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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

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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  • Summary
  • 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 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-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

Embodiment 1

[0064] Get andrographolide, add 5.5 times the amount of acetic anhydride (62%) and glacial acetic acid (38%) to dissolve, and under stirring, slowly add 4.5 times the amount of sulfuric acid at a rate of 1.6ml per minute for 1g andrographolide (52%) and glacial acetic acid (48%), mix evenly, adjust the temperature of the reactor at 16° C., and place it for 90 minutes for sulfonation. Add an equal amount of purified water, stir well, adjust the pH to about 7.0 with 33% NaOH, add 95% ethanol to make the alcohol content reach more than 82%, recover ethanol under reduced pressure, and separate the aqueous solution through macroporous adsorption resin and ODS column chromatography. Gradient elution with water: ethanol, the proportion of water is 80-20%, the proportion of ethanol is 20-80%, the eluate is collected in sections, the same components are combined, and crystallized to obtain 17-hydrogen-9-dehydroandrographis paniculata Sodium lactone-3-sulfate, its sodium salt formula C ...

Embodiment 2

[0072] Get andrographolide, add 5.3 times the amount of acetic anhydride (62%) and glacial acetic acid (38%) to dissolve, and under stirring, slowly add 4.3 times the amount in equal proportions at a rate of 2.2ml per minute for 1g of andrographolide Sulfuric acid glacial acetic acid, mix well, adjust the temperature of the reaction kettle at 15°C, place it for 90 minutes for sulfonation, add an equal amount of purified water, then pour it into saturated sodium chloride solution, and then go through macroporous adsorption resin and ODS column chromatography Separation, gradient elution with water: ethanol, the proportion of water is 80-20%, the proportion of ethanol is 20-80%, the eluate is collected in sections, the same components are combined, and crystallized to obtain 17-hydrogen-9-de Sodium hydroandrographolide-3,19-disulfate, its sodium salt Molecular formula: C 20 h 28 Na 2 o 11 S 2 , Molecular weight: 554.

[0073] Reaction example:

[0074]

[0075] 17-Hydro...

Embodiment 3

[0080] Get andrographolide, add 6.0 times the amount of acetic anhydride (58%) and glacial acetic acid (42%) to dissolve, and under stirring, feed 1.3 liters of 1.4% sulfur trioxide at a rate of 0.07 liters per minute for 1 g of andrographolide , adjust the temperature of the reactor at 17°C, and place it for 100 minutes for sulfonation. Add an equal amount of purified water, stir well, adjust the pH to about 7.0 with 45% KOH, add 95% ethanol to make the alcohol content reach more than 85%, filter, recover ethanol from the filtrate under reduced pressure, and dry it in vacuum to obtain 17-hydrogen-9 - Dehydroandrographolide-3-potassium sulfate, 17-hydro-9-dehydroandrographolide-3,19-potassium disulfate and other mixtures, the mixture was dissolved with a small amount of water, passed through Sephadex LH-20 column, the mixture The ratio of loading sample volume to Sephadex LH-20 is 1:5.5, the ratio of Sephadex LH-20 column diameter to height is 1:22, eluted with 2.5 times colum...

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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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