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High purity cortex fraxini and its preparation method

A technology of quincetin and extracting solution, which is applied in the field of high-purity quincetin and its preparation, can solve the problems of liver damage, troublesome operation, environmental pollution and the like, and achieves the effects of avoiding injury, simple operation and high purity

Active Publication Date: 2011-08-03
SHANGHAI SINE PHARMA LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, 95% ethanol and ethyl acetate are used, the cost is high, and the extraction process is easy to emulsify, and the operation is troublesome
Moreover, there are great difficulties in the concentration step, because the solution volume is too small, the viscosity is too high, and it is difficult to separate crystals
In addition, and containing a large amount of feudaletine in the obtained feudaletine crystal, the purity is not ideal
[0004] In addition, in the existing method of extracting teretin, ethyl acetate is usually used for extraction. If the operator is exposed to ethyl acetate for a long time in the work project, it will cause harm to the human body, such as liver damage, etc., and will also affect the human body. environmental pollution

Method used

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preparation example Construction

[0011] The present invention provides a method for preparing zinpyridone, which comprises the steps of extracting zinpyridin from zinpi, separating, concentrating and crystallization, wherein the separation step is the following column chromatography step:

[0012] a) The extract obtained in the centrifugation or filtration extraction step, the filtrate or the supernatant is directly added to the macroporous adsorption resin column, wherein the weight-to-volume ratio of the raw material and the resin is 1:2 to 1:3; b) all the extracts to be extracted After passing through the resin column, eluate with eluent. After the eluent is clarified, start to collect the eluent, and stop collecting the eluent until 10-15 times the column volume is collected.

[0013] In the method of the present invention, the extraction step is conventional in the art. For example, the specific process of the extraction step can be carried out as follows:

[0014] 1) Crush the traditional Chinese medic...

Embodiment 1

[0028] Add 10 liters of water to 1 kg of Qinpi coarse powder (origin: Gansu) (20 mesh), and heat under reflux for extraction for 1 hour. The residue was then extracted twice with water, 8 liters of water was added each time, and the reflux time was 1 hour. The extracts were combined, and the resulting extract was directly added to a 1kg 2000ml AB-8 resin column (Tianjin Nankai University Chemical Factory, styrene type), and the sample was loaded at 3 column volumes per hour. After the sample was loaded, eluate with 30 liters of water, and after the eluate was clarified, start to collect the eluate until 20 liters of the eluate was collected. The collected 20 liters of eluate were concentrated to 1 liter and placed in the refrigerator overnight. The next day, the refrigerated concentrate was filtered and the filter cake was washed with a small amount of water. Then, the filter cake was dissolved by heating with 1 liter of water, and the resulting solution was placed in a refr...

Embodiment 2

[0030] Add 10 liters of water to 1 kg of Qinpi coarse powder (origin: Gansu) (20 mesh), and heat and reflux for extraction for 1.5 hours. The residue was then extracted with water for three times, 8 liters of water was added each time, and the reflux time was 1 hour. The extracts were combined, and the resulting extract was directly added to 3000 ml of Diaion HP-20 resin (produced by Mitsubishi Corporation, styrene type), and the sample was loaded at 3 column volumes per hour. After the sample was loaded, eluate with 60 liters of water. After the eluate was clear, the eluate was collected until 40 liters of the eluate was collected. The collected 40 liters of eluate were concentrated to 1 liter and the concentrate was placed in the refrigerator overnight. The next day, the refrigerated concentrate was filtered and the filter cake was washed with a small amount of water. Then, the filter cake was dissolved by heating with 1 liter of water, and the resulting solution was place...

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Abstract

This invention provides a preparation of aesculin. The mentioned preparation includes steps such as: extraction, column chromatography, concentration and crystallization. Among them the step of column chromatography is as following: a) centrifugalize or filter extract which is obtained in extracting step, filter liquor or clear supernatant liquid is directly added into macroporous resin column, among them the proportion by weight of cortex medical material and resin is 1:2-1:3;b) After all of the extract pass resin column, use eluting reagent to elute, after elutriant has clarified, begin tocollect elutriant, don't stop collecting until collecting 10-15 times of elutriant of column volume.

Description

technical field [0001] The present invention relates to a high-purity quincetin and a preparation method thereof. Background technique [0002] Qinpi is a commonly used traditional Chinese medicine, usually derived from the dry bark or dried bark of Fraxinus chinensis Roxb, Fraxinusszaboana Lingelsh. or Fraxinus stylosaLing. According to the theory of traditional Chinese medicine, Qinpi has the functions of clearing away heat and dampness, reducing astringency, and improving eyesight. Modern research shows that Qinpi has anti-pathogenic microorganisms, anti-inflammatory, diuretic, anticoagulant and anti-allergic effects. The main components of Qinpi are coumarins, including Qinpi A, Qinpi B, Qinpi, etc. Among them, Qinpi A has the highest content, about 1%. [0003] At present, 95% ethanol reflux extraction method is adopted for the preparation of quincetin, which includes extracting with ethyl acetate after concentrating the extract until there is no alcohol smell, so as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/76
Inventor 杨保华雷仕庆郭雅琦乌旭琼夏凌云
Owner SHANGHAI SINE PHARMA LAB
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