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Method for preparing castalagin

A chestnut ellagitannin and supercritical technology, which is applied in the field of chestnut ellagitannin preparation, can solve problems such as less research on chestnut ellagitannin, and achieve the effects of easy industrialization, good separation effect and simple production process.

Inactive Publication Date: 2013-08-21
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, domestic research on ellagitannin from chestnut wood is less, and it is still in its infancy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Crush the stem bark of elm green wood, take 1kg, put it into a supercritical extraction device, extract at a temperature of 35°C and a pressure of 25MPa for 30min, add 8L of 80% ethanol solution to the residue for ultrasonic extraction, the ultrasonic frequency is 45KHz, extract 3 time, each 1h, filter, combine the extracts, concentrate at low temperature, add a gelatin solution with a concentration of 3%, stir until no precipitation occurs, centrifuge, dissolve the precipitate with 50% acetone aqueous solution, filter out the gelatin, and obtain a preliminary purified solution. Put on 1LHPD-400 macroporous resin column, after the adsorption is completed, first elute with 4L water, then elute with 4L70% ethanol solution, control the flow rate at 3.5ml / min, collect the eluate rich in chestnut ellagitin, concentrate , add methanol to the concentrated solution to prepare a clear solution, and use preparative high-performance liquid chromatography to separate. The preparativ...

Embodiment 2

[0024] Crush the stem bark of elm green wood, take 1kg, put it into a supercritical extraction device, extract at a temperature of 45°C and a pressure of 30MPa for 50min, add 10L of 70% ethanol solution to the residue for ultrasonic extraction, the ultrasonic frequency is 65KHz, and extract 2 1 hour each time, filter, combine the extracts, concentrate at low temperature, add a gelatin solution with a concentration of 6%, stir until no precipitation occurs, centrifuge, dissolve the precipitate with 70% acetone aqueous solution, filter the gelatin, and obtain a preliminary purified solution. Put on 1LHPD-400 macroporous resin column, after the adsorption is completed, first elute with 5L of water, then with 5L of 70% ethanol solution, control the flow rate to 4.5ml / min, collect the eluate rich in chestnut ellagitin, concentrate , add methanol to the concentrated solution to prepare a clear solution, and use preparative high-performance liquid chromatography to separate. The prepa...

Embodiment 3

[0026] Crush the bark of elm green wood, take 1kg, put it into a supercritical extraction device, extract at a temperature of 40°C and a pressure of 30MPa for 30min, add 10L of 70% ethanol solution to the residue for ultrasonic extraction, the ultrasonic frequency is 50KHz, and extract 2 time, each time for 0.5h, filter, combine the extracts, concentrate at low temperature, add a gelatin solution with a concentration of 5%, stir until no precipitation occurs, centrifuge, dissolve the precipitate with 70% acetone aqueous solution, filter out the gelatin, and obtain a preliminary purified solution , on a 1LADS-17 macroporous resin column, after the adsorption is completed, first elute with 3L of water, then elute with 6L of 70% ethanol solution, control the flow rate to 3.5ml / min, collect the eluate rich in chestnut ellagitin, Concentrate, add methanol to the concentrated solution to prepare a clear solution, and use preparative high-performance liquid chromatography to separate....

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PUM

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Abstract

The invention discloses a method for preparing castalagin. According to the method, anogeissus barks are used as raw materials. The technical flow of the method mainly comprises four steps of: (1) extracting fat-type substances from anogeissus bark medicinal materials by supercritical carbon dioxide fluid, and performing ultrasonic extraction to obtain an extract; (2) concentrating the extract at a low temperature, adding gelatine solution into the extract, performing centrifugation, dissolving precipitates by acetone aqueous solution, and filtering out gel to obtain preliminarily purified liquid; (3) purifying the preliminarily purified liquid by macroporous resin, eluting the preliminarily purified liquid by water and ethanol water, and concentrating the eluant; and (4) carrying out preparative liquid chromatography separation on the concentrated liquid to obtain castalagin, thus obtaining the castalagin. The preparation method is executed at the temperature being less than 50 DEG C; the chemical and structural changes of active components caused by overhigh temperature in the conventional thermal backflow extraction process are avoided; therefore, by the method, castalagin with higher purity can be obtained; castalagin content of a product is over 95 percent; the method is short in extraction period, safe and suitable for industrial production; and the method lays a foundation for deep research on the pharmacological activity and pharmaceutic preparations of tannin type components.

Description

technical field [0001] The invention relates to a preparation method of active ingredients of traditional Chinese medicines, in particular to a method for preparing chestnut ellagitannin from bark and fruit of elm tree bark. Background technique [0002] Chestnut ellagitann (Castalagin), is a variety of elm green wood from the Combretaceae (Combretaceae) Anogeissus acuminata (Roxb. ex DC.) Guill. & Pers. var. lanceolata A tannin compound isolated from the stem of Wall.ex C.B.Clarke, which is off-white powder with the molecular formula C 19 h 18 o 4 , the molecular weight is 934.34, and the structural formula is [0003] . [0004] Pharmacological studies have shown that chestnut ellagitannin has antihypertensive activity, and intravenous injection of this product can reduce the blood pressure of spontaneously hypertensive rats, which is due to the inhibition of sympathetic nerve activity and direct expansion of blood vessels; it has cytotoxic activity and is effecti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/22
CPCY02P20/54
Inventor 苏刘花万冬梅
Owner NANJING ZELANG AGRI DEV