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Method for preparing palmatine by producing salting-out waste liquid by means of palmatine

A technology of patellogenin and salting out, applied in the field of preparing patellogenin, can solve problems such as waste of resources, and achieve the effects of low production cost, simple process engineering and high content

Active Publication Date: 2018-08-24
云南海沣药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for a long time, these waste liquids have been discarded, causing a serious waste of resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: Take 10L of the salting-out waste liquid from the production of palmetine, adjust the pH=9.5 with sodium hydroxide with a mass concentration of 40%, and filter; the filtrate passes through the AB-8 resin column with a flow rate of 1 column volume / h, and the filtrate goes After that, wash the resin column with 3 times the column volume of purified water to elute impurities, and then use an ethanol solution with a volume concentration of 60% to elute the alkaloid at a flow rate of 1 column volume per hour, and the eluent is detected by TLC spot plate , collect the alkaloid segment eluate; the alkaloid segment eluate is concentrated to obtain concentrate 20.2g; Minutes, add an equal volume of purified water to the reaction solution, mix well and pass through the AB-8 resin column to absorb, then wash the column with 2 times the column volume of purified water, and then elute the alkaloid with an ethanol solution with a volume concentration of 80%. Collect the...

Embodiment 2

[0019] Example 2: Take 10L of the salting-out waste liquid from the production of palmetine, adjust the pH=9 with sodium hydroxide with a mass concentration of 35%, and filter; the filtrate passes through the D101 resin column with a flow rate of 2 column volumes / h. After the filtrate is finished, , wash the resin column with 4 times the column volume of purified water to elute impurities, and then use an ethanol solution with a volume concentration of 70% to elute the alkaloids at a flow rate of 2 column volumes per hour. The eluent is detected by TLC spot plate, and collected The alkaloid section eluate; the alkaloid section eluent was concentrated to obtain 19.8g of a concentrate; the concentrate was dissolved in 179g of tetrahydrofuran, then 2.97g of DMAP was added, and 29g of methyl iodide was slowly added dropwise. After the addition was completed, continue to stir for 30 minutes. Add an equal volume of purified water to the reaction solution, mix it, and then absorb it t...

Embodiment 3

[0020] Embodiment 3: Get 100L of the salting-out waste liquid produced by palmetine, adjust the pH=10 with 45% sodium hydroxide in mass concentration, and filter; the filtrate passes through the AB-8 resin column, and the flow rate is 1.5 column volumes / h, After that, wash the resin column with 3.5 times the column volume of purified water to elute impurities, and then use an ethanol solution with a volume concentration of 65% to elute the alkaloid at a flow rate of 1.5 column volumes per hour, and the eluent is detected by TLC spot plate , collect the alkaloid segment eluate; the alkaloid segment eluate is concentrated to obtain concentrate 210g; the concentrate is dissolved with 2100g tetrahydrofuran, then 31g DMAP is added, 250g methyl iodide is slowly added dropwise, and after the dropwise addition is completed, continue to stir for 30 minutes. Add an equal volume of purified water to the reaction solution, mix well and pass through the AB-8 resin column for adsorption, the...

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PUM

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Abstract

The invention discloses a method for preparing palmatine by producing salting-out waste liquid by means of the palmatine. The method comprises the steps that alkali for producing the salting-out wasteliquid with the palmatine is subjected to pH adjustment and then filtered, filtrate enriches alkaloid through a resin column, impurities are eluted with purified water, the alkaloid is eluted with anethanol solution, eluent is concentrated and dried to obtain an alkaloid mixture containing jateorhizine, palmatine and columbamine, the alkaloid mixture is dissolved and then subjected to iodomethane methylation, the alkaloid is re-enriched through the resin column, hydrochloric acid is used for adjusting the pH, and then a crude palmatine product is obtained; the crude palmatine product is subjected to recrystallization with ethyl alcohol, filtered and dried, and the palmatine is obtained. Accordingly, the palmatine production waste liquid is reused, the content of the obtained palmatine islarger than 98%, the resource utilization rate is increased, the production cost is lowered, and the method for preparing the palmatine is simple, easy to implement and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical medicine preparation, and relates to a method for preparing palmetine from salting-out waste liquid produced by palmetine. Background technique [0002] Palmatine hydrochloride, also known as palmatine hydrochloride, chemically named 5,6-dihydro-2,3,9,10-tetramethoxydibenzo[a,g]quinazine ylide, has broad-spectrum antibacterial , antiviral effect, anti-inflammation, increase leukocyte phagocytosis and other pharmacological effects, has been made into a variety of preparations for clinical use, can be used to treat gynecological inflammation, bacillary dysentery, enteritis, respiratory tract and urinary tract infection, surgical infection and conjunctivitis Etc.; Lutein can be extracted and refined from the dried cane of Caulis Fibraurear, but the resource is scarce and the supply is in short supply. [0003] In addition to palmatine, Huangteng contains jatrorrhizine, African tetrandrine, palmatin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D455/03
CPCC07D455/03
Inventor 杨丽梅郭占伟杨杰陈谷林
Owner 云南海沣药业有限公司
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