Preparation method of arctiin

A technique for arctiside and arctifolia, which is applied in the field of arctiside drug preparation, can solve the problems of yield and purity impact, inconvenient and unsuitable purification treatment, etc., and achieves increased purity, improved product output rate and less pollution. Effect

Pending Publication Date: 2021-04-30
BENGBU COLLEGE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the above-mentioned preparation method also has the following technical defects in the specific operation: arctiin contains a lactone ring structure, which is easily hydrolyzed under heating conditions, which brings great inconvenience to the later stage purification treatment, and will lead to high yield and low yield. The purity is reduced due to certain influences, which is very inappropriate

Method used

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  • Preparation method of arctiin

Examples

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Effect test

Embodiment 1

[0032] Example 1: Take 1 kg of arctium coarse powder with a particle size of about 2 mm after drying and crushing, add it to 10 times the aqueous solution for 2 times of reflux extraction, leave the extract standing, filter, combine, and apply DA-201 type macroporous adsorption resin column (column volume 500ml) for adsorption and enrichment, then elute with 3 times the column volume and ethanol with a mass concentration of 40%, and collect the eluate to stand still, concentrate, filter, and then use the ratio A 1:4 water-ethyl acetate mixed solvent was used for 3-stage countercurrent extraction, the extracts were combined, the solvent was recovered under reduced pressure and concentrated, and the HPD-700 macroporous adsorption resin column (column volume 500ml) was used for adsorption and enrichment. Then elute with 40% ethanol of 3 times the column volume mass concentration, and collect the eluate to stand still, concentrate, filter to obtain 500ml of arctium fruit enrichment...

Embodiment 2

[0033] Embodiment 2: Get 1 kg of arctium coarse powder with a particle diameter of about 0.5 mm after drying and crushing, add it to 10 times of aqueous solution and carry out reflux extraction for 2 times, leave the extract, filter, merge, and apply DA- 201 type macroporous adsorption resin column (column volume 500ml) carries out adsorption and enrichment, then carries out eluting with 5 times column volume mass concentration 70% ethanols, and collects eluate and leaves standstill, concentrates, filters, and then uses the ratio of A 1:4 water-ethyl acetate mixed solvent was used for 5-stage countercurrent extraction, the extracts were combined, the solvent was recovered under reduced pressure and concentrated, and the HPD-700 macroporous adsorption resin column (column volume 500ml) was used for adsorption and enrichment, and then Elute with 5 times column volume mass concentration of 60% ethanol, and collect the eluate to stand still, concentrate, and filter to obtain 1000ml...

Embodiment 3

[0034] Example 3: Take 10 kg of arctium coarse powder with a particle size of about 2 mm after drying and crushing, add it to 20 times the aqueous solution for 2 times of reflux extraction, leave the extract standing, filter, combine, and apply DA-201 type macroporous adsorption resin column (column volume 5L) for adsorption and enrichment, then elute with 3 times column volume mass concentration of 40% ethanol, and collect the eluate to stand still, concentrate, filter, and then use a ratio of 1 : 4 water-ethyl acetate mixed solvents carry out 3 stages of counter-current extraction, combine the extracts, reclaim the solvent under reduced pressure and concentrate, go to the HPD-700 type macroporous adsorption resin column (column volume 5L) for adsorption and enrichment, and then use Elute with ethanol with a mass concentration of 3 times column volume and mass concentration of 40%, and collect the eluate to stand still, concentrate, and filter to obtain 5 L of Arctium fruit en...

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Abstract

The invention provides a preparation method of arctiin, which comprises the following steps: taking arctiin coarse powder, adding the arctiin coarse powder into an aqueous solution for reflux extraction, standing the extracting solution, filtering, merging, adding into a macroporous adsorption resin column, eluting with ethanol, collecting the eluent, standing, concentrating, filtering, and carrying out counter-current extraction with a water-ethyl acetate mixed solvent, merging extract liquor, recovering solvent under reduced pressure, concentrating, adding into a macroporous adsorption resin column, eluting by using ethanol, collecting eluent, standing, concentrating, filtering, filling into a semipermeable membrane or a selective permeable membrane bag, putting into dialysate, dialyzing, collecting dialysate, performing standing, concentrating, adding into a methanol solution, crystallizing at a certain temperature, and separating crystals, and washing and drying to obtain an arctiin finished product with the purity of more than 95%. According to the arctiin prepared by the method, the product yield can be greatly improved, the product purity is increased, the resource utilization rate is increased, the energy consumption is low, and the pollution is small.

Description

technical field [0001] The invention relates to the technical field of arctiin medicine preparation, in particular to a preparation method of arctiin. Background technique [0002] Arctiin (arctiin) is a main active substance in Arctium Fructus, with a molecular formula of C27H34O11 and a molecular weight of 534.5523. Its content is about 8.4% in Arctium Fructus. The Chinese Pharmacopoeia (2005 edition) stipulates the Chemicalbook of arctiin under Arctium Fructus The content should reach more than 5% of the quality of the medicinal material. Pharmacological studies have shown that arctiin has significant physiological activities such as anti-tumor, anti-virus, and anti-oxidation, and it can also be used as a raw material for the synthesis of other active derivatives. The preparation of arctiin has attracted widespread attention. [0003] In the prior art, the application number is "200910233827.6" a kind of preparation method of arctiin, the process step is to take the coar...

Claims

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Application Information

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IPC IPC(8): C07H1/08C07H15/26
CPCC07H1/08C07H15/26Y02A50/30
Inventor韩伟邓源喜马龙许晖张斌李妍
OwnerBENGBU COLLEGE