Preparation of pure magnolol

A honokiol, high-purity technology is applied in the field of preparation of a single active ingredient of medicinal plants, and can solve the problems of inability to distinguish, difficult to prepare in large quantities, and high cost

Inactive Publication Date: 2005-02-23
HEBEI AGRICULTURAL UNIV.
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Using the traditional preparation route, the extraction rate of magnolol by alcohol extraction is generally 60-70%, which is not very high. The purification step requires the use of column separation technology. The cost of industrial preparation is high, and it is difficult to achieve large-scale preparation.
Using the supercritical fluid extraction route, the direct extract is often a mixture, the purity is not high, and needs to be further refined, and the supercritical fluid extraction equipment is expensive, and the one-time investment is too high, so it is not easy to popularize
Adopt lye percolation or lye extraction back extraction and purification technology, literature does not report the purity of product, just confirms that extract is pure magnolol according to the result of thin-layer chromatographic separation and the result of infrared, ultraviolet spectroscopic analysis, draws thus The conclusion of a higher yield is obviously not convincing
We know that the resolution of thin-layer chromatography is not high, and some substances with similar properties cannot be separated on it. Using high-resolution separation techniques, it can be seen that the single substance identified on thin-layer chromatography is not necessarily Pure; some mixtures of structures cannot be resolved by UV and IR spectroscopy
Our similar experiments showed that the pure material identified only by spectral analysis and chromatographic separation data was not very pure as confirmed by thermal analysis techniques

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] The Magnolia officinalis is crushed into 55 mesh particles. The particle size is the optimized particle size. It is placed in a Soxhlet extractor at the ratio of 1g Magnolia officinalis and 8mL ethyl acetate (preferred solvent), and heated and extracted at 85°C. 3.8 h, only one extraction, the extraction rate of magnolol is 80%, the extract is transferred to a rotary evaporator, the residue is washed once with ethyl acetate, the washing liquid is combined into the rotary evaporator and concentrated under reduced pressure at 40℃ To thicken the paste and recover the ethyl acetate, transfer the thick paste to the extraction bottle, add it to the extraction bottle 4 times according to the ratio of 20mL petroleum ether per 1g of magnolia thick paste, extract 4 times, combine the extracts, The extraction rate of phenol is 88%. The extract is transferred to a rotary evaporator, the volume of the extract is concentrated to 1 / 6 of the original volume at a temperature of 40°C, and th...

Embodiment 2

[0012] Crush Magnolia officinalis into 65-mesh particles. The particle size is optimized. Place it in a Soxhlet extractor at the ratio of 1g Magnolia officinalis and 9mL ethyl acetate (preferably solvent), and heat and extract at 95℃. 4.1 h, only one extraction, the extraction rate of magnolol is 83%, the extract is transferred to a rotary evaporator, the residue is washed once with ethyl acetate, the washing liquid is combined in the rotary evaporator, and concentrated under reduced pressure at 45℃ To thicken the paste and recover the ethyl acetate, transfer the thick paste to the extraction bottle, add it to the extraction bottle 5 times according to the ratio of 30mL petroleum ether per 1g of magnolia thick paste, extract 5 times, combine the extracts, The extraction rate of phenol is 90%, the extract is transferred to a rotary evaporator, the volume of the extract is concentrated to 1 / 7 of the original volume at a temperature of 50°C, and the concentrated extract is transferre...

Embodiment 3

[0014] Crush Magnolia officinalis into 60-mesh particles. The particle size is the optimized particle size. Place it in a Soxhlet extractor at a ratio of 1 g Magnolia officinalis plus 10 mL ethyl acetate (preferably solvent), and heat and extract 4.5 at 90°C. h, only one extraction, the extraction rate of magnolol was 82%, the extract was transferred to a rotary evaporator, the residue was washed once with ethyl acetate, the washing liquid was combined into the rotary evaporator, and concentrated under reduced pressure at 50℃ To thicken the paste and recover the ethyl acetate, transfer the thick paste to the extraction bottle, add it to the extraction bottle 4 times according to the ratio of 25mL petroleum ether per 1g of magnolia thick paste, extract 4 times, combine the extracts, The extraction rate of phenol is 93%. The extract is transferred to a rotary evaporator, the volume of the extract is concentrated to 1 / 8 of the original volume at a temperature of 45°C, and the concent...

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PUM

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Abstract

A process for preparing high-purity magnolol from magnolia bark includes such steps as pulverizing, thermal extracting in ethyl acetate, vacuum concentrating while recovering ethyl acetate, extracting by petroleum ether 4-5 times, collecting liquid extract, concentrating is rotary evaporator, adding the aqueous solution of NaOH, back extracting 4-5 times, and drying deposit in air.

Description

Technical field [0001] The invention relates to a preparation technology of a single effective ingredient of a medicinal plant, in particular a preparation technology of high-purity magnolol. technical background [0002] The traditional preparation route of magnolol is to extract magnolol from the traditional Chinese medicine Magnolia officinalis by alcohol heat reflux extraction method, and then extract it with ether or ester and concentrate it into an extract, and finally use column chromatography to analyze the extract mixture Purify. At present, in the preparation technology of magnolol that has been reported, in addition to traditional technology or direct column chromatography after alcohol extraction similar to traditional technology, it also includes supercritical fluid extraction technology, lye percolation or lye extraction followed by extraction and purification. technology. [0003] Using the traditional preparation route, the extraction rate of the alcohol-extracted...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/70C07C39/21
Inventor 陈冠华庞立业郝庆红冯雅琪田益玲屈平
Owner HEBEI AGRICULTURAL UNIV.
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