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Method for simultaneously preparing andrographolide and dehydrated andrographolide

A technology for dehydrating andrographis paniculata and andrographolide is applied in directions such as medical raw materials derived from angiosperm subphylum, organic chemistry, etc., and can solve the problem of not simultaneously preparing dehydrating andrographolide and the like

Inactive Publication Date: 2008-04-30
INST OF TROPICAL BIOSCI & BIOTECH CHINESE ACADEMY OF TROPICAL AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent application CN1935798A discloses a preparation method of andrographolide, through which high-purity andrographolide is prepared, but dehydroandrographolide is not prepared at the same time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] After crushing 50g of Andrographis paniculata, its particle size reaches 4mm, add 150mL of 50% ethanol aqueous solution to mix, soak and extract 3 times, and extract for 3, 2 and 1 days respectively. The extract is filtered and decompressed to recover the solvent until the andrographolide is still in a dissolved state, add an appropriate amount of water to dilute, filter or centrifuge to discard the precipitate, pass the filtrate through the non-polar DA201-A macroporous resin produced by the chemical factory of Nankai University, and pass the filtrate through the resin column The flow rate of exchange and adsorption is 3mL / min; after the exchange is completed, they are eluted with water, 35%, 45%, 55%, and 60% ethanol respectively. Ester standard substance carries out contrast decision to collect the starting point of eluent, andrographolide and dehydroandrographolide content in the high performance liquid chromatography detection eluent, mainly contain andrographolide ...

Embodiment 2

[0020] After 50g of the whole herb of Andrographis paniculata is crushed, its particle size reaches 5mm, put it into an extractor, add 200mL of 50% ethanol aqueous solution to mix, then put the mixed solution in the ultrasonic generator container, and use ultrasonic waves to extract the Andrographis paniculata powder. The ultrasonic frequency used is 20KHz, the power is 50W-10000W, the ultrasonic extraction time is 60 minutes, and the temperature is 40 degrees. The extract is filtered and decompressed to recover the solvent until the andrographolide is still in a dissolved state, add an appropriate amount of water to dilute, filter or centrifuge to discard the precipitate, pass the filtrate through the non-polar DA201-B macroporous resin produced by the chemical factory of Nankai University, and pass the filtrate through the resin column The flow rate of exchange and adsorption is 3mL / min; after the exchange is completed, they are eluted with water, 30%, 50%, 70%, and 90% respe...

Embodiment 3

[0023] After crushing 50g of Andrographis paniculata, its particle size reaches 2mm, add 250mL of 60% ethanol aqueous solution to mix, soak and extract for 3 times, and extract for 3, 2 and 1 days respectively. The extract is filtered and decompressed to recover the solvent until the andrographolide is still in a dissolved state, add an appropriate amount of water to dilute, filter or centrifuge to discard the precipitate, pass the filtrate through the non-polar DA201-B macroporous resin produced by the chemical factory of Nankai University, and pass the filtrate through the resin column The flow rate of exchange and adsorption is 3mL / min; after the exchange is completed, they are eluted with water, 30%, 45%, 60%, and 70% ethanol respectively. The ester standard substance carries out contrast decision to collect the starting point of eluent, andrographolide and dehydroandrographolide content in the high performance liquid chromatography detection eluent, mainly contain androgra...

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Abstract

The invention relates to a method for simultaneously preparing andrographolide and didehydroandrographolide. The method includes that common andrographis herbs are smashed and then added into alcohol solvent with certain concentration to be abstracted, extracting solution is filtered, solvent is recycled to lead the concentration of the alcohol solvent in filtrate to be lower than 20 percent; after being filtered, the filtrate is taken to be exchanged through macroporous resin and to be absorbed, the alcohol solvent with certain concentration is used to operate the gradient elution, so as to lead the andrographolide and the didehydroandrographolide to be desorbed in elutriant with different concentration; after being concentrated, the elutriant is recrystallized and refined to obtain andrographolide crystal and didehydroandrographolide crystal. The purity degree of the two crystals obtained through the method reaches above 97 percent, and the method has the advantages that the process is simple, the operation is easy, the cost is low, the industrializing production can be operated, etc.

Description

technical field [0001] The invention relates to a method for simultaneously separating and preparing andrographolide and dehydroandrographolide, in particular to a method for simultaneously separating and preparing the two main active ingredients in andrographolide by using a macroporous resin. Background technique [0002] The main active ingredients of Andrographis paniculata are diterpene lactones, which have anti-inflammatory, antibacterial, and antiviral effects. Among them, andrographolide and dehydroandrographolide have the highest content, and dehydroandrographolide is the most effective one in andrographolide compounds. Drugs made from andrographolide or dehydroandrographolide and their derivatives, such as andrographolide tablets, Chuanhuning injection, Yanhuning injection, etc., have been widely used clinically. [0003] At present, the traditional techniques for extracting diterpene lactones in Andrographis paniculata include water extraction, alkaline water ext...

Claims

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Application Information

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IPC IPC(8): C07D307/58A61K36/19
Inventor 吴娇戴好富梅文莉
Owner INST OF TROPICAL BIOSCI & BIOTECH CHINESE ACADEMY OF TROPICAL AGRI SCI
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