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Method for rapidly and efficiently extracting carboline alkaloids

A technology of alkaloids and carbine, applied in the direction of organic chemistry, etc., can solve the problems of poor purity, poor effect and efficiency, etc., and achieve the effect of high extraction yield

Inactive Publication Date: 2015-02-04
EAST CHINA UNIV OF SCI & TECH
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  • Description
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Problems solved by technology

However, this method is mainly aimed at compounds with medium polarity or low polarity. If the polarity of the compound is high, the effect and efficiency of the separation and extraction method of silica gel column chromatography will not be good; and if the recrystallization method is selected, how Choosing the right solvent is a difficult problem
In addition, the purity of kabbeline alkaloids obtained by separation and extraction by silica gel column chromatography is not very good.

Method used

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  • Method for rapidly and efficiently extracting carboline alkaloids
  • Method for rapidly and efficiently extracting carboline alkaloids
  • Method for rapidly and efficiently extracting carboline alkaloids

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Extraction and purification of β-carbene-4-methoxy-2-ethanoic acid methyl ester:

[0022]

[0023] (1), preliminary treatment steps: 4.1 kilograms of Nitraria fruit (collected from the Qaidam Basin in Qinghai).

[0024] Soak in 25L of 95% ethanol for three days, extract by percolation at room temperature, repeat twice, combine the extracts, concentrate under reduced pressure and evaporate all the ethanol to obtain 230 g of ethanol extract. After the extract was dissolved in deionized water (about 3 L), it was sequentially extracted with petroleum ether, ethyl acetate and n-butanol (each 3 L×3). Then, the ethyl acetate and n-butanol extracts were concentrated under reduced pressure to obtain 68.3 g of ethyl acetate extract and 153.2 g of n-butanol extract respectively.

[0025] The extract obtained after the ethyl acetate extraction part was concentrated was dissolved in 150 mL of chloroform, mixed with 120 g of 100-200 mesh coarse silica gel, and the solvent was rem...

Embodiment 2

[0036] Extraction and Purification of (3S,4R)-1-β-carbene-3,4,5-trihydroxyketone

[0037]

[0038] (1), pre-treatment steps: 3.6 kilograms of Nitraria stalks (collected from the Qaidam Basin in Qinghai) were soaked in 25L 95% ethanol for three days, extracted by percolation at room temperature, repeated twice, the extracts were combined, and concentrated under reduced pressure to obtain Ethanol extract. After the extract was dissolved in deionized water (about 3 L), it was sequentially extracted with petroleum ether, ethyl acetate and n-butanol (each 3 L×3). Then, the ethyl acetate and n-butanol extracts were concentrated under reduced pressure to obtain 43.8 g of ethyl acetate extract and 103.2 g of n-butanol extract respectively. The processing step of n-butanol extract is identical with step (one) among the embodiment 1 afterwards.

[0039] (2) MCI gel CHP-20P column chromatography: after that, according to the results of TLC thin-layer chromatography tracking, the com...

Embodiment 3

[0045] Extraction and Purification of O-Acetyl Nitronine:

[0046]

[0047] (1), pre-treatment steps: 7.6 kg of Viet Nam Phyllostachys chinensis (collected from Nanning, Guangxi) was soaked in 25L 95% ethanol for three days, extracted by percolation at room temperature, and repeated twice, the extracts were combined, concentrated under reduced pressure to obtain ethanol-leached paste. After the extract was dissolved in deionized water (about 3 L), it was sequentially extracted with petroleum ether, ethyl acetate and n-butanol (each 3 L×3). Then, the ethyl acetate and n-butanol extracts were concentrated under reduced pressure respectively to obtain 83.8 g of ethyl acetate extract and 183.7 g of n-butanol extract. The processing step of ethyl acetate extractum is identical with step (one) among the embodiment 1 afterwards.

[0048] (2) MCI gel CHP-20P column chromatography: after that, according to the results of TLC thin-layer chromatography tracking, the components where...

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Abstract

The invention relates to a method for extracting carboline alkaloids from plant herbs. The method comprises: (1) soaking the selected herbs with ethanol, carrying out percolate extraction and pressure reducing concentration to obtain an ethanol extract, and sequentially adopting petroleum ether, ethyl acetate and n-butanol to carry out extraction treatments on the obtained ethanol extract; (2) carrying out crude extraction on the ethyl acetate extraction layer and / or the n-butanol extraction layer through silica gel column chromatography, and adopting a TLC thin layer chromatography method to track, wherein the eluent is selected from a chloroform-methanol system, a petroleum ether-acetone system and a petroleum ether-ethyl acetate system; (3) carrying out chromatography separation on the crude extract through an MCI gel CHP-20P column, and adopting a TLC thin layer chromatography method to track; (4) carrying out chromatography separation on the extract obtained in the step (3) through an Sephadex LH-20 dextran gel column, wherein a methanol-chloroform solution is adopted as an eluent; and (5) purifying the extract obtained in the step (4) through HPLC to obtain the carboline alkaloid product, wherein the chromatography column is the reversed-phase column, and the mobile phase is the methanol-water solution. With the method of the present invention, the alkaloid with the high purity (more than 99%) can be obtained through purification, and the extraction yield of the method of the present invention is much higher than the extraction yield of the conventional method.

Description

technical field [0001] The invention relates to a method that can be used for rapid and high-efficiency extraction of carborinoid alkaloids in plants. Background technique [0002] Traditional Chinese medicine is a precious wealth accumulated by human beings through continuous cognition and practice in the process of fighting against diseases and injuries for thousands of years. It is the crystallization of human wisdom for thousands of years. Traditional Chinese medicine generally comes mainly from plants, animals, etc., and there are many types. Li Shizhen, a great medical scientist in the Ming Dynasty, revised "Zheng Lei Materia Medica" and compiled a masterpiece that meets the needs of the development of the times - "Compendium of Materia Medica". "Added 1021 kinds of Chinese herbal medicines. According to relevant survey data, among more than 20,000 species of higher plants in the world, less than 15% have undergone activity research or activity screening. Therefore,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/04C07D471/10C07D471/14
CPCC07D471/04C07D471/10C07D471/14
Inventor 王成云沈永嘉王雨清姜坤
Owner EAST CHINA UNIV OF SCI & TECH
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