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Method of preparing flaccid anemone saponins W1 and W3 from rhizome of flaccid anemone

A technology of kunain and black medicinal materials, which is applied in the field of preparation of kusaponin W1 and W3, which can solve problems such as unfavorable safety management, serious environmental pollution, and high toxicity, and achieve the effects of reducing production costs, pollution, and health threats

Active Publication Date: 2014-01-08
广州康和药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method reported in the above-mentioned literature has complex procedures, and the final product yield is low due to repeated use of silica gel column chromatography
Simultaneously, because organic solvents such as chloroform (first class solvent), acetonitrile (second class solvent) and ethyl acetate (flammable and explosive solvent) have been used in the preparation process, the toxicity of belonging to class one and second class solvents is big (carcinogenicity is strong ), serious environmental pollution, and the above-mentioned flammable and explosive solvents are not conducive to safety management in the production process, so they are not suitable for industrial production

Method used

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  • Method of preparing flaccid anemone saponins W1 and W3 from rhizome of flaccid anemone
  • Method of preparing flaccid anemone saponins W1 and W3 from rhizome of flaccid anemone
  • Method of preparing flaccid anemone saponins W1 and W3 from rhizome of flaccid anemone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1) Take 1 kg of dried Diwu raw material and add it to the heating vessel. The raw material of Diwu medicinal material is generally in powder form.

[0041] 2) Pour 10L (10kg) of water into the heating vessel, heat and decoct for 1 hour, filter out the decoction, and keep the residue in the heating vessel.

[0042] 3) Repeat step 2) once, and combine the decoction filtered out each time.

[0043] 4) First, put the combined decoction on a D-101 macroporous resin column;

[0044] Then, carry out gradient elution with water, 10% ethanol, 50% ethanol and 95% ethanol solution in sequence, and achieve the purpose of removing impurities and cleaning through the elution treatment of water, 10% ethanol and 95% ethanol solution, and collect 50% ethanol wash The eluate after de-treatment,

[0045] Finally, the collected eluate was concentrated and dried under reduced pressure to obtain 62 g of the total saponins extract.

[0046] 5) Firstly, dissolve the obtained Diwu saponin ex...

Embodiment 2

[0056] 1) Take 1 kg of dried Diwu raw material and add it to the heating vessel. The raw material of Diwu medicinal material is generally in powder form.

[0057] 2) Pour 8L (8kg) of water into the heating vessel, heat and decoct for 3 hours, filter out the decoction, and keep the residue in the heating vessel.

[0058] 3) Repeat step 2) twice, and combine the decoction filtered out each time.

[0059] 4) First, put the combined decoction on the AB-8 macroporous resin column;

[0060] Then, carry out gradient elution with water, 25% ethanol, 80% ethanol and 95% ethanol solution in sequence, and achieve the purpose of removing impurities and cleaning through the elution treatment of water, 25% ethanol and 95% ethanol solution, and collect 80% ethanol wash The eluate after de-treatment,

[0061] Finally, the collected eluate was concentrated and dried under reduced pressure to obtain 58 g of the total saponins extract.

[0062] 5) Firstly, dissolve the obtained Diwu saponin e...

Embodiment 3

[0072] 1) Take 1 kg of dried Diwu raw material and add it to the heating vessel. The raw material of Diwu medicinal material is generally in powder form.

[0073] 2) Pour 5L (5kg) of water into the heating vessel, heat and decoct for 2 hours, filter out the decoction, and keep the residue in the heating vessel.

[0074] 3) Repeat step 2) twice, and combine the decoction filtered out each time.

[0075] 4) First, put the combined decoction on the AB-8 macroporous resin column;

[0076] Then, gradient elution was carried out with water, 35% ethanol, 75% ethanol and 95% ethanol solution in sequence, and the purpose of removing impurities and cleaning was achieved through the elution treatment of water, 35% ethanol and 95% ethanol solution, and the 75% ethanol solution was collected. The eluate after de-treatment,

[0077] Finally, the collected eluate was concentrated and dried under reduced pressure to obtain 60 g of the total saponins extract.

[0078] 5) Firstly, dissolve t...

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Abstract

The invention discloses a method of preparing flaccid anemone saponins W1 and W3 from rhizome of flaccid anemone. The method is high in end-product yield, and no toxicity or flammable solvent is used in the preparation process. The method includes: 1, adding rhizome of flaccid anemone to a heating vessel; 2, adding water into the heating vessel, decocting and filtering, and keeping residue; 3, repeating the step 2 for once to two times, and combining filtered decoctions; 4, applying the decoction combination to D-101 macroporous resin columns, performing gradient elution with 10% ethanol solution, 50% ethanol solution and 95% ethanol solution respectively, collecting eluent after 50% ethanol elution, and concentrating and drying under reduced pressure; 5, dissolving obtained flaccid anemone total saponins in water, adding a sample of solution to reverse phase ODS columns, eluting with 30% ethanol solution, 65% ethanol solution and 100% ethanol solution respectively, and drying under reduced pressure; 6, separating by means of preparative efficient liquid chromatography to obtain purified flaccid anemone saponins W1 and W3.

Description

technical field [0001] The present invention relates to a kind of preparation kusaponin W 1 and W 3 The method, specifically, relates to a higher yield of the final product, which does not involve toxic and flammable and explosive solvents in the preparation process from the medicinal material Diguanin W simultaneously. 1 and W 3 Methods. Background technique [0002] Rheumatoid arthritis (RA) is an autoimmune disease characterized by chronic inflammation of the joint synovium. Excessive activation, proliferation and infiltration of T lymphocytes during the body's immune response will aggravate joint inflammation and periosteal tissue hyperplasia. , can cause joint swelling and pain, destruction of articular cartilage, narrowing of the joint space, late joint deformity, and eventually varying degrees of disability. According to statistics, RA occurs all over the world, with an average incidence rate of 1%, while the prevalence rate in my country is 0.3% to 0.4%. If not d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 范春林王英王贵阳叶文才鲁展雨裴红于江月蔡道菊黄杰文
Owner 广州康和药业有限公司
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