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Once preparation method of composite of 17-hydrogen-9-dehydro-andrographolidume-3-sodium (or potassium) disulfate and 17-hydrogen-9-dehydro-andrographolidume-19-sodium (or potassium) disulfate, and purposes of medicine prepared by the same

A technology of andrographolide, sodium sulfate, applied in 17-hydro-9-dehydroandrographolide-3-sulfate sodium (or potassium), 17-hydro-9-dehydroandrographolide-19- The one-time preparation of the sodium sulfate (or potassium) composition and the field of its pharmaceutical use can solve the problems of difficulty in preparing liquid preparations, restricting production efficiency, complicated production processes, etc., to ensure pharmacological activity, the preparation method is simple and convenient, and the water solubility is good. Effect

Inactive Publication Date: 2013-06-19
JIANGZI QINGFENG PHARMACEUTICALS INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, oral preparations are usually made into tablets, capsules, dripping pills, and soft capsules; because andrographolide is insoluble in water, it brings difficulties to the preparation of liquid preparations
[0005] In the prior art, there is no particularly effective and suitable preparation method for extracting active ingredients in actual production, especially when two active ingredients need to be used together to form a composition, they can only be extracted separately, and then mixed in proportion to produce The process is complicated and the production cost is high, which seriously restricts the production efficiency

Method used

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  • Once preparation method of composite of 17-hydrogen-9-dehydro-andrographolidume-3-sodium (or potassium) disulfate and 17-hydrogen-9-dehydro-andrographolidume-19-sodium (or potassium) disulfate, and purposes of medicine prepared by the same
  • Once preparation method of composite of 17-hydrogen-9-dehydro-andrographolidume-3-sodium (or potassium) disulfate and 17-hydrogen-9-dehydro-andrographolidume-19-sodium (or potassium) disulfate, and purposes of medicine prepared by the same
  • Once preparation method of composite of 17-hydrogen-9-dehydro-andrographolidume-3-sodium (or potassium) disulfate and 17-hydrogen-9-dehydro-andrographolidume-19-sodium (or potassium) disulfate, and purposes of medicine prepared by the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Take andrographolide, add 5.5 times the amount of acetic anhydride (62%) and glacial acetic acid (38%) to dissolve, while stirring, slowly add 4.5 times the amount of sulfuric acid at a rate of 1.6ml per minute of 1g andrographolide (52%) and glacial acetic acid (48%), mix well, adjust the temperature of the reactor at 16°C, and place it for 90 minutes to sulfonate. Add the same amount of purified water, stir well, adjust the pH to about 7.0 with 33% NaOH, add 95% ethanol to make the alcohol content more than 82%, recover the ethanol under reduced pressure, and separate the aqueous solution by macroporous adsorption resin and ODS column chromatography. Elute with a gradient of water:ethanol, the ratio of water is 80-20%, and the ratio of ethanol is 20-80%. Collect the eluate in sections, combine the same components, and crystallize to obtain 17-hydro-9-dehydroandrographis Sodium lactone-3-sulfate, its sodium salt molecular formula C 20 H 29 NaO 8 S, molecular weight: 452...

Embodiment 2

[0071] Take andrographolide, add 5.6 times the amount of acetic anhydride (60%) and glacial acetic acid (40%) to dissolve it, while stirring, slowly add 4.5 times the same amount of sulfuric acid at a rate of 2.0 ml per minute of 1g andrographolide Mix well with glacial acetic acid, adjust the temperature of the reactor at 18°C, and let it stand for 100 minutes to sulfonate. Add the same amount of purified water, stir well, adjust the pH to about 7.0 with 36% NaOH, add 95% ethanol to make the alcohol content more than 82%, recover the ethanol under reduced pressure, and separate the aqueous solution by macroporous adsorption resin and ODS column chromatography. Elute with a gradient of water: ethanol, the ratio of water is 80-20%, the ratio of ethanol is 20-80%, collect the eluent components, combine the same components, and crystallize to obtain 17-hydro-9-dehydroandrographis Sodium lactone-19-sulfate, the molecular formula of its sodium salt: C 20 H 29 NaO 8 S, molecular weig...

Embodiment 3

[0079] Take andrographolide, add 5.5 times the amount of acetic anhydride (60%) and glacial acetic acid (40) to dissolve, while stirring, add 3.5 times the amount of sulfuric acid (52%) at a rate of 2.1ml per minute for 1g andrographolide Mix well with glacial acetic acid (48%), adjust the temperature of the reaction kettle at 17°C, place for 80 minutes to sulfonate, and pour the reactants into saturated potassium chloride solution to obtain 17-hydro-9-dehydroandrographolide- 3-potassium sulfate, 17-hydro-9-dehydroandrographolide-19-potassium sulfate and other mixed solutions are concentrated under reduced pressure and dried in vacuum to obtain a mixture. The mixture is dissolved in a small amount of water and passed through a Sephadex LH-20 column. The loading ratio of the mixture to Sephadex LH-20 is 1:7, and the column diameter to height ratio of Sephadex LH-20 is 1:28. Elute with 3 times the column volume of water, discard the eluent, and use 25% ethanol for 6 times the colu...

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Abstract

The invention relates to a composite of 17-hydrogen-9-dehydro-andrographolidume-3-sodium ( or potassium) disulfate and 17-hydrogen-9-dehydro-andrographolidume-19-sodium (or potassium) disulfate, and discloses components of the composite, and a once preparation method of the components. The composite can be used for preparing medicine having antipyretic, anti-inflammatory and antiviral purposes. The composite is made into dosage forms which can be accepted pharmaceutically.

Description

Technical field [0001] The present invention relates to a combination of 17-hydro-9-dehydroandrographolide-3-sulfate sodium (or potassium), 17-hydro-9-dehydroandrographolide-19-sulfate sodium (or potassium) The preparation method and its use for preparing medicine. Background technique [0002] Andrographis paniculata is the dry aerial part of Andrographi spaniculata (Burm.f.) Nees. The chemical composition and pharmacological experiments show that the active ingredients of Andrographis paniculata are mainly diterpenoids represented by andrographolide [National Chinese Medicine Administration. Chinese Materia Medica·Volume 7. Shanghai: Shanghai Science and Technology Press, 1999:439], the structure of andrographolide is: [0003] [0004] Molecular formula: C 20 H 30 O 5 , It is a colorless square crystal, m.p.230-232℃, [α] 0 20 -126°(c0.2, H 2 O). Very bitter taste, soluble in methanol, ethanol, propanol, pyridine, slightly soluble in chloroform, ether, insoluble in water and pe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/58A61K31/365A61P29/00A61P31/04A61P31/12A61P31/16
Inventor 唐春山吕武清杨小玲刘地发李志勇程帆
Owner JIANGZI QINGFENG PHARMACEUTICALS INC
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