Process for preparing magnolia officinalis total phenol extract by adsorptive separation

A technology of adsorption separation and preparation process, applied in the direction of medical preparations containing active ingredients, plant/algae/fungus/moss components, plant raw materials, etc., can solve the problems of large solvent loss, small preparation amount, cumbersome process, etc., and achieve The effect of low production cost, easy operation and simple process

Active Publication Date: 2014-07-23
NANKAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ultrasonic extraction method has fast extraction speed and short time, but its noise is large, and the purity of the extract is not high; the subsequent steps of hot-dipping extraction method are cumbersome, and the steps of extraction, recrystallization and other steps use a large amount of organic solvent, and the loss of extract is serious; high-speed countercurrent chromatography The purity of magnolol and honokiol can be met by separation and preparation of magnolol and honokiol, but the preparation amount is small, so it is not suitable for industrial expansion production; while the supercritical extraction method is complicated in equipment, and the initial equipment investment is large, which limits supercritical extraction. Large-scale industrial application of the method
The process of solvent extraction is cumbersome, there are many operation steps, and the loss of solvent is also large
And above-mentioned method all faces the problem that contains alkaloid component in the total magnolol of extraction gained, and the combination of residual alkaloid component and magnolol makes the simultaneous extraction of magnolol and honokiol very difficult. Difficult to achieve
[0006] In recent years, the macroporous adsorption resin method has played an increasingly important role in the separation and purification of natural plant active ingredients due to its advantages of simple process operation, environmental friendliness, reusable adsorption resin, and low separation cost. The extraction p

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  • Process for preparing magnolia officinalis total phenol extract by adsorptive separation
  • Process for preparing magnolia officinalis total phenol extract by adsorptive separation

Examples

Experimental program
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Effect test

Embodiment 1

[0021] A process for extracting high-purity total magnolol with commercialized AB-8 macroporous adsorption resin, the steps are as follows:

[0022] 1) Weigh 23g of Chinese herb Magnolia officinalis, crush it, extract it with 90mL of 5% (v%) hydrochloric acid ethanol solution at 60°C, reflux for 2 hours, filter with suction, extract twice, combine the filtrate to recover ethanol by vacuum distillation, and add Water with pH=2, centrifuged to collect the precipitate. Dissolve the precipitated solid in 140 mL of 30% ethanol aqueous solution with pH = 12.5, and centrifuge to remove a small amount of insoluble matter to obtain an adsorption liquid.

[0023] 2) Pass 60mL (2BV) of the above adsorption solution through a resin column equipped with AB-8 macroporous adsorption resin (the inner diameter of the column is 8 mm, the column length is 250 mm, and 30 mL of wet resin is installed), and the adsorption rate is 1.0 BV / h ;

[0024] 3) After the adsorption is completed, clean the...

Embodiment 2

[0029] The process for extracting high-purity total magnolol with commercialized D101 macroporous adsorption resin, the steps are as follows:

[0030] 1) Weigh 25g of Chinese herb Magnolia officinalis, crush it, extract it with 90mL of 4% (v%) hydrochloric acid ethanol solution at 55°C, reflux for 2 hours, filter with suction, extract twice, combine the filtrate to recover ethanol by vacuum distillation, and add Water with pH=2.5, centrifuged to collect the precipitate. Dissolve the precipitated solid in 145 mL of 30% ethanol aqueous solution with pH = 11.5, and centrifuge to remove a small amount of insoluble matter to obtain an adsorption liquid.

[0031] 2) Pass 90mL (3BV) of the above adsorption solution through a resin column equipped with D101 macroporous adsorption resin (the inner diameter of the column is 8mm, the column length is 250mm, and 30 mL of wet resin is installed), and the adsorption rate is 0.5 BV / h;

[0032] 3) After the adsorption is completed, clean the...

Embodiment 3

[0037] The process for extracting high-purity total magnolol with commercialized CAD-40 macroporous adsorption resin, the steps are as follows:

[0038] 1) Weigh 26g of Chinese herb Magnolia officinalis, crush it, extract it with 85mL of 6% (v%) hydrochloric acid ethanol solution at 62°C, reflux for 2.5h, filter with suction, extract twice, combine the filtrate to recover ethanol by vacuum distillation, and replenish Add water with pH=2, centrifuge to collect the precipitate. The precipitated solid was dissolved in 140 mL of 30% ethanol aqueous solution with pH=12, and the insoluble matter was removed by centrifugation to obtain an adsorption liquid.

[0039] 2) Pass 90mL (3BV) of the above adsorption solution through a resin column equipped with CAD-40 macroporous adsorption resin (the inner diameter of the column is 8 mm, the column length is 250 mm, and 30 mL of wet resin is installed), and the adsorption rate is 1 BV / h ;

[0040] 3) After the adsorption is completed, cle...

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Abstract

The invention provides a process for extracting two isomeride components in magnolia officinalis, namely honokiol and magnolol. The process comprises the steps of preparing an adsorption liquid, adsorbing by macroporous resin, balancing after adsorption, desorbing magnolia officinalis total phenol and post-treating the desorption solution. The process can be used for overcoming the interference of co-existing alkaloid when the magnolia officinalis total phenol extract is prepared by adsorptive separation, a method for preparing the adsorbent which is extracted from an organic solvent by acid-alkali isolation is provided, a continuous process for pre-separating alkaloid and extracting high-purity magnolia officinalis total phenol adsorptive resin is established, and the magnolia officinalis total phenol extract with purity higher than 70 percent is obtained by an 'adsorption-elution' process flow. The adsorptive resin method extraction process is convenient to operate, the resin can be recycled, and the process is applicable to large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of extraction and purification of monomeric active ingredients in natural plants. Especially the extraction process of honokiol and magnolol, two isomer components in magnolia bark. Background technique [0002] Magnolia officinalis is a commonly used traditional Chinese medicine. It was first recorded in "Shen Nong's Materia Medica", and was listed as a middle grade. It was recorded in successive dynasties of herbal medicines and "Chinese Pharmacopoeia". The 2010 edition of "Chinese Pharmacopoeia" stipulates that magnolia officinalis is the dry dry bark and root of Magnolia officinalis Rehd. et Wils. or Magnolia officinalis Rehd. et Wils. Var. biloba Rehd. et Wils. Bark and branches. Modern pharmacological experiments have proved that magnolia bark has broad-spectrum antibacterial, anti-tumor, anti-inflammatory, cardiovascular and cerebrovascular protection, anti-ulcer and anti-coagulant effects. [0003...

Claims

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Application Information

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IPC IPC(8): A61K36/575
Inventor 王春红
Owner NANKAI UNIV
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