Production technique of andrographolide and neoandrographolide, dehydroanddrographolide, oxyandrographolide

A technology of neoandrographolide and total andrographolide can be applied to cardiovascular system diseases, medical raw materials derived from angiosperm subphylum, digestive system, etc. To meet the screening and clinical application of pharmacological activity, it is not conducive to the labor protection and environmental protection of operators, to achieve the effect of simple production equipment, conducive to labor protection and environmental protection, and to achieve large-scale industrial production

Active Publication Date: 2009-10-21
雷允上药业集团有限公司
View PDF2 Cites 35 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, a lot of impurities are still mixed after the impurities are removed by the macroporous adsorption resin, and the silica gel column chromatography is directly used, the amount of solvent used is large, the separation process is complicated, and the toxic reagents chloroform and methanol are used as eluents, which is als

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Production technique of andrographolide and neoandrographolide, dehydroanddrographolide, oxyandrographolide
  • Production technique of andrographolide and neoandrographolide, dehydroanddrographolide, oxyandrographolide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation of embodiment 1 andrographolide

[0026] Take 2 kg of Andrographis paniculata stem and leaf powder, heat-dip and extract twice with 18 times the amount of 95% ethanol, recover the ethanol extract, dilute it to about 4000ml with water, and wash away fat-soluble impurities such as chlorophyll with 6000ml of petroleum ether for three times, and the aqueous solution Concentrate, dissolve the concentrated extract in 1500ml of 95% ethanol, reflux with 50g of activated carbon for decolorization, filter while it is hot, recover the ethanol to 800ml, slowly add 200ml of water, when the water is added, there should be no solid precipitation, place it, and most of the andrographolide will precipitate Crystallize, filter, concentrate the mother liquor to 400ml, place, and then separate out a small part of andrographolide crystals, filter, recycle the solvent from the filtrate to dryness, and obtain an extractum, which is heated and dissolved in 1000ml95% ethanol, and...

Embodiment 2 3

[0027] The separation of three kinds of andrographis paniculata diterpene lactone monomers of embodiment 2

[0028] Get 20g of total andrographolide in Example 1, grind finely, dissolve with chloroform 200ml, filter, and insoluble matter is cold-dissolve 2 times with chloroform 200ml, 100ml respectively again, filter, merge the chloroform liquid, obtain Two parts of chloroform liquid and insoluble matter. Recover the chloroform solution to dryness, dissolve it in 100ml of 95% ethanol, place it, and precipitate deoxyandrographolide flaky crystals, concentrate the mother liquor to 60ml, place it, and precipitate dehydroandrographolide needle crystals, and continue to concentrate the remaining mother liquor alternately Crystallization, merging deoxyandrographolide crystals, and recrystallization with ethanol and acetone respectively to obtain pure product 3.6g (deoxyandrographolide can still be recovered in the filtrate). The combined dehydroandrographolide crystals were recrystal...

Embodiment 3

[0029] The preparation of embodiment 3 total andrographolides

[0030] Take 1kg of Andrographis paniculata stem and leaf coarse powder, use 15 times the amount of 95% ethanol to extract by cold soaking twice, each time for 24 hours, recover the ethanol extract, dilute it to about 2000ml with water, and use 3000ml of petroleum ether to wash off the chlorophyll etc. Fat-soluble impurities, concentrated aqueous solution, heat-dissolve the concentrated extract in 1000ml of methanol, reflux with 30g of activated carbon for decolorization, filter while it is hot, recover methanol to about 500ml, slowly add 100ml of water, no solids should be precipitated after adding water, first place it at room temperature , and then transferred to the refrigerator overnight, until the andrographolide crystals are completely separated out, vacuum filtered, the filtrate is concentrated to about 350ml, placed in the same way as above, a small amount of andrographolide crystals continue to separate ou...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a production technique of andrographolide and neoandrographolide, dehydroanddrographolide and oxyandrographolide; the technique comprises the following steps of: firstly preparing stem and leaf extract of andrographis paniculata, removing fat-soluble impurities such as chlorophyll and the like with petroleum ether, and then hot-melting the extract in lower alcohol or aqueous lower alcohol, conducting reflux and decolorization with active carbon, separating out a majority of andrographolide crystals, then removing flavonoid through an alumina column or alkali cleaning, obtaining the andrographolide, cold-melting the andrographolide with trichloromethane or dichloromethane for 2 to 4 times, filtering and obtaining two parts of filtrate and insoluble substances, concentrating the filtrate, then conducting solvent crystallization and recrystallization or column chromatography for separation, and finally, respectively obtaining dehydroanddrographolide and pure product of andrographolide; the insoluble substances go through solvent crystallization and recrystallization or column chromatography for separation to obtain the neoandrographolide and pure product of andrographolide. The technique has simple production equipment, simplified routes and easy operation, can realize industrialized batch production; and the proportion of neoandrographolide, dehydroanddrographolide and oxyandrographolide in the obtained andrographolide is high, while the content of impurities is low. The obtained neoandrographolide, dehydroanddrographolide and oxyandrographolide all have monomer purity of higher than 98 percent, thus being capable of being used as chemical reference substance of the traditional Chinese medicine, or being applied as raw materials of medicine and chemical industry.

Description

technical field [0001] The invention relates to the extraction and separation of Chinese herbal medicines, more precisely to the production technology of neoandrographolide, dehydroandrographolide and deoxyandrographolide. Background technique [0002] Andrographis Paniculata (Burm.f.) Nees is the dry aerial part of Andrographis Paniculata (Burm.f.) Nees. Originally produced in India, it is cultivated in East China, Central South and other regions of my country. Bitter in nature, cold, Guixin, lung, large intestine, bladder channel. It has the effects of clearing heat and detoxification, cooling blood, reducing swelling and relieving pain. Clinically, it is mainly used for symptoms such as cold and fever, sore throat, aphtha of the mouth and tongue, sudden cough and overworked cough, diarrhea and dysentery, astringent pain due to hot stranguria, carbuncle and sore, venomous snake bite and other symptoms. [0003] The main components of Andrographis paniculata contain dite...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): A61K36/19C07D307/60C07D307/58A61P1/16A61P9/00A61P31/04A61P31/12A61P37/04A61K135/00A61K127/00
Inventor 周一君杨增石荣火卢扬陆荣
Owner 雷允上药业集团有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap