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

A technology of andrographolide, sodium sulfate, applied in 17-hydro-9-dehydroandrographolide-3-sulfate sodium (or potassium), 17-hydro-9-dehydroandrographolide-3, The one-time preparation of the 19-disulfate sodium (or potassium) composition and the field of its pharmaceutical use can solve the problems of restricted production efficiency, high production cost, complicated production process, etc., and achieve simple and convenient preparation method, high productivity and good water solubility. Effect

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

AI Technical Summary

Problems solved by technology

[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 t

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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0063] Example 1

[0064] 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, mol...

Example Embodiment

[0071] Example 2

[0072] Take andrographolide, add 5.3 times the amount of acetic anhydride (62%) and glacial acetic acid (38%) to dissolve it, while stirring, slowly add 4.3 times the amount of 1g andrographolide at a rate of 2.2ml per minute. Mix the glacial acetic acid with sulfuric acid, adjust the temperature of the reactor at 15℃, place for 90 minutes to sulfonate, add the same amount of purified water, then pour into saturated sodium chloride solution, and then pass the macroporous adsorption resin, ODS column chromatography Separate, elution with a gradient of water: ethanol, the ratio of water is 80-20%, the ratio of ethanol is 20-80%, collect the eluate in sections, combine the same components, and crystallize to obtain 17-hydrogen-9-de Hydroandrographolide-3,19-disulfate sodium, its sodium salt molecular formula: C 20 H 28 Na 2 O 11 S 2 , Molecular weight: 554.

[0073] Example of reaction formula:

[0074]

[0075] The physical and chemical properties and spectral data...

Example Embodiment

[0079] Example 3

[0080] Take andrographolide, add 6.0 times the amount of acetic anhydride (58%) and glacial acetic acid (42%) to dissolve it. Under stirring, pass in 1.3 liters of 1.4% sulfur trioxide at a rate of 0.07 liters per minute of 1g andrographolide , Adjust the temperature of the reactor at 17°C, and place it for 100 minutes to sulfonate. Add the same amount of purified water, stir well, adjust the pH to about 7.0 with 45% KOH, add 95% ethanol to make the alcohol content above 85%, filter, the filtrate is decompressed to recover the ethanol, and vacuum-dried to obtain 17-hydrogen-9 -Dehydroandrographolide-3-potassium sulfate, 17-hydro-9-dehydroandrographolide-3,19-disulfate potassium and other mixtures, the mixture is dissolved in a small amount of water, and the mixture is passed through a Sephadex LH-20 column. The ratio of sample load to Sephadex LH-20 is 1:5.5, and the column diameter to height ratio of Sephadex LH-20 is 1:22. Elute with 2.5 times the column vol...

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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-3, 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 17-hydrogen-9-dehydroandrographolide-3-sulfate sodium (or potassium), 17-hydrogen-9-dehydroandrographolide-3,19-disulfate sodium (or potassium) combination One-time preparation method of substance and its preparation medicine use. Background technique [0002] Andrographis paniculata is the dry aerial part of Andrographis paniculata (Burm.f.) Nees of the Acanthaceae plant. Chemical composition and pharmacological experiments show that the active ingredients of Andrographis paniculata are mainly diterpenoids represented by andrographolide [National Traditional Chinese Medicine Authority. 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 , 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, s...

Claims

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Application Information

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IPC IPC(8): A61K31/365C07D307/60A61P29/00A61P31/12A61P31/16A61P43/00
Inventor 谢宁吕武清杨小玲刘地发李志勇程帆
Owner JIANGZI QINGFENG PHARMACEUTICALS INC
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