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Method of refining plamatine from herba fibranreae recisae total ulkuloid and its application

A technology of total alkaloids and PH value, applied in the direction of drug combination, pharmaceutical formula, medical preparations containing active ingredients, etc. The problem of non-conformity in the purity of tin, to achieve the effect of low cost, reduced impurity content, and low cost

Inactive Publication Date: 2005-08-10
郭曙平
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And above-mentioned technique or method of prior art prepares the highest content of palmatine can only reach about 96.0%, impurity jatrorrhizine content has about 3.0%, berberine also has about 1.0%
Therefore, the purity of its palmatine does not meet the requirements of modern pharmacology, and cannot meet the requirements of the modern pharmaceutical industry for the high purity of raw materials
[0009] The reason why the existing technology cannot solve the problem of the purity of palmatine is because no suitable process conditions have been found, so it is impossible to break through this technical problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Using solvent pH value separation method:

[0045]100g of total alkaloids of vine vine, the total alkaloids of vine vine is the product extracted by the above-mentioned prior art process, add 1000ml of deionized water, and heat to dissolve it; adjust the pH value of the solution to 14 with 10% NaOH solution, keep warm 2 hours; add refined sodium chloride (referring to pharmaceutical grade) 77g, stir, leave for 12 hours, make precipitation separate out completely; Filter, remove salt-containing mother liquor; Fully wash, precipitate with the alkalized water that pH value is 14, pump Dry and filter cake; then place it at 70°C and dry for more than 12 hours; suspend the dry matter in 95% ethanol and heat to reflux to fully dissolve palmatine in the alcohol solution; filter to remove insoluble substances; filtrate with 10 Adjust the pH value to 3.5 with % HCl solution; then place it at a low temperature of 2-10°C for more than 24 hours; at this time, a large number of yello...

Embodiment 2

[0049] Separation by column chromatography:

[0050] Total alkaloids 10g of Phytophthora fructus (source is the same as in Example 1), put on an aluminum oxide chromatography column (also can go on an ion resin chromatography column or a macroporous resin chromatography column or a silica gel chromatography column or a polyamide chromatography column), and use 80 ~ Elute with 96% ethanol; collect the ethanol eluate and concentrate; the concentrate is applied to an alumina chromatography column again, and eluted with chloroform, chloroform:methanol (6:4) and methanol successively, and the eluate is collected in sections; Partially recover the solvent from the eluent; then adjust the pH value to 2-4 with 10% HCl; place it at a low temperature (2-10°C) for more than 24 hours; precipitate yellow needle-like crystals, which are palmatine hydrochloride. The precipitated reddish-brown needle-like crystals are the hydrochloride of impurity jatrorrhizine; the content of palmatine deter...

Embodiment 3

[0053] Embodiment 3: the preparation of palmatine hydrochloride injection

[0054] Get 20g of palmatine hydrochloride, add water for injection, stir and make it dissolve, then add water for injection to 800ml, measure the pH value, adjust the pH value at 3.0-8.0 with 10% hydrochloric acid or 10% sodium hydroxide solution, the specific value is 5.5; Add about 0.2% activated carbon for needles, stir evenly; keep warm for 30 minutes, clarify and filter, add water for injection to the filtrate to 1000ml; sterilize and filter, divide into 1ml ampoules, and sterilize at 100°C The palmatine hydrochloride injection preparation was obtained in 30 minutes.

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Abstract

A process for preparing the refined palmatine from general fibraurea alkaloid faetures that the principle that different kinds of alkaloid have the difference in pH value and solvent polarity is used for separation or the column photography is used for separation, and the relative refining technique is also used to make its purity be 99.0% or more.

Description

technical field [0001] The invention relates to a method for refining palmatine, in particular to a method for refining palmatine from total alkaloids of vine vine. Background technique [0002] Palmatine is also known as Palmatine, African Tetrandine, and Palmatine, and its English name is Palmatine. ) quinozine structure. This is an alkaloid widely found in Berberis genus plants. [0003] Pharmacological studies have confirmed that palmatine has a broad-spectrum antibacterial effect, and has inhibitory effects on bacteria such as Gram-positive bacteria and Gram-negative bacteria, 12 common pathogenic molds and various viruses including cold viruses. Moreover, palmatine can enhance the phagocytic ability of white blood cells in the body. Clinically, it can be used to treat upper respiratory tract infection, tonsillitis, enteritis, dysentery, genitourinary infection, surgical and gynecological infectious inflammation, leukopenia caused by chemotherapy and radiotherapy, in...

Claims

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Application Information

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IPC IPC(8): A61K31/4748A61P1/16A61P11/00A61P11/04A61P13/00A61P15/00C07D491/147
Inventor 郭曙平
Owner 郭曙平
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