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Preparation method of high-purity magnolia bark total-phenol

A high-purity, magnolol technology, applied in pharmaceutical formulations, medical preparations containing active ingredients, plant raw materials, etc., can solve the problems of large initial investment, expensive equipment, low product content, etc., to ensure product quality and consumption. Quantity reduction, high yield effect

Active Publication Date: 2009-08-19
湖南省中药提取工程研究中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The medicinal materials used are all Magnolia officinalis raw materials processed by traditional methods, including branch officinalis, root bark, etc. In order to reduce the production cost, it is even necessary to make the total phenolic content of Magnolia officinalis over 20 years old at 8%, which often causes the destruction of wild resources
Although the ethanol extraction method can obtain a higher extraction rate in the initial extraction, the content of the obtained product is not high, and it is difficult to follow-up to the high-purity product; supercritical CO 2 The extraction method and equipment are expensive, the initial investment is large, the cost is too high, and it is difficult to realize large-scale industrial production; although silica gel column chromatography has a good separation effect on active ingredients and high product yield, it is difficult for large-scale industrial production. It is difficult to realize; although the macroporous resin method can realize industrial production, the cycle is long and the cost is high
TLC and HPLC methods are only suitable for small-scale preparation and detection in the laboratory, and cannot be used for large-scale industrial production applications; crude products obtained by alkali extraction and alkali extraction and acid precipitation methods are extracted with petroleum ether and cyclohexane by reflux At this time, the extraction rate of active ingredients is not high, the amount of solvent consumed is large, and the repeated transfer of a large amount of solvents has great potential safety hazards

Method used

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  • Preparation method of high-purity magnolia bark total-phenol
  • Preparation method of high-purity magnolia bark total-phenol
  • Preparation method of high-purity magnolia bark total-phenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 2-year-old Magnolia officinalis Rehd.et Wils.var.bilobaRehd.et Wils. roots, all fresh and dry, weigh 1kg after drying (total phenol content is 2.8% according to the determination), cut into 1-2cm small pieces , use 20L of 1% sodium hydroxide solution to leak, add concentrated hydrochloric acid to the seepage to adjust the pH value between 1 and 2, let it stand for 3 hours, pour out the supernatant, and filter the lower part to obtain a precipitate, which is dried with six No. solvent Soxhlet extraction 5-6 hour, No. 6 solvent is reclaimed, let cool and separate out a large amount of crystals, the crystallization drying after filtering promptly gets 20.3g Magnolia officinalis extract, is 91.6% through HPLC measurement total phenolic content (its magnolol content is 37.8%, and honokiol content is 53.8%).

Embodiment 2

[0037]Take 1kg of 3-year-old Magnolia officinalis Rehd.et Wils. root bark, with a total phenol content of 6.5%, cut into 1-2cm segments, add 30L of 1% sodium hydroxide solution to infiltrate, filter the percolate, and the filtrate Add hydrochloric acid to adjust the pH value to 1-2, let it stand for 3 hours, pour out the supernatant, filter the lower part to obtain a precipitate, and extract the precipitate with n-hexane Soxhlet for 5 hours after drying, recover the extract and let it cool to precipitate a large amount of crystals, filter, After drying, 48g was obtained. The Magnolia officinalis extract with a total phenol content of 92.7% (wherein the magnolol content is 48.5%, and the honokiol content is 44.2%) is determined by HPLC.

Embodiment 3

[0039] Take 1kg of the root bark of Magnolia officinalis Rehd.et Wils.var.bilobaRehd.et Wils., which is 4 years old, and the content is 7%, cut into small pieces of 1-2cm, add 20L of 1% sodium hydroxide solution and percolate , add concentrated hydrochloric acid to the leachate to adjust the pH value to 1-2, let it stand for 4 hours, pour out the supernatant, filter the lower part to obtain a precipitate, extract 5kg of the precipitate with No. 6 solvent Soxhlet, recover the solvent, and let it cool to precipitate a large amount of crystals , to obtain 62g after crystallization and drying, the magnolol extract (wherein the magnolol content is 36.8%, and the honokiol content is 54.7%) that the total phenol content is 91.5% as measured by HPLC.

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Abstract

The invention relates to a method for preparing high purity magnolia P.E.. The method is to cut root or root bark of young magnolia officinalis planted for 2 to 5 years into small segments, carry out seepage by an alkaline solution, regulate a seepage solution by acid until the solution is slight acidic, precipitate by Soxhlet extraction of a lower organic solvent, concentrate to obtain crystal, and dry the crystal to obtain a magnolia officinalis extract product with high total phenolic content. The magnolia P.E. prepared by the method has the advantages of high content, low cost, simple preparation process and small pollution.

Description

technical field [0001] The invention relates to a plant extract, in particular to a preparation method of total magnolol obtained from magnolia bark root or root bark. technical background [0002] The raw material used in the traditional preparation of magnolol is the dry bark or branch bark of the perennial Magnolia officinalis Rehd.et Wils. or Magnolia officinalis Rehd.et Wils.var.bilobaRehd.et Wils. The raw materials are extracted and refined to obtain a high-content magnolia total phenol extract. The main active ingredients in Magnolia officinalis are magnolol, honokiol, isomagnanolol, tetrahydromagnokiol, magnolol, etc. Among them, magnolol and honokiol have the highest content. Chinese Pharmacopoeia It is stipulated that the content of these two phenols can be used medicinally if the content of these two phenols reaches more than 2% in the medicinal material. Generally, the content of the trunk bark of a tree that has grown for about 15 years is between 3-5%, and the...

Claims

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Application Information

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IPC IPC(8): A61K36/575A61P21/02A61P29/00A61P31/04A61P31/00A61P1/04A61P39/06A61P35/00A61P25/36A61P7/02A61P25/18A61K125/00
Inventor 曾建国欧阳勇
Owner 湖南省中药提取工程研究中心有限公司
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