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Method for separating kudinoside A and kudinoside D from Ilex kudingcha C.J.Tseng

A technology of Kudingcha holly and Kudingchai, which is applied in the field of saponins, can solve the problems of no clear specific implementation method, small differences in properties, difficult separation, etc. Great prospect and good economical applicability

Inactive Publication Date: 2015-03-11
GUANGZHOU UNIVERSITY OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, patent CN101016328B separates and purifies ursolic acid and oleanolic acid from Kudingcha holly, the adopted method is very complicated, the steps are cumbersome, and the purity is only about 90%; patent CN101775061A adopts 95% ethanol heat reflux to extract , and then extracted with petroleum ether, chloroform and n-butanol to obtain extracts of various parts, repeated normal phase, reversed phase silica gel column chromatography, Sephadex column chromatography separation means to obtain a group of Kudingcha saponins, including Kubutanone A, B, D, E, F, G, Kuding saponin LZ 11 and LZ 12 , does not relate to Kubutin A and Kubutin D targeted by the present invention
The methods reported in the literature all use various organic solvent extractions and various fillers to carry out column chromatography for separation and purification. Not only are there no specific implementation methods for each step, but the required steps are lengthy, cumbersome, time-consuming, and the yield is low (only mg grade), and the purity is low
At present, there is no literature report on the rapid separation and purification of Kudinoside A (Kudinoside A) and Kudinoside D (Kudinoside D) at the same time. The main reason is that the two have similar structures, small differences in properties and difficult separation.

Method used

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  • Method for separating kudinoside A and kudinoside D from Ilex kudingcha C.J.Tseng
  • Method for separating kudinoside A and kudinoside D from Ilex kudingcha C.J.Tseng
  • Method for separating kudinoside A and kudinoside D from Ilex kudingcha C.J.Tseng

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. Separation of Kubutin A and D

[0031] (1) Weigh 500 g of dried Kudingcha holly leaves, crush them through a No. 3 sieve, and extract by percolation with 20 times the amount of methanol (10 L). Recover methanol to obtain Kudingcha Dongqing extract 212g, add 300mL of distilled water to make a dispersion system. First extract with chloroform three times, each time 350mL, and then extract with water-saturated n-butanol three times, each time 350mL. Concentrate the n-butanol extract to a thick paste.

[0032] (2) the gained thick paste is absorbed with 214g macroporous resin, uses 860g macroporous resin as column chromatography filler, washes 6 column volumes with pure water earlier, then uses methanol-water gradient elution (30% → 60% →80%), each gradient eluent is 8-10 column volumes. After TLC analysis, the target compound was collected in the 60% methanol eluent, and the components containing the target compound were combined to recover the solution to obtain 24 g...

Embodiment 2

[0052] 1. Separation of Kubutin A and D

[0053] (1) Weigh 500 g of dried Kudingcha holly leaves, pulverize them through a No. 3 sieve, extract with 8 times the amount (4 L) of ethanol with a mass fraction of 75% under reflux, and extract twice, each time for 60 minutes. Recover the solvent to obtain 233g of Kudingcha Dongqing extract, add 350mL of distilled water to form a dispersion system, first extract three times with chloroform, 400mL each time, and then extract 3 times with water-saturated n-butanol, 400mL each time. Concentrate the n-butanol extract to a thick paste.

[0054] (2) 250g macroporous resin adsorption is mixed sample with gained thick paste, use 900g macroporous resin as filler, carry out column chromatography, elution 6 column volumes with pure water earlier, then use ethanol-water gradient elution ( 25% → 55% → 75%), each gradient elution solution is 8-10 column volumes. After TLC analysis, the target compound was collected in the 55% ethanol eluent, an...

Embodiment 3

[0061] 1. Separation of Kubutin A and D

[0062] (1) Weigh 300 g of dried leaves of Ilex kudingcha, crush them through a No. 3 sieve, extract by percolation with 20 times the amount (6 L) of ethanol with a mass fraction of 80%, and recover the solvent to obtain 126 g of Ilex kudingcha extract. Add 200 mL of distilled water to form a dispersed system, first extract three times with chloroform, 250 mL each time, and then extract three times with saturated n-butanol, 250 mL each time. Concentrate the n-butanol extract to a thick paste.

[0063] (2) The obtained thick paste is adsorbed and mixed with 120g macroporous resin, and 480g of macroporous resin is used as a filler to carry out column chromatography, and eluted with pure water for 6 column volumes, and then ethanol-water gradient elution (25%→55%→75%), each gradient elution solution is 8-10 column volumes. After TLC analysis, the target compound was collected in the 55% ethanol eluent, and the components containing the t...

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Abstract

The invention relates to a method for separating Kudinoside A and Kudinoside D from Ilex kudingcha C.J.Tseng. The method comprises the following steps: using an Ilex kudingcha C.J.Tseng (Ilex kudingcha C.J.Tseng ) medicinal material as a raw material, extracting through an alcohol solution, chloroforming for removing impurities, extracting through n-butyl alcohol, and performing macroporous resin column chromatography and reversed-phase high performance liquid refining separation and recrystallization so as to obtain a high-purity monomeric compound of the Kudinoside A (Kudinoside A) and the Kudinoside D (Kudinoside D). The technical method disclosed by the invention is simple and reliable, raw materials are easy to obtain, the economic cost is low, the purity of the monomeric compound is high, and the method is suitable for large-scale preparation of the kudinoside A and the kudinoside D.

Description

technical field [0001] The present invention relates to saponin compounds, in particular to Kudinoside A (Kudinoside A) and Kudinoside D (Kudinoside D). Background technique [0002] Ilex kudingcha is the dry leaf of Ilex kudingcha C.J.Tseng, a plant of the genus Ilex in the family Ilex (Aquifoliaceae). Kudingcha Dongqing has the effects of dispersing wind and heat, clearing the head, and relieving headaches. It is used for symptoms such as aversion to cold and fever, headache, abdominal pain, nausea and diarrhea caused by exogenous wind and cold in summer months and internal injuries. In my country, it is mainly distributed in Southwest China (Sichuan, Chongqing, Guizhou, Hunan, Hubei) and South China (Jiangxi, Guangdong, Fujian, Hainan) and other places. Modern pharmacological research shows that Kudingcha holly has pharmacological effects such as improving cardiovascular system, lowering blood fat, lowering blood pressure, lowering blood sugar and improving immunity. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00
CPCC07J71/0005
Inventor 赵钟祥杨滔周联向松涛张蕾朱锦萍杨宝谭庆龙
Owner GUANGZHOU UNIVERSITY OF CHINESE MEDICINE
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