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Disaccharide compound and separation and purification method thereof

A technology for separation and purification of compounds, which is applied in the field of disaccharide compounds and their separation and purification, can solve the problems of unfavorable compound drug efficacy research and application, high production cost of disaccharide compounds, no compound standard products, etc., to achieve cost reduction and extraction time Short, energy-reducing effect

Inactive Publication Date: 2012-03-28
LUZHOU MEDICAL COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, the extraction time is long, and Rhodiola rosea needs to be used as a raw material. Due to the relatively high price of Rhodiola rosea, the production cost of the disaccharide compound is high, which is not conducive to further drug effect research and Application in the actual production process; and, in this method, the use of toxic and strong solvents (such as tetrachloromethane, acetonitrile) in many places makes the production and use of this product have certain dangers
[0009] At present, there is no relevant report about the existence of this compound in other plants, and there is no report about the preparation of a standard product of this compound

Method used

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  • Disaccharide compound and separation and purification method thereof
  • Disaccharide compound and separation and purification method thereof
  • Disaccharide compound and separation and purification method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1 The separation and purification method of formula 1 compound of the present invention

[0028] 10kg of coarse powder of Radix isatidis, soaked in 65% ethanol for 1 hour, and refluxed for 3 times, 1 hour each time. The extracts were combined, ethanol was recovered under reduced pressure until there was no alcohol smell, vacuum-dried at 50° C., and pulverized to obtain 1390 g of dry extract powder of the crude extract, with a yield of 13.9%. Take 500g of crude extract dry extract powder and extract with 95% ethanol under reflux for 3 times, each time for 1 hour, filter, combine the extracts, recover ethanol under reduced pressure until there is no alcohol smell, dry in vacuum at 50°C, and crush to obtain Radix Radix dry infusion Paste powder 140g, the yield is 3.9%.

[0029] The dry extract powder of Radix isatidis was separated by dry column chromatography on a silica gel column, eluted with dichloromethane-methanol (100:0-1:1) gradient, checked by thin-lay...

Embodiment 2

[0033] Embodiment 2 The separation and purification method of the compound of formula 1 of the present invention

[0034] 10kg of coarse powder of Radix isatidis, soaked in 65% ethanol for 1 hour, and refluxed for 3 times, 1 hour each time. The extracts were combined, ethanol was recovered under reduced pressure until there was no alcohol smell, vacuum-dried at 50° C., and pulverized to obtain 1390 g of dry extract powder of the crude extract, with a yield of 13.9%. Take 500g of crude extract dry extract powder and extract with 80% ethanol under reflux for 3 times, each time for 1 hour, filter, combine the extracts, recover ethanol under reduced pressure until there is no alcohol smell, vacuum dry at 50°C, and pulverize to obtain Radix Radix dry infusion Paste powder 172g, the yield is 4.8%.

[0035] The dry extract powder of Radix isatidis was separated by dry column chromatography on a silica gel column, eluted with dichloromethane-methanol (100:0-1:1) gradient, checked by ...

Embodiment 3

[0036] Embodiment 3 The separation and purification method of the compound of formula 1 of the present invention

[0037]10kg of coarse powder of Radix isatidis, soaked in 50% ethanol for 1 hour, and refluxed for 3 times, 1 hour each time. The extracts were combined, the ethanol was recovered under reduced pressure until there was no alcohol smell, vacuum-dried at 50° C., and pulverized to obtain 1560 g of dry extract powder of the crude extract, with a yield of 15.6%. Take 500g of crude extract dry extract powder and extract with 95% ethanol under reflux for 3 times, each time for 1 hour, filter, combine the extracts, recover ethanol under reduced pressure until there is no alcohol smell, vacuum dry at 50°C, and crush to obtain Radix Radix dry infusion Paste powder 168g, the yield is 5.2%.

[0038] The dry extract powder of Radix isatidis was separated by dry column chromatography on a silica gel column, eluted with dichloromethane-methanol (100:0-1:1) gradient, checked by t...

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Abstract

The invention provides a compound. The structural formula of the compound is shown as the formula I, and the purity of the compound is over 95 percent. The invention also provides a new separation and purification method for the compound shown as the formula I. Isatis roots are used for substituting relatively expensive rhodiola kirilowii in the method, so that the cost of the raw materials is greatly reduced; the compound with high purity and high yield is prepared by a specific extracting solvent and an extracting method, and the prepared compound can be used as a standard substance; compared with the conventional separation and purification method, the method has the advantages that: the extraction time is short, the energy consumption is reduced, and the production cost is further reduced; and because the conventional solvent is adopted in the whole preparation process, toxic solvents such as tetra-chloromethane and acetonitrile and the like are saved, and the safety of the production process and the product is improved.

Description

technical field [0001] The invention relates to a disaccharide compound and a separation and purification method thereof. Background technique [0002] Disaccharides are formed by two molecules of monosaccharides through glycosidic bonds. After hydrolysis, two monosaccharide molecules can be formed. Naturally occurring free and functional sugars are represented by lactose in mammals, trehalose in bacteria and insect blood, and plant sucrose. They are used as energy sources for various organisms, or as raw materials for organisms. [0003] Common disaccharides include lactose, maltose, and sucrose. Among them, sucrose is formed from a molecule of glucose and a molecule of fructose. After entering the human body, it is decomposed into glucose and fructose to provide energy for the human body. [0004] At present, another disaccharide compound similar to sucrose structure is found, which is also formed by condensation of one molecule of fructose and one molecule of glucose, th...

Claims

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Application Information

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IPC IPC(8): C07H3/04C07H1/08
Inventor 孙琴张丹陈斯玮彭腾刘明华张诗静姜黎胡晓燕
Owner LUZHOU MEDICAL COLLEGE
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