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Method for extracting honokiol and magnolol from mangnolia officinalis crude extract

A honokiol and crude extract technology, applied in the field of preparation of natural chemicals, can solve the problems of low single component content, complicated operation, long cycle, etc., and achieve simple purification process, good selectivity, and high throughput big effect

Active Publication Date: 2014-07-16
浙江得恩德制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the techniques for separating honokiol and magnolol from the crude extract of magnolia bark are mainly macroporous resin adsorption method, TLC preparation and separation method, high-speed countercurrent extraction method, silica gel column chromatography, high performance liquid chromatography preparation method, etc. , the high-speed countercurrent extraction method and the high-performance liquid chromatography preparation method are expensive in equipment, the initial investment is large, the cost is too high, and the operation is complicated, the production volume is small, and large-scale production is difficult to achieve; although silica gel column chromatography and macroporous resin adsorption method It can be produced on a large scale, but the content of the single component obtained is not high, and the workload is large, the cycle is long, the production cost is too high, and the product has no market competitiveness at all; the TLC preparation and separation method can only be used for small-scale preparation in the laboratory, not for large-scale industrial production
[0005] Chinese patent application number 201110328031.6 discloses a method for preparing high-purity magnolol and honokiol from magnolia bark, which is characterized in that the total magnolol is extracted with ethanol solution, and then the total magnolol is wetted with silica gel. Separation by column chromatography using petroleum ether-ethyl acetate-methanol, the obtained magnolol content is only about 90%, and the mother liquor needs to be re-purified by silica gel column, which has long cycle, low efficiency and high cost, so it is not suitable industrialized production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 100g of the crude extract of Magnolia officinalis, add 1000ml of cyclohexane, put it in a 10000ml round bottom flask, heat to reflux at 85°C on a water bath to dissolve, and react for 2 hours when the reflux starts. Take purified water and heat it to about 80°C, add 2.1g of analytically pure sodium bicarbonate and 0.712g of analytically pure sodium hydroxide, add purified water to 1000ml, and prepare a pH10.5 buffer solution. Add 5000ml of buffer solution prepared according to the aforementioned method into a 10000ml round-bottomed flask, start stirring for 30 minutes to fully mix, let it stand for 10 minutes and then place layers on the separatory funnel, separate the lower layer of buffer solution, and perform the same operation five times. Take the residual liquid to detect no magnolol spots, then add 1% sodium hydroxide solution to extract honokiol; add 4M HCL to the lower buffer layer (add 10ml 4M hydrochloric acid to every 1000ml buffer solution) to make the p...

Embodiment 2

[0025] Take 1000g of magnolia bark crude extract, add 10000ml of cyclohexane, heat and reflux at 80°C in a 100L reactor for 3 hours; take another 100Kg of drinking water, put it in an open pot and heat it to about 80°C, press 0.9g of sodium hydroxide, carbonic acid Sodium hydrogen 2.1g, add drinking water to a ratio of 1000ml, add sodium bicarbonate and sodium hydroxide, stir to fully dissolve into a buffer solution with a pH of 10.5. Turn on the reactor mixer, add 50Kg of buffer solution while stirring, and then stir for 15 minutes, let it stand, and separate layers; operate in the same way, extract five times in total, take samples of the residual liquid to detect no magnolol spots, and prepare with drinking water 1% sodium hydroxide solution, extract twice. Add 4M HCL to the lower buffer layer (10ml 4M hydrochloric acid per 1000ml buffer) to make the pH around 3, stir well and then stand for crystallization to obtain 408g of magnolol coarse crystals; add 4M HCL to the lower...

Embodiment 3

[0028]Take 10Kg of Magnolia officinalis crude extract, add 80Kg of cyclohexane, heat and reflux in a multi-functional extraction tank for 4 hours to fully dissolve; take another 500Kg of drinking water in an open pot, heat it to about 80°C with steam, press hydrogen Sodium oxide 0.9g, sodium bicarbonate 2.1g, add drinking water to a ratio of 1000ml, add sodium bicarbonate and sodium hydroxide, stir to fully dissolve into a buffer solution with a pH of 10.5. Turn on the multifunctional extraction tank mixer, add 500Kg of buffer solution while stirring, and then stir for 15 minutes, let it stand, and separate layers; operate in the same way, extract five times in total, take samples of the residual liquid to detect no magnolol spots, and take drinking Prepare 1% sodium hydroxide solution with water and extract twice. Add 4M HCL to the lower buffer layer (add 10ml 4M hydrochloric acid to every 1000ml buffer) to make the pH around 3, stir well and let stand for crystallization to ...

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Abstract

The invention discloses a method for extracting honokiol and magnolol from a mangnolia officinalis crude extract. In existing methods of separating the honokiol from the magnolol in the mangnolia officinalis crude extract, in some methods, the cost is too high, the production volume is low, and mass production is not easy to achieve. In the method disclosed by the invention, by means of the characteristic that the magnolol and the honokiol contained in the mangnolia officinalis crude extract can be completely separated in a weak polar solution under an alkaline condition with certain concentration, the magnolol is extracted from a mixed solution by using a weak alkaline solvent, the honokiol is left in the solution, the honokiol is extracted by a strong alkaline solution, some oily impurities are left in an organic solvent layer, then acid regulation and precipitate out are carried out respectively, at this time, the contents of the honokiol and the magnolol in the obtained coarse-grain are greatly improved. The method disclosed by the invention is simple and feasible in separation and purification process and is suitable for large-scale industrial production, and the prepared magnolol and honokiol can be used for developing new medicines with single components.

Description

technical field [0001] The invention relates to a method for preparing natural chemicals from plant extracts, in particular to a method for extracting honokiol and magnolol, a single component, from magnolia bark crude extract. Background technique [0002] Magnolol and Honokiol are the main chemical constituents of the traditional Chinese medicine Magnolia officinalis. Pharmacological tests have shown that magnolol has a special, long-lasting muscle relaxation effect and strong antibacterial effect, and can inhibit platelet aggregation. It is mainly used as an antibacterial and antifungal drug clinically. In terms of antibacterial effect, magnolol has significant antibacterial activity against Gram-positive bacteria, acid-resistant bacteria, and filamentous fungi, and has a more significant antibacterial effect on Streptococcus mutans, and has the strongest inhibitory effect on Staphylococcus. Clinically, it is mainly used to eliminate fullness in the chest and abdomen, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/21C07C37/68C07C37/72C07C37/84
CPCC07C37/685C07C37/70C07C37/72C07C39/21
Inventor 吕文辉刘法千鲍立曾
Owner 浙江得恩德制药股份有限公司
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