynum venetifolia leaves. Modern pharmacological studies h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 刘志辉陈武贾媛夏建龙钱芳陆超
Owner JIANGSU PROVINCIAL HOSPITAL OF TCM
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