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New alkaloids and extraction and separation method and application thereof

A separation method and new biological technology, applied in the directions of sugar derivatives, sugar derivatives, sugar derivatives preparation, etc., can solve the problems of unfavorable and lagging ethnic medicines, few effective ingredients and pharmacological activities, etc. Simple, effective, high-purity results

Active Publication Date: 2020-09-11
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the research on Jiuzilian mainly focuses on ornamental value, cultivation techniques, and breeding methods, but there are few reports on its active ingredients and pharmacological activities. The relative lag in these research aspects is very unfavorable for the development of national medicines in my country.

Method used

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  • New alkaloids and extraction and separation method and application thereof
  • New alkaloids and extraction and separation method and application thereof
  • New alkaloids and extraction and separation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] 1. Extraction and separation of alkaloid compounds

[0074] 1) Take 20 kg of dried rhizomes of Jiuzilian, heat and reflux extraction with pure methanol whose volume is 6 times the mass of dried rhizomes of Jiuzilian, extract 4 times, each time for 2 hours, combine the extracts to recover the solvent under reduced pressure, and obtain the total extract;

[0075] 2) Suspend the total extract in 4 times the amount of water, fully mix, extract 4 times with equal volume of ethyl acetate, then extract 4 times with equal volume of n-butanol, and remove the organic solvent in the extraction layer to obtain acetic acid respectively Ethyl ether layer and n-butanol layer.

[0076] 3) Take 200 g of the n-butanol extraction layer, firstly, by using silica gel column chromatography, chloroform / methanol is 100:0~0:100 in volume ratio (v / v) for gradient elution, collect a fraction every 800mL, and pass through TLC A total of 15 fractions (Bu-1~Bu-15) were obtained after identification...

Embodiment 2

[0092] 1. Extraction and separation of alkaloid compounds

[0093] 1) Take 20 kg of dried rhizomes of Jiuzilian, heat and reflux extract with methanol whose volume is 6 times the mass of dried rhizomes of Jiuzilian, extract 4 times, each time for 2 hours, combine the extracts to recover the solvent under reduced pressure, and obtain the total extract;

[0094] 2) Suspend the total extract in 4 times the amount of water, fully mix, extract 4 times with equal volume of ethyl acetate, then extract 4 times with equal volume of n-butanol, and remove the organic solvent in the extraction layer to obtain acetic acid respectively Ethyl ether layer and n-butanol layer.

[0095] 3) Take 200 g of the n-butanol extraction layer, firstly, by using silica gel column chromatography, chloroform / methanol is 100:0~0:100 in volume ratio (v / v) for gradient elution, collect a fraction every 800mL, and pass through TLC A total of 15 fractions (Bu-1~Bu-15) were obtained after identification and com...

Embodiment 3

[0117] 1) Take 10 kg of dried rhizomes of Jiuzilian, heat and reflux extract 4 times with 75% ethanol whose volume is 3 times the mass of dried rhizomes of Jiuzilian, for 3 hours each time, combine the extracts and recover the solvent under reduced pressure to obtain the total extract;

[0118] 2) Suspend the total extract in 3 times the amount of water, extract 4 times with equal volumes of petroleum ether, then extract 4 times with equal volumes of ethyl acetate and n-butanol, and remove the solvent from the extraction layer to obtain petroleum ether layers respectively, Ethyl acetate layer and n-butanol layer.

[0119] 3) Take 100 g of the n-butanol extraction layer, firstly, through silica gel column chromatography, chloroform / methanol is used for gradient elution at a volume ratio (v / v) of 100:0 to 0:100, and after TLC detection and merging of the same fractions A total of 15 fractions (Bu-1 to Bu-15) were obtained.

[0120] 4) Wherein the 9th fraction Bu-9 is separated by...

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Abstract

The invention discloses new alkaloids in common calanthe herb, and an extraction, separation and preparation method and application of the new alkaloids. The alkaloid compounds are separated from therhizome of the Tujia national medicine common calanthe herb (Shaanxi qi medicine fimbriate calanthe pseudobulb) for the first time, a molecular formula of the alkaloid compounds is C20H26N2O7 or C26H36N2O12, a structure of the alkaloid compounds is an indole alkaloid glycoside compound with one or two glucoses, and a mother core structure is two pairs of isomers. A special alkaline chromatographiccolumn is adopted, the isomers can be effectively separated, and thereby the method has the characteristics that the method is simple and convenient and effective, and the obtained compounds have high purity. The method can effectively extract and separate the new alkaloid compounds with anti-diabetic effects from the dried rhizome of the Tujia national medicine common calanthe herb (Shaanxi qi medicine fimbriate calanthe pseudobulb).

Description

technical field [0001] The invention belongs to the field of natural medicines, and relates to a class of new alkaloids and their extraction and separation methods and applications. Background technique [0002] Diabetes is the third killer that threatens human health after cardiovascular and cerebrovascular diseases and cancer. my country has now become the world's largest diabetes country. The prevalence rate of adults over 20 years old exceeds 10%, with more than 100 million patients, and nearly Among the 200 million pre-diabetic patients, one-third of this huge number of diabetes reserve army will eventually develop into real diabetes, and the situation is very grim. The harm of diabetes is mainly caused by various complications, such as vascular disease, neuropathy, kidney disease and so on. Although a variety of hypoglycemic drugs other than insulin are currently in clinical use, on the one hand, these drugs have different degrees of side effects and are not effective ...

Claims

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Application Information

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IPC IPC(8): C07H17/02C07H1/08A61P3/10
CPCC07H17/02C07H1/08A61P3/10
Inventor 张海龙高阳杨敏飞张昌龙鲍和刘杏
Owner XI AN JIAOTONG UNIV
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