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Method for preparing flavonoid glycoside and stibene glucoside type compound by separating from fenugreek

A technology of stilbene glycosides and flavonoid glycosides, which is applied in the field of separation and preparation of natural medicines, can solve the problems of large consumption of organic reagents, difficulty in efficient separation, long required period, etc., and achieves shortened separation time, simple process, heavy weight, etc. good effect

Inactive Publication Date: 2013-09-18
湖州藏源生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the polarities of the target components in fenugreek are very similar, it is difficult to efficiently separate them by traditional column chromatography and extraction methods reported in existing patents, the required cycle is long, the product purity is low, the sample loss is more, and the consumption of organic reagents Big
[0008] High-speed counter-current chromatography (HSCCC) is a liquid-liquid partition chromatography technique that does not use solid supports or carriers, which overcomes the disadvantages of loss and denaturation caused by the adsorption of solid carriers to samples. And it can realize high-efficiency preparative separation in a short time, so it has been widely used in the separation and preparation of plant active ingredients. At present, there are no literature reports at home and abroad to separate and prepare stilbene compounds from fenugreek. And there is no high-speed countercurrent chromatography technology applied to the separation and preparation of flavonoid glycosides and stilbene glycoside monomer compounds in fenugreek plants

Method used

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  • Method for preparing flavonoid glycoside and stibene glucoside type compound by separating from fenugreek
  • Method for preparing flavonoid glycoside and stibene glucoside type compound by separating from fenugreek
  • Method for preparing flavonoid glycoside and stibene glucoside type compound by separating from fenugreek

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] 1) Preparation of the sample to be separated:

[0068] Take 10 g of mature and dry seeds of wild or cultivated fenugreek plants, cut or crush them, pass through a 40-mesh sieve, extract with 100 mL of ethanol aqueous solution with a concentration of 95% by mass, and conduct heating and reflux extraction for 3 times at an extraction temperature of 90°C , each 2h, combined and concentrated to obtain the fenugreek extract with a solid content of 48%;

[0069] Get this fenugreek extract and dissolve it with deionized water earlier, after extracting 10 times with sherwood oil, collect the lower layer liquid and extract 10 times with ethyl acetate again, obtain ethyl acetate extract, 60 ℃, reduce under the condition of 0.07MPa Pressure evaporated to dryness to obtain 510 mg of sample A to be separated, figure 1 -A is the HPLC figure of sample A to be separated;

[0070] 2) Preparation by high-speed countercurrent chromatography:

[0071] High-speed countercurrent chromatog...

Embodiment 2

[0096] 1) Preparation of samples to be separated

[0097] Take 10g of mature and dry seeds of wild or cultivated fenugreek plants, cut or crush them, pass through a 60-mesh sieve, and extract them ultrasonically in 80mL of 60% ethanol aqueous solution at an extraction temperature of 80°C and an ultrasonic power of 120W. 2 times, each 1h, combined and concentrated to obtain the fenugreek extract with a solid content of 45%;

[0098] Take the fenugreek extract and dissolve it with deionized water first, then extract it with petroleum ether for 5 times, collect the lower layer liquid and extract it with ethyl acetate for 5 times to obtain the ethyl acetate extract, and reduce it under the conditions of 50°C and 0.08Pa Evaporate under pressure to obtain 430 mg of sample A to be separated;

[0099] 2) Preparation by high-speed countercurrent chromatography:

[0100] High-speed countercurrent chromatography (Shanghai Tongtian Biochemical Co., Ltd.) was used to separate and prepare...

Embodiment 3

[0109] 1) Preparation of samples to be separated

[0110] Take 10 g of mature and dry seeds of wild or cultivated fenugreek plants, cut or crush them, pass through a 40-mesh sieve, and microwave-assisted in 50 mL of 75% ethanol aqueous solution at an extraction temperature of 70 °C and a microwave power of 500 W. Extract 1 time, 90s each time, combine and concentrate to obtain the fenugreek extract with a solid content of 51%;

[0111] Take the fenugreek extract and dissolve it with deionized water first, then extract it twice with petroleum ether, collect the lower layer liquid and then extract it twice with ethyl acetate to obtain the ethyl acetate extract. Evaporate to dryness under reduced pressure to obtain 420 mg of sample A to be separated;

[0112]2) Preparation by high-speed countercurrent chromatography:

[0113] High-speed countercurrent chromatography (Shanghai Tongtian Biochemical Co., Ltd.) was used to separate and prepare deoxyrhein, emodin, orientin, vitexin,...

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Abstract

The invention discloses a method for preparing a flavonoid glycoside and stibene glucoside type compound by separating from fenugreek. By virtue of a high-speed countercurrent chromatography (HSCCC) separation technology, isomerides such as vitexin and isovitexin and stibene glucoside type compounds such as rhaponticin, deoxyrhapontin and rhapontigenin which have the similar polarity to that of the isomerides in the fenugreek are subjected to separation preparation, so that the separation time is effectively shortened, and the shortcomings of complicated operation, sample die-adsorption loss, low yield and the like of the conventional preparation method are overcome. According to the method, the technology is simple, the reproducibility is high, and the separation efficiency is high; the obtained monomer content is higher than 96.0 percent and can meet the requirements of a type of botanical drugs and standard contrasts; and the method is suitable for industrial production of medical medicines, standard substances, health protection food, health protection medicines and the like.

Description

technical field [0001] The invention relates to a method for separating and preparing natural medicines, in particular to a method for separating and preparing flavonoid glycosides and stilbene glycosides from fenugreek. Background technique [0002] Fenugreek (Trigonella foenum-graecum L.) is an annual herbaceous plant belonging to the genus Fenugreek of the Papilionaceae subfamily of Fabaceae. Its dried and mature seeds are included in the Pharmacopoeia of the People's Republic of China as a commonly used traditional Chinese medicine. Studies have shown that fenugreek contains a large amount of flavonoid active substances, which have the effects of lowering blood sugar, blood fat and anti-oxidation. Stilbene glycosides, also known as stilbene polyphenols, have various physiological activities and medicinal values ​​such as lowering blood fat, anti-aging, and inhibiting tumors. With the in-depth development of the pharmacological activities of flavonoid glycosides and stil...

Claims

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Application Information

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IPC IPC(8): C07H15/203C07H1/08C07C43/23C07C41/38C07D407/04
Inventor 王洪伦何彦峰王小艳索有瑞
Owner 湖州藏源生物科技有限公司
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