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Method for preparing indigo and indirubin from dyers woad leaf

A technology of Daqingye and indirubin, which is applied in the direction of organic chemistry, etc., can solve the problems of difficulty in industrialization, difficult to reuse, and short use cycle, and achieve the effects of short extraction cycle, low toxicity and increased content.

Active Publication Date: 2011-09-07
JILIN HENGJIN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chromatography uses a large amount of alumina, which has a short service life, is not easy to reuse, and has high process costs, making it difficult to realize industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: A method for preparing indigo and indirubin from Folium Folium, its main feature is to include the following steps: 1) drying Folium Folium, pulverizing, passing through a 40-120 mesh sieve, and using 0.05-0.2 60wt%-90wt% of mol / L sodium hydroxide

[0020] Ethanol is heated and refluxed for 2-3 times, the extracts are combined, filtered, and the filtrate is set aside;

[0021] 2) Recover ethanol from the filtrate, concentrate, adjust the pH to 7 with hydrochloric acid solution, centrifuge, dissolve the precipitate with hydrochloric acid solution and

[0022] Adjust the pH to 3-5, centrifuge, and use the supernatant for later use;

[0023] 3) Microfilter the above supernatant in a membrane separation device;

[0024] 4) Adsorption and desorption: put the above-mentioned microfiltered stock solution on the resin column for adsorption, the ratio of resin column diameter to column height is 1:8-1:15; the amount of resin column added is the step 3) after The...

Embodiment 2

[0026] Embodiment 2: a kind of method for preparing indigo, indirubin from Folium Folium, its main feature is to comprise the following steps:

[0027] Take Folium Folium and crush it, pass through a 80-mesh sieve, weigh 100g accurately, add 1000ml of 70% ethanol solution containing 0.1mol / L sodium hydroxide, heat and reflux for extraction twice, each time for 2.0 hours, combine the extracts, filter, and filtrate spare.

[0028] The above filtrate was recovered with ethanol, concentrated, adjusted to pH 7 with sodium hydroxide solution, centrifuged, the precipitate was dissolved with hydrochloric acid solution and adjusted to pH 5, centrifuged, and the supernatant was set aside.

[0029] The above supernatant was subjected to microfiltration at room temperature in a roll-type membrane device, and the membrane material was a polyvinylidene fluoride membrane with a pore size of 0.45 µm.

[0030] Pass the above-mentioned microfiltered stock solution through D101 macroporous resi...

Embodiment 3

[0032] Embodiment 3: a kind of method for preparing indigo, indirubin from Folium Folium, its main feature is to comprise the following steps:

[0033] Take Folium Folium and crush it, pass it through a 100-mesh sieve, weigh 100 g accurately, add 1000 ml of 80% ethanol solution containing 0.1mol / L sodium hydroxide, heat and reflux for extraction twice, each time for 1.5 hours, combine the extracts, and filter , and the filtrate is set aside.

[0034] Recover ethanol from the above filtrate, concentrate, adjust the pH to 7 with sodium hydroxide solution, centrifuge, dissolve the precipitate with hydrochloric acid solution, adjust the pH to 5, centrifuge, and use the supernatant for later use.

[0035] The above supernatant was subjected to microfiltration at room temperature in a roll-type membrane device, and the membrane material was a polyvinylidene fluoride membrane with a pore size of 0.45 µm.

[0036] Pass the above-mentioned microfiltered stock solution through D101 mac...

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PUM

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Abstract

The invention belongs to the field of natural product chemistry, and relates to extraction, separation and purification of natural products, in particular to a technical method for extracting high-purity total alkaloids from dyers woad leaf. The method for preparing indigo and indirubin from dyers woad leaf is mainly characterized by comprising the following steps of: drying, pulverizing and sieving dyers woad leaves; heating and extracting by reflux by an ethanol solution containing sodium hydroxide; recovering ethanol from filtrate; concentrating the filtrate, regulating the pH to be neutral by a hydrochloric acid solution, centrifuging; dissolving the precipitate by the hydrochloric acid solution, and centrifuging to obtain supernatant for later use; performing microfiltration on the supernatant in membrane separation equipment; loading the stock solution after microfiltration on a resin column for absorption, then eluting with water to remove water soluble impurities, discarding the water eluent; eluting with aqueous ethanol, collecting the eluent; and recovering ethanol from the eluent, concentrating and drying to obtain a dark red product. The method has the advantages of low production cost of the products, simple process route, smaller toxicity of the extraction solvent and short extraction cycle, and is suitable for application in industrial production. Based on the advantages, the method can further promote industrialized development of the dyers woad leaf extract as a multifunctional product such as a medicine, a health product and the like.

Description

technical field [0001] The invention belongs to the field of natural product chemistry, relates to the extraction, separation and purification of natural products, in particular to a process for extracting high-purity total alkaloids from Folium folium. Background technique [0002] Daqingye is a traditional Chinese medicine in my country. It is the dried leaf of Isats indigotica Fort, a cruciferous plant. It is mainly distributed in Hebei, Jiangsu, Zhejiang, Fujian, Henan, Guangxi and other places. Efficacy of detoxifying, cooling blood and relieving sore throat. The chemical components contained are indigo, indirubin, tryptanthone, 3-hydroxyphenylquinazolone, organic acids and so on. Pharmacological studies have shown that it has antibacterial, antiviral, anticarbuncle, and immune-enhancing effects. It is widely used clinically to treat various viral influenza, epidemic encephalitis B, mumps, viral hepatitis, and pharyngitis. , Chickenpox and other infectious diseases. L...

Claims

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Application Information

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IPC IPC(8): C07D209/36
Inventor 梁剑平李雪虎陆锡宏陶蕾周翔王署阳
Owner JILIN HENGJIN PHARMA CO LTD
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