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Preparing method for chlorogenic acid and similar compounds thereof

A compound, the technology of chlorogenic acid, applied in the field of medicine and chemical industry, can solve the problems of high cost, expensive equipment and materials, etc., and achieve the effect of simple method, low cost, high yield and purity

Active Publication Date: 2016-10-12
JIANGSU TIANSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] At present, chlorogenic acid and its analogues are extracted by lime mercaptan method, water extraction and alcohol precipitation method, ultrasonic method, polyamide column chromatography, etc., and then further purified by different column chromatography, but the obtained compound The purity is generally around 70%. If you want a compound with a higher purity (≧95%), you generally need to prepare a liquid phase, but the equipment and materials required are expensive, and the cost will increase a lot

Method used

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  • Preparing method for chlorogenic acid and similar compounds thereof

Examples

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Effect test

Embodiment 1

[0032] Add 10 kg of dried honeysuckle to 85% ethanol with a concentration of 6 times the weight of honeysuckle, reflux extraction at 85°C for 3 hours, repeat the extraction of the filter residue once after filtering, and combine 155 L of extracts; Concentrate to an extract at ℃; then dissolve the extract in water 3 times the weight of the extract, extract with ethyl acetate after dissolving to obtain an ethyl acetate extract, and concentrate the extract to 0.3 times the original extract, to obtain a concentrated solution; then use 0.1mol·L -1 Adjust the pH value of the concentrated solution to neutral with NaOH, pass through a D-101 macroporous resin column after filtration, then wash the macroporous resin column with 70% ethanol, combine the effluent and water washes, and concentrate at 70°C To a paste, dry at 60°C to obtain 325g of light green powder, the content of chlorogenic acid and its similar compounds is 90.1%; take 1g of the concentrated solution and dissolve it in m...

Embodiment 2

[0034] Add 10 kg of dried honeysuckle to 70% ethanol with 8 times the weight of honeysuckle, reflux and extract at 0°C for 2 hours, repeat the extraction of the filtered residue once, and combine 158 L of extracts; extract 70 Concentrate to an extract at ℃; then dissolve the extract in water with 5 times the weight of the extract, extract with ethyl acetate after dissolving to obtain an ethyl acetate extract, and concentrate the extract to 0.15 times the original extract, to obtain a concentrated solution; then use 0.1mol·L -1 Adjust the pH value of the concentrated solution to neutral with NaOH, pass through the NKA-9 macroporous resin column after filtration, then wash the macroporous resin column with 65% ethanol, combine the effluent and water washes, and concentrate at 70°C To a paste, dry at 60°C to obtain 355g of light green powder, the content of chlorogenic acid and its similar compounds is 85.4%; take 1.5g of the concentrated solution and dissolve it in methanol, use...

Embodiment 3

[0036] Add 10 kg of dried honeysuckle to 14 times the weight concentration of honeysuckle in ethanol with a concentration of 65%, reflux extraction at 65°C for 4 hours, repeat the extraction of the filter residue twice, and combine 156 L of extracts; extract 70 Concentrate to an extract at ℃; then dissolve the extract in water with 8 times the weight of the extract, extract with ethyl acetate after dissolving to obtain an ethyl acetate extract, and concentrate the extract to 0.1 times the original extract, to obtain a concentrated solution; then use 0.1mol·L -1 Adjust the pH value of the concentrated solution to neutral with NaOH, pass through the NKA-11 macroporous resin column after filtration, then wash the macroporous resin column with 60% ethanol, combine the effluent and water washings, and concentrate at 70°C To paste, dry at 60°C to obtain 325g of light green powder, the content of chlorogenic acid and its similar compounds is 89.6%; take 2g of the concentrated solutio...

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Abstract

The invention discloses a preparing method for chlorogenic acid and similar compounds thereof. The preparing method comprises the following steps that firstly, reflux extraction is carried out with an extracting agent; secondly, an extracting solution is concentrated into an extract state; thirdly, extract is dissolved and extracted with ethyl acetate; fourthly, the pH value of a concentrated solution obtained after extraction is regulated to be neutral, and filtration with a macroporous resin column is carried out; fifthly, a thin layer preparing plate is used, a spreading agent is selected for spreading, and high-purity chlorogenic acid and similar compounds thereof are obtained through belt scraping, grinding, column filling, washing and concentration drying. The method is clear in flow, simple and low in cost, and the obtained products through purification are good in color and high in yield and purity; besides, the multiple similar compounds of chlorogenic acid are can be obtained at the same time, and a base is provided for wider and more effective application of chlorogenic acid and the similar compounds thereof.

Description

technical field [0001] The invention relates to a preparation method of chlorogenic acid and similar compounds, belonging to the technical field of medicine and chemical industry. Background technique [0002] Chlorogenic acid [0003] [0004] It is a depsipolic acid composed of the caffeoyl group in caffeic acid and the quinic acid group in quinic acid, also known as coffee tannic acid. [0005] Wherein, the structure of caffeoyl is: [0006] , [0007] The structural formula of quinic acid is: [0008] , [0009] The groups represented by R1-R4 in the above-mentioned quinic acid radical structure formula are different, and different chlorogenic acid analogs are formed, such as the following situations: (1) R 1 =R 3 = caffeoyl, R 2 =R 4 = H; (2) R 1 =R 2 = caffeoyl, R 3 =R 4 = H; (3) R 1 =R 3 =R 4 = H, R 2 = caffeoyl; (4) R 1 =R 2 =R 4 = H, R 3 = caffeoyl; (5) R 3 =R 2 = H, R 1 = caffeoyl, R 4 = Me. [0010] Chlorogenic acid and its similar ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/48C07C67/56C07C67/58C07C69/732
CPCC07C67/48C07C67/56C07C67/58C07C69/732
Inventor 季浩胡亚京于燕燕阚建伟孔繁博
Owner JIANGSU TIANSHENG PHARMA
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