Method for extracting qingdainone from isatis tinctoria

A technology of indigo and woad, which is applied in the field of medicine to achieve the effects of improving purity, increasing extraction rate, and saving solvents

Inactive Publication Date: 2012-02-15
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For above-mentioned situation, the purpose of the present invention is to provide a kind of method of extracting indigo from woad, can effectively solve the problem of extracting indigo from woad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Grind the stems and leaves of Isatis indigo, weigh 1000g, add 95% methanol solution equivalent to three times the amount of raw materials, soak for 2 hours, then heat to 84°C for Soxhlet extraction for 6 hours, collect the extract and take the liquid to recover methanol under reduced pressure until there is no alcohol smell. Add water to dissolve and disperse, centrifuge, put the supernatant on the HZ841 macroporous adsorption resin column, first flush the column with 20% ethanol solution until the eluate flows out colorless, then elute with 60% ethanol solution, collect the 60% ethanol eluate, Concentrate under reduced pressure, extract repeatedly 6 times with diethyl ether, and concentrate and dry the extract to obtain the crude product of Qingdanone. Dissolve the crude Qingdan ketone in methanol, filter it through a microporous membrane, and separate it by preparative high-performance liquid chromatography. Chromatographic column: C18, mobile phase: acetonitrile-water...

Embodiment 2

[0016] Crush the stems and leaves of Isatis indigo, weigh 1000g, add 75% ethanol solution equivalent to 5 times the amount of raw materials, soak for 2 hours, then heat to 93°C for Soxhlet extraction for 8 hours, collect the extract and take the liquid to recover ethanol under reduced pressure until it has no alcohol smell. Add water to dissolve and disperse, centrifuge, put the supernatant on a carboxymethyl-type weakly acidic cationic resin column, first wash the column with water until the eluate flows out colorless, then elute with 5% ammonia water by volume, collect the ammonia water eluate, Concentrate under reduced pressure, extract repeatedly 5 times with diethyl ether, concentrate and dry the extract to obtain crude Qingdan ketone. Dissolve the crude Qingdan ketone in methanol, filter it through a microporous membrane, and separate it by preparative high-performance liquid chromatography. Chromatographic column: C18, mobile phase: acetonitrile-water (60:40), flow rate ...

Embodiment 3

[0018] Grind the stems and leaves of Isatis indigo, weigh 1000g, add 60% methanol solution equivalent to 4 times the amount of raw materials, soak for 1h, then heat to 85°C for Soxhlet extraction for 10h, collect the extract and take the liquid to recover methanol under reduced pressure until there is no alcohol smell. Add water to dissolve and disperse, centrifuge, put the supernatant on D101 macroporous adsorption resin column, first flush the column with 10% ethanol solution until the eluate flows out colorless, then elute with 80% ethanol solution, collect 75% ethanol eluate, Concentrate under reduced pressure, extract repeatedly 3 times with ether, and concentrate and dry the extract to obtain the crude product of Qingdanone. Dissolve the crude Qingdan ketone in methanol, filter it through a microporous membrane, and separate it by preparative high-performance liquid chromatography. Chromatographic column: C18, mobile phase: acetonitrile-water (62:38), flow rate 50ml / min, ...

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PUM

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Abstract

The invention provides a method for extracting qingdainone from isatis tinctoria, which comprises the following steps of: crushing isatis tinctoria leaves, adding a proper amount of methanol or ethanol solution for carrying out Soxhlet extraction, concentrating the extracted liquid until the concentration liquid does not have the alcohol flavor, using a macroporous adsorption resin column or a cation resin column for primary separation, adopting eluent for concentration, adopting diethyl ether for extraction, concentrating and drying the extracted liquid to obtain qingdainone crude products and then preparing efficient liquid for carrying out phase separation to obtain the qingdainone. The method has the advantages that the process is simple, the yield is high, the product quality is good, and the purity is high.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for extracting indigo from woad. Background technique [0002] Woad, Latin plant name: Isatis indigotica Fortune , Alias: tea blue, isatis root, big green leaf. Nature and flavor: bitter in the mouth, cold in nature. Return through: return liver; Stomach meridian. Function: heat-clearing and toxic substances removing, cooling blood and eliminating spots. Indications: used for febrile disease fever, spots, wind-heat cold, sore throat. Erysipelas, Japanese encephalitis, hepatitis and mumps embolism. Mainly distributed in Inner Mongolia, Shaanxi, Gansu, Hebei, Shandong, Jiangsu, Zhejiang, Anhui, Guizhou and other places. [0003] Qingdanone, dark purple fine needle crystals, indole alkaloids, chemical number: 97457-31-3, molecular formula: C 23 h 13 N 3 o 2 , molecular weight: 363.38. Derived from the stems and leaves of Isatis indigo, it has antitumor activity. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
Inventor 刘东锋吴艳波
Owner NANJING ZELANG MEDICAL TECH
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