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Method for preparing corilagin through matsumura leafflower herb

A technology of citrus and equipment, applied in the field of medicine, can solve the problems of large amount of entrainer, large one-time investment and high selectivity, and achieve the effects of product quality protection, saving ethanol consumption and reducing energy consumption.

Inactive Publication Date: 2012-01-25
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese Patent (Application No. 201010535378.3) "A Preparation Method for Curry Latin" discloses that supercritical CO 2 Extraction, the extract is dissolved in water, filtered, the filtrate is adsorbed by a macroporous adsorption resin, ethanol is eluted, the eluate is concentrated, and then acetic acid is added to adjust the pH, and the mixed solvent of ethyl acetate-water with a ratio of 10:2 is used for 6-10 Stage countercurrent extraction, combined extracts, solvent recovery under reduced pressure, adding absolute ethanol to crystallize, and drying to obtain Corilagin. This method has a large one-time investment in equipment, high selectivity, low extraction rate, and a large amount of entraining agent. Not easy to recycle

Method used

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  • Method for preparing corilagin through matsumura leafflower herb

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Grind the citrus citrus medicinal material, take 2kg and put it into a Soxhlet extraction tank, add 50% ethanol solution 3 times the amount of the raw material, soak for 1 hour, then put it into the neat heating to 85°C, extract for 4 hours, and add the extract with a molecular weight cut-off of 6000 The roll-type polyvinylidene fluoride ultrafiltration membrane is used for ultrafiltration, and the permeate is added to the roll-type polyvinylidene fluoride reverse osmosis membrane to concentrate, the concentrated solution is adjusted to pH 5.0, extracted 3 times with ethyl acetate, and the extract is concentrated to a small volume spare. Take methyl tert-butyl ether, n-butanol, acetonitrile, and 0.1% trifluoroacetic acid, mix them in a ratio of 16:8:16:38, let stand and separate, the upper phase is the stationary phase, the lower phase is the mobile phase, and the stationary phase is taken. The phase is pumped into the high-speed countercurrent chromatographic column, s...

Embodiment 2

[0020] Grind the citrus citrus medicinal material, take 2kg and put it into a Soxhlet extraction tank, add 40% ethanol solution 5 times the amount of the raw material, soak for 0.5 hours, then put it into neat heating to 90°C, extract for 6 hours, add the extract with a molecular weight cut-off of 10000 The tubular polypropylene ultrafiltration membrane is used for ultrafiltration, and the permeate is added to the tubular polypropylene reverse osmosis membrane to concentrate, the concentrated solution is adjusted to pH 4.3, extracted three times with ethyl acetate, and the extract is concentrated to a small volume for later use. Take methyl tert-butyl ether, n-butanol, acetonitrile, and 0.1% trifluoroacetic acid, mix them in a ratio of 15:8:14:36, let stand and separate, the upper phase is the stationary phase, the lower phase is the mobile phase, and the stationary phase is taken. The phase is pumped into the high-speed countercurrent chromatographic column, start the main eng...

Embodiment 3

[0022] Grind the citrus citrus medicinal material, take 5kg and put it into a Soxhlet extraction tank, add 60% ethanol solution of 6 times the amount of raw materials, soak for 2 hours, then put it into neat heating to 80°C, extract for 3 hours, add the extract with a molecular weight cut-off of 5000 The tubular polyethersulfone ultrafiltration membrane is used for ultrafiltration, the permeate is added to the tubular polyethersulfone reverse osmosis membrane to concentrate, the concentrated solution is adjusted to pH 4.0, extracted twice with ethyl acetate, and the extract is concentrated to a small volume for later use. Take methyl tert-butyl ether, n-butanol, acetonitrile, and 0.1% trifluoroacetic acid, mix them in a ratio of 13:6:15:33, let them stand and separate, the upper phase is the stationary phase, and the lower phase is the mobile phase. The phase is pumped into the high-speed countercurrent chromatographic column, start the main engine, adjust the speed to 900rpm, ...

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Abstract

The invention discloses a method for preparing corilagin through a matsumura leafflower herb. The method comprises the steps of: crushing a matsumura leafflower herb medicinal material; performing Soxhlet extraction by adding 40-60 percent of ethanol; filtering an extracted solution; ultra-filtering by adding an ultra-filtration membrane system; concentrating a liquid permeating the ultra-filtration membrane system through a reverse osmosis membrane to obtain a concentrated liquid; regulating the pH value of the concentrated liquid to be pH 4-5; extracting through ethyl acetate; separating through a high-speed countercurrent chromatography after concentrating an extract liquid; collecting target components according to a chromatogram of an ultraviolet detector; and drying at a low temperature to obtain a product. By adopting the method for producing the corilagin, the energy consumption is low, the yield rate is high, and the product content is high.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for preparing corilagin from citrus citrus. Background technique [0002] Corilagin (Corilagin), also known as myrobalan subtannin, vermiculite, etc., the chemical name is 1-O-galloyl-3,6-O-hexahydroxybiphenyldiformyl-β-D-glucose, Molecular formula: C 27 h 22 o 18 ; Molecular weight: 634.453, CAS accession number: 23094-69-1, molecular structure formula is as follows: [0003] [0004] Corilagin is a water-soluble inverse gallate tannin that can be extracted from many plants, and widely exists in a variety of plants, such as Citrus phyllophylla and Citrus citrus, Yak Ermiao, Geranium Plants of the genus Grass, Euphorbia, Amaranth, Pomegranate, Acer and Terminalia, etc. Studies in recent years have shown that Corilagin has antihypertensive activity, anti-HBV activity, and antithrombotic activity. Some Japanese patents disclose that Corilagin can incre...

Claims

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Application Information

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IPC IPC(8): C07H13/08C07H1/08
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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