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New method for extracting and separating high-purity huperzine A from thousand-layer column

A technology of huperzine A and Melaleuca tower, which is applied in the field of extraction and separation of high-purity huperzine A, can solve the problems of not meeting market demand, small production scale, and low product purity, and achieve saving of reagents, short process cycle, The effect of high purity

Inactive Publication Date: 2010-04-14
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Above-mentioned various methods or the product purity that obtains is lower, or yield is lower, or operation is troublesome, and the production cost that has is higher, and production scale is small, can't satisfy market demand

Method used

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  • New method for extracting and separating high-purity huperzine A from thousand-layer column
  • New method for extracting and separating high-purity huperzine A from thousand-layer column
  • New method for extracting and separating high-purity huperzine A from thousand-layer column

Examples

Experimental program
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Effect test

preparation example Construction

[0027] Preparation of the extract: ① Add 3-25 times the amount of 0.2-2% sulfuric acid to the pulverized Melaleuca tower, and soak it at room temperature for 0-24 hours; The extract is ready for use;

[0028] Macroporous resin pre-separation: ① adjust the pH of the extract to 8-10, and put it on a macroporous adsorption resin column; ② use 0-15% ethanol for the first time to elute, and discard the eluent; ③ use 15% for the second time -Elute with 70% ethanol, collect the eluent, recycle the ethanol, and obtain the extract extract;

[0029] Purification by high-speed countercurrent chromatography: using petroleum ether-n-butanol-phosphate buffer as a solvent system, the crude extract of huperzine A obtained above is purified by high-speed countercurrent chromatography to obtain high-purity huperzine A. The purity is above 98%.

Embodiment 1

[0031] Take 100g of crushed melaleuca medicinal material, add 1.5L of 1% sulfuric acid, soak at room temperature for 24 hours, percolate until no huperzine A can be detected in the effluent, and adjust the pH of the extract to 8 with ammonia water.

[0032] Put the above pH-adjusted extract on a macroporous adsorption resin column, elute with 5% ethanol until the effluent is colorless, and discard the eluent. Then elute with 30% ethanol, detect that there is no huperzine A in the eluate, collect the eluate, and distill under reduced pressure to recover the solvent to obtain the extract of huperzine A.

[0033] Using petroleum ether-n-butanol-phosphate buffer as a high-speed countercurrent chromatography two-phase solvent system to separate and purify the extract of huperzine A, the stationary phase is petroleum ether-n-butanol (1.5:3.5, V / V), and the mobile The phase is a phosphate buffer containing both sodium dihydrogen phosphate and disodium hydrogen phosphate at 1%.

Embodiment 2

[0035] Take 100g of crushed melaleuca medicinal materials, add 1.5L of 1% sulfuric acid, soak at room temperature for 24 hours, and ultrasonically sonicate for 30 minutes to separate the medicinal liquid. 1L of 1% sulfuric acid was added to the medicinal residues, and the medicinal liquid was separated by ultrasonic treatment for 20 minutes. Combine the medicinal solutions, filter to remove impurities in the extract, and adjust the pH of the extract to 8.

[0036] Put the above pH-adjusted extract on a macroporous adsorption resin column, elute with 5% ethanol until the effluent is colorless, and discard the eluent. Then elute with 30% ethanol until there is no huperzine A in the effluent, collect the eluate, and distill under reduced pressure to recover the solvent to obtain the extract of huperzine A.

[0037] Using petroleum ether-n-butanol-phosphate buffer as a high-speed countercurrent chromatography two-phase solvent system to separate and purify the extract of huperzin...

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Abstract

The invention relates to a new method for extracting and separating high-purity huperzine A from a thousand-layer column. The method comprises the following three technological steps: first, the preparation of extract liquor, second, the pre-separation of macroporous resin, and third, the purification by high-speed countercurrent chromatogram. The preparation of the extract liquor comprises immersing the grinded thousand-layer column in acid liquor, implementing diacolation and ultrasonic extraction, and obtaining the extract liquor for further use. The pre-separation of the macroporous resin comprises regulating the pH value of the extract liquor to 8 to 10, delivering the extract liquor through a macroporous resin column, eluting the extract liquor with alcohol of different concentration, and obtaining extract extractum after recovering solvent with alcohol eluent. The purification by high-speed countercurrent chromatogram comprises taking petroleum ether, n-butyl alcohol and phosphate buffer as the solvent system to purify the extractum by a high-speed countercurrent chromatogram method, and obtaining the high-purity huperzine A.

Description

technical field [0001] The invention relates to a method for extracting and separating high-purity huperzine A from Chinese herbal medicine Melaleuca pagoda. Background technique [0002] Melaleuca pagoda is the whole herb of the genus Hupermus serrata of the genus Hupermus serrata, a fern. It is used in folk to dissipate blood stasis and blood, reduce swelling and relieve pain, dehumidify, clear away heat and detoxify. The alkaloids huperzine A and huperzine B contained in it have a strong inhibitory activity on cholinesterase, and clinical experiments have confirmed that huperzine A has a significant effect on the treatment of Alzheimer's disease. Huperzine A extracted from Melaleuca pagoda is a new drug created in China. Belonging to reversible cholinesterase inhibitors, it is currently one of the safest and most effective drugs for the treatment of benign memory impairment and Alzheimer's disease. [0003] There are existing literature reports on methods for extracting...

Claims

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Application Information

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IPC IPC(8): C07D221/22A61P25/28
CPCY02P20/582
Inventor 孙爱玲柳仁民
Owner LIAOCHENG UNIV
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