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Method for extracting total alkaloid of common fibraurea stems, separate fibriuretinin and jatrorrhizine

A technology of total alkaloids and extraction methods, which can be used in pharmaceutical formulations, medical preparations containing active ingredients, plant/algae/fungus/moss components, etc., and can solve problems such as waste, inability to obtain palmetine, and environmental pollution. Achieve the effects of reducing pollution, improving the utilization rate of medicinal material resources, and making the process simple and feasible

Inactive Publication Date: 2010-04-21
CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the method reported at present, it is only used to extract palmatine, and the extracted palmatine contains 95.0%-98% of palmatine hydrochloride, so higher purity of palmatine cannot be obtained. According to the cost estimation of the advanced technology, to produce 1 ton of palmatine, the crude alkali mother liquor is 4,000 tons, and the salt is about 250 tons. The crude alkali mother liquor is completely discarded, which not only loses a lot of salt, pollutes the environment, but also wastes medicinal materials. jatrorrhizine

Method used

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  • Method for extracting total alkaloid of common fibraurea stems, separate fibriuretinin and jatrorrhizine
  • Method for extracting total alkaloid of common fibraurea stems, separate fibriuretinin and jatrorrhizine
  • Method for extracting total alkaloid of common fibraurea stems, separate fibriuretinin and jatrorrhizine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1 The extraction and separation method of palmatine and jatrorrhizine of the present invention

[0038] Pulverize the yellow vine into a coarse powder, add 12 times the amount of 0.2% sulfuric acid solution, soak for 24 hours, filter, and collect the filtrate; add 10 times the amount of 0.2% sulfuric acid solution to the dregs, soak for 24 hours, filter, combine the two filtrates, Obtain alkaloid extract.

[0039] D. 101 The technological conditions of macroporous adsorption resin purification of vine alkaloids are as follows: the crude drug concentration of the loading sample liquid is 0.5g / ml, and the adsorption flow rate is controlled between 2BV / h; Elution with ethanol, collect the eluate to 2BV; ①Recover ethanol from the eluate, concentrate, and evaporate to dryness to obtain the total alkaloids of Phytophthora vine, or ②Recover ethanol from the eluate, and continue to concentrate to a certain volume (approximately 1 / 5 of that), adjust the pH to 2 with...

Embodiment 2

[0043] Embodiment 2 The difference between the inventive method and the traditional extraction method

[0044] At present, the conventional preparation method of the total alkaloids of Phytophthora fragrans, the crude and refined products of Phytophthora fructus is: adopting the salting-out method to obtain the crude alkaloids of Phytophthora fructus (namely total alkaloids) by precipitating from the extract of medicinal materials. After two more crystallizations, a content of 94% of palmatine was obtained. The process flow and the transfer rate of each step are shown in figure 1 ; Process flow of the present invention and each step transfer rate, see figure 2 .

[0045] pass figure 1 and figure 2 The comparison shows that the extraction and separation method of the present invention makes the transfer rate of palmatine hydrochloride reach more than 26%, which is 1.7 times higher than the existing traditional technology (about 15%).

Embodiment 3

[0046] Embodiment 3 palatine HPLC assay

[0047] 1. Chromatographic conditions

[0048] Column used: Hypersil BDS C 18 (5 μm, 4.6mm × 250mm); mobile phase is acetonitrile: water (containing 0.4% phosphoric acid and 0.4% diethylamine) (30:70); detection wavelength is 345nm; column temperature 25 ℃; flow rate 1.0ml / min.

[0049] 2. Preparation of the test solution

[0050] Take 30mg of palmatine, weigh it accurately, put it in a 50ml measuring bottle, add methanol to the scale, and shake well; accurately draw 1ml of the stock solution, put it in a 10ml measuring bottle, add methanol to the scale, shake well, and use it as the test solution. Inject into a liquid chromatograph for determination.

[0051] 3. Preparation of reference solution

[0052] Take an appropriate amount of palmatine hydrochloride reference substance, accurately weigh it, put it in a 10ml measuring bottle, add methanol to set the scale, shake well, and use it as the reference substance stock solution (970...

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Abstract

The invention provides a total alkaloid of common fibraurea stems, which contains palmatine hydrochloride with the weight percentage content over 60 percent and jatrorrhizine hydrochloride with the weight percentage content more than 10 percent. The invention also provides a method for preparing the total alkaloid of common fibraurea stems, fibriuretinin and jatrorrhizine. The method can be adopted to prepare the total alkaloid of common fibraurea stems and to extract separate fibriuretinin and jatrorrhizine, wherein if dry products are calculated on the basis of anhydrous palmatine hydrochloride (C21H22O4N.HCl), the fibriuretinin has the weight percentage content higher than 98.0 percent and is high in purity. The extraction-separation method enables the transfer rate of the palmatine hydrochloride to be up to over 26 percent and is 1.7 times higher than the prior conventional process (about 15 percent). The extraction process also maintains the jatrorrhizine while raising the transfer rate of the palmatine hydrochloride serving as a main component of the fibriuretinin, thereby greatly improving the resource utilization rate of medicinal materials. The process adopts a resin purification method, is simple and feasible in process flow, capable of regenerating and repeatedly utilizing resin and reducing environmental pollution caused by lye compared with the conventional salting-out method.

Description

technical field [0001] The invention relates to a preparation method of the total alkaloids of Phustophthora vine, and an extraction and separation method for simultaneously separating and obtaining high-purity palmatine and jatrorrhizine. Background technique [0002] Huangteng is the dried cane of Huangteng Fibraurerecisa Pierre., a plant of Fangjiaceae. It is a commonly used traditional Chinese medicine in Yunnan, Guangxi, Guangdong and other places. Aliases are: Rhubarb Rhizoma (Guangxi "Chinese Herbal Medicine New Medical Method Prescription Collection"), Tuhuanglian ("Nanning Drug State"), Garcinia Cambogia ("Guangxi Traditional Chinese Medicine"), and Huanglianteng ("Chinese Medicine Plant Illustrated Book"). The vines of the yellow vine mainly contain alkaloids: Palmatine, Jatrorrhizine, Pseudocolumbamine and Fibralactone, as well as Fibranine, Fibraminine, Sterol, etc. [0003] [0004] Palmatine Jatrorrhizine [0005] Palmatine is a quaternary ammonium alkalo...

Claims

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Application Information

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IPC IPC(8): A61K36/59A61P9/06A61P25/20A61P31/04A61P31/10A61P31/14A61P31/20A61P37/04C07D455/03A61K135/00
Inventor 刘友平陈鸿平程贝
Owner CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE
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