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Method for analyzing and separating preparation of Huperzine A and Huperzine B

A technology of Huperzine A and Huperzine B, applied in the field of analytical chemistry, can solve the problems of low yield, discard, long process cycle and the like, and achieve the effects of low separation, good presentation and high sensitivity

Inactive Publication Date: 2005-12-07
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a simple and accurate method for analyzing the content of huperzine A and huperzine B, and overcome the large consumption of toxic and harmful organic solvents and long process cycle in the existing separation and preparation of huperzine A , the yield is low, and the effective components such as huperzine B are discarded and other defects, thus providing a method for efficiently separating and purifying huperzine A and huperzine B by utilizing chromatographic integration technology and using low-toxic organic solvents, to Obtain pure huperzine A and huperzine B with high purity and recovery

Method used

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  • Method for analyzing and separating preparation of Huperzine A and Huperzine B
  • Method for analyzing and separating preparation of Huperzine A and Huperzine B
  • Method for analyzing and separating preparation of Huperzine A and Huperzine B

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Effect test

Embodiment 1

[0032]Embodiment 1, with the huperzine A 0.053% containing, the huperzine B 0.013% phyllocolumn as raw material, separation and purification preparation 99.1% huperzine A and 98.4% huperzine B, the process adopts high-efficiency liquid phase The content of huperzine A and huperzine B was analyzed by chromatography.

[0033] The HPLC analysis conditions of the sample are: Waters Alliance 2695 high performance liquid chromatograph, 2996 ultraviolet diode array detector, chromatographic column filler is phenyl bonded phase silica gel Inertsil Ph-3, mobile phase methanol: water=90: 10, sample injection The volume is 20 μl, and the flow rate is 1ml / min.

[0034] 1) After 1 kg of dry Melaleuca tower containing huperzine A 0.053% and huperzine B 0.013% is pulverized, soak for 24 hours with 10 liters of 0.1% nitric acid; after pouring out the supernatant, add 5 liters to the residue Soak in 0.1% nitric acid for 12 hours; filter and wash the filter residue several times with the same ...

Embodiment 2

[0040] Embodiment 2, with the huperzine A 0.016% containing, the huperzine B 0.0033% melaleuca tower as raw material, separation and purification prepare 98.5% huperzine A and 98.2% huperzine B, the process adopts high-efficiency liquid phase The content of huperzine A and huperzine B was analyzed by chromatography.

[0041] The HPLC analysis method of sample is: Beckman FL750 high performance liquid chromatograph, ultraviolet multi-wavelength detector, chromatographic column filler is pentafluorophenyl bonded phase silica gel Curosil-PFP, mobile phase methanol: water=70: 30, sample volume 10μl, flow rate 2ml / min.

[0042] 1) After pulverizing the dried Melaleuca tower containing 0.016% of huperzine A and 0.0033% of huperzine B, soak it with 1% sulfuric acid for 24 hours; after pouring out the supernatant, add 1% sulfuric acid to the residue to soak for 12 hours; filter, wash the filter residue several times with the same acid solution; combine the filtrate and washing liquid...

Embodiment 3

[0048] Embodiment 3, with the huperzine A 0.0035% containing, the huperzine B 0.0014% melaleuca tower as raw material, separate and purify and prepare 98.5% huperzine A and 98.1% huperzine B, the process adopts high-efficiency liquid phase The content of huperzine A and huperzine B was analyzed by chromatography.

[0049] The HPLC analysis method of sample is: Agilent 1100 high-performance liquid chromatograph, ultraviolet multi-wavelength detector, chromatographic column filler is nitrile-based bonded phase silica gel Lichrospher 100 CN, mobile phase methanol: water=60: 40, and the injection volume is 20 μ l , flow rate 0.5ml / min.

[0050] 1) After pulverizing the dried Melaleuca tower containing 0.053% of huperzine A and 0.013% of huperzine B, soak it with 2% sulfuric acid for 36 hours; after pouring out the supernatant, add 2% sulfuric acid to the residue and soak it for 12 hours; filter, wash the filter residue several times with the same acid solution; combine the filtra...

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Abstract

The invention relates to a process for analyzing and separating preparation of Huperzine A and Huperzine B, which comprises the steps of disintegrating and immersing raw material, enriching and concentrating with macroporous absorption resin, reversed phase column chromatography, non-alkyl bonded phase silica gel medium column chromatography, concentrating and crystallizing.

Description

technical field [0001] The invention relates to the field of analytical chemistry and a method for extracting traditional Chinese medicines, in particular to a method for analyzing, separating and preparing huperzine A and huperzine B. Background technique [0002] Huperzine A is a new alkaloid isolated from the traditional Chinese medicine Huperzia melaleuca. It is a potent, reversible and highly selective acetylcholinesterase (AChE) inhibitor, which is a second-generation AChE inhibitor. , is also the most successful drug for the treatment of Alzheimer's disease (Alzheimer's Disease, AD, also known as senile dementia) developed in China. Food additives or nutraceuticals used to improve memory. In addition, Melaleuca contains other alkaloids with strong AChE inhibitory activity, among which huperzine B is the most representative, and its content is second only to huperzine A. Due to the similar structure of huperzine B and huperzine A, it becomes the most difficult substa...

Claims

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Application Information

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IPC IPC(8): C07D221/22
Inventor 苏志国李秀男孙海虹马润宇
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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