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Method for preparing bergeninum

A petrolatum and ultrafiltration membrane technology, which is applied in the field of membrane separation and macroporous resin preparation petrolatum, can solve the problems of high energy consumption, low degree of industrialization, and high consumption of organic reagents, and achieves low energy consumption, low production cost, The effect of reducing the number of acid-base treatments

Inactive Publication Date: 2011-02-02
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] As mentioned above, there are problems such as high energy consumption or high organic reagent consumption or low industrialization degree in the existing process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take the rock cabbage raw material and crush it, take 10kg, add 20 times the amount of saturated lime water to percolate and extract for 20 hours, filter, add the extract solution to ultrafiltration with a tubular composite ultrafiltration membrane system with a molecular weight cut-off of 3000-6000, add an appropriate amount of water for dialysis, and dialysis Adjust the ph2 precipitation with liquid hydrochloric acid, filter out the precipitate, reflux and dissolve the precipitate in hot water, add the AB-8 macroporous resin column for adsorption, and elute with a lime solution with a pH of 8, collect the eluate and adjust the pH of hydrochloric acid to place it for crystallization, and the crystallization Filter it out, then reflux with 99% ethanol to dissolve and recrystallize, and dry in vacuo to obtain white needle-like crystal petgenin with a content of 98.6% and a yield of 3.5%.

Embodiment 2

[0021] Take astilbee raw material and pulverize it, take 10kg, add 15 times the amount of saturated lime water to percolate and extract for 24 hours, filter, add the extract solution to a tubular composite ultrafiltration membrane system with a molecular weight cut-off of 3000-6000 for ultrafiltration, add an appropriate amount of water for dialysis, and dialysis Liquid sulfuric acid adjusts the ph3 precipitation, filters out the precipitate, dissolves the precipitate in hot water reflux, adds ADS-8 macroporous resin column for adsorption, and elutes with a lime aqueous solution of ph10, collects the eluate and adjusts the sulfuric acid ph3 to place crystallization, the crystallization Filtrate, then reflux with 99% ethanol to dissolve and recrystallize, and vacuum-dry to obtain white needle-like crystalline petgenin with a content of 98.2% and a yield of 3.0%.

Embodiment 3

[0023] Grind the raw material of Aodi tea, take 10kg, add 20 times the amount of saturated lime water to percolate and extract for 20 hours, filter, add the extract solution to ultrafiltration with a tubular composite ultrafiltration membrane system with a molecular weight cut-off of 3000-6000, add appropriate amount of water for dialysis, Adjust the ph3 precipitation through liquid hydrochloric acid, filter out the precipitate, reflux and dissolve the precipitate in hot water, add the HZ818 macroporous resin column for adsorption, and then elute with the lime aqueous solution of ph9, collect the eluate and adjust the ph5 to place it for crystallization, and filter out the crystallization. Then reflux with 99% ethanol to dissolve and recrystallize, and vacuum dry to obtain white needle-like crystal petgenin with a content of 97.5% and a yield of 2.8%.

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PUM

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Abstract

The invention provides a method for preparing bergeninum. The method comprises the following steps of: crushing saxifragaceae plants such as purple bergenia, astilbe chinensis or Japanese ardisia serving as raw materials; adding 15 to 20 times the amount of saturated limewater for percolating and extracting; filtering and adding an ultrafiltration membrane into extracting solution for performing ultrafiltration; adding a proper amount of water for dialyzing; collecting permeate liquid; regulating the pH of the permeate liquid to be between 2 and 3; filtering precipitate out; refluxing and dissolving the precipitate by using hot water; adding macroporous resin for performing column adsorption; eluting by using the solution of limewater with the pH of between 8 and 10; regulating the pH of eluent to be between 3 and 5; filtering crystals; refluxing and dissolving a filtrate with 99 percent ethanol; and performing recrystallization and vacuum-drying to obtain a product. The method for preparing the bergeninum has simple process operation and low energy cost, meets the requirements on energy-saving and emission-reduction, and is suitable for industrialization.

Description

Technical field: [0001] The invention relates to a preparation method of petracenin, in particular to a method for preparing petracenin by membrane separation and macroporous resin. Background technique: [0002] Petgenin, also known as petracenolide, is white loose needle-like crystal or crystalline powder; odorless, bitter taste; gradually changes color when exposed to light or heat. Soluble in methanol, slightly soluble in water or ethanol. Molecular formula: C14H16O9; molecular weight: 328.27. [0003] Begenin has antitussive and expectorant properties and is used for the treatment of chronic bronchitis. Now the petracenin extract has been included in the "Chinese Pharmacopoeia", and there are also patented petracenin tablets. [0004] Betgenin is mainly extracted from saxifrage plants, rock cabbage, astilbe and dwarf tea. There are many extraction processes of petogenin, including organic reagent or water reflux extraction, acid-base precipitation method, resin meth...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCY02P20/10
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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