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Preparation method of dieckol

A technology of carbon dioxide and extraction, applied in the production of bulk chemicals, organic chemistry, etc., can solve the problems of less research on dikelminol, and achieve the effects of easy industrialization, good separation effect, and reduced dissolution

Inactive Publication Date: 2013-12-18
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are few domestic researches on dikelminol, and it is still in its infancy.

Method used

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  • Preparation method of dieckol

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Experimental program
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Effect test

Embodiment 1

[0025] Grind the dried kelp, 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, and the ultrasonic frequency is 45KHz, extract 3 times, Filter each time for 1 hour, combine the extracts, add the extracts to a hollow polyethersulfone ultrafiltration membrane with a molecular weight cut-off of 5000 for ultrafiltration, and concentrate the permeate with a tubular polyethersulfone reverse osmosis membrane to obtain a concentrated solution with a concentration of 3 % gelatin solution, stir until no precipitation occurs, centrifuge, dissolve the precipitate with 70% acetone aqueous solution, filter out the gelatin to obtain a preliminary purified solution, put it on a 1LAB-8 macroporous resin column, and elute with 4L of water after the adsorption is completed , then elute with 4L60% ethanol solution, control the flow rate to be 3.5ml / min,...

Embodiment 2

[0027] Crush the dried kelp, 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 60% ethanol solution to the residue for ultrasonic extraction, and extract twice at an ultrasonic frequency of 65KHz. Filter each time for 1 hour, combine the extracts, add the extracts to ultrafiltration with a roll-type polypropylene ultrafiltration membrane with a molecular weight cut-off of 8000, and concentrate the permeate with a roll-type polyvinylidene fluoride reverse osmosis membrane to obtain a concentrated solution, adding a concentration of 6% gelatin solution, stir until no precipitation occurs, centrifuge, dissolve the precipitate with 90% acetone aqueous solution, filter out the gelatin to obtain a preliminary purified solution, put it on a 1LAB-8 macroporous resin column, and wash it with 5L of water after the adsorption is completed Remove, then elute with 5L60% ethanol solution, control the flow r...

Embodiment 3

[0029] Grind the dried kelp, 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 60% ethanol solution to the residue for ultrasonic extraction, the ultrasonic frequency is 50KHz, and extract twice, Each time, filter for 0.5h, combine the extracts, add the extracts to ultrafiltration with a hollow polyethersulfone ultrafiltration membrane with a molecular weight cut-off of 10000, and concentrate the permeate with a hollow membrane polyethersulfone reverse osmosis membrane to obtain a concentrate, adding a concentration of 5% gelatin solution, stir until no precipitation occurs, centrifuge, dissolve the precipitate with 80% acetone aqueous solution, filter out the gelatin to obtain a preliminary purified solution, put it on a 1LADS-17 macroporous resin column, and wash it with 3L of water after the adsorption is completed Then, use 6L60% ethanol solution to elute, control the flow rate to be 3.5ml...

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Abstract

The invention discloses a preparation method of dieckol. The method uses laminaria as a raw material. The technical process mainly comprises the following steps: (1) extracting oil substances from a laminaria drug in an supercritical carbon dioxide fluid extraction mode, and carrying out ultrasonic extraction to obtain an extracting solution; (2) ultrafiltering the extracting solution through an ultrafiltration membrane system, and concentrating the permeation solution with a reverse osmosis membrane; (3) adding a gelatin water solution into the concentrated solution, centrifuging, dissolving the precipitate in an acetone water solution, and filtering out the gelatin to obtain a primary purified solution; (4) purifying through a macroporous resin, eluting with water and an ethanol water solution, and concentrating the eluate; (5) separating the concentrated solution by preparative liquid chromatography to obtain the dieckol. The preparation method is carried out at 50 DEG C, thereby avoiding chemical and structural changes of active components caused by overhigh temperature in the conventional hot reflux extraction process; and therefore, the method can obtain high-purity dieckol, and the dieckol content in the product is higher than 98%. The method has the advantages of short extraction period and high safety, and is suitable for industrial production. The method can lay the foundation for deep research into pharmacological activities and pharmaceutical preparations of tannin components.

Description

technical field [0001] The invention relates to a preparation method of active ingredients of traditional Chinese medicine, in particular to a method for preparing dikelnbucol from kelp. Background technique [0002] Dieckol is a tannin compound isolated from the alariaceae (Alariaceae) kombu Ecklonia kukrome Okamura, with the molecular formula C 36 h 22 o 18 , the molecular weight is 743.55, and the structural formula is [0003] [0004] Pharmacological studies have shown that kelpmol has anti-fibrinolysis, and its IC50 for α2-macroglobulin and α2-plasmin inhibitors are 5.0μg / mL and 0.8μg / mL, respectively. [0005] At present, there are few domestic researches on kelpinkol, which is still in its infancy. Therefore, it is very necessary to develop a method for preparing kelpmol, which is of great significance for expanding the source of medicine and the comprehensive utilization of kelp. Contents of the invention [0006] The technical problem to be solved by the ...

Claims

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Application Information

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IPC IPC(8): C07D319/24
CPCY02P20/54
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH