CN101879265A - Process for co-producing total saponins and polysaccharide from star-of-Bethlehem - Google Patents

Process for co-producing total saponins and polysaccharide from star-of-Bethlehem Download PDF

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Publication number
CN101879265A
CN101879265A CN2010101568428A CN201010156842A CN101879265A CN 101879265 A CN101879265 A CN 101879265A CN 2010101568428 A CN2010101568428 A CN 2010101568428A CN 201010156842 A CN201010156842 A CN 201010156842A CN 101879265 A CN101879265 A CN 101879265A
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China
Prior art keywords
polysaccharide
total saponins
ethanol
herba phyllanthi
phyllanthi urinariae
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CN2010101568428A
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Chinese (zh)
Inventor
苏刘花
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Nanjing Zelang Agricultural Development Co Ltd
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Nanjing Zelang Agricultural Development Co Ltd
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Priority to CN2010101568428A priority Critical patent/CN101879265A/en
Publication of CN101879265A publication Critical patent/CN101879265A/en
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Abstract

The invention relates to a process for co-producing total saponins and polysaccharide from star-of-Bethlehem, which comprises the following process steps: grinding the star-of-Bethlehem used as the raw material; carrying out reflux extraction for 2 to 3 times by using water; settling impurities by using a ZTC-II settling agent; enriching saponins and separating the polysaccharide by using macroporous resin; carrying out gradient alcohol precipitation repeatedly; carrying out decoloration by using an activated-charcoal column to prepare the polysaccharide; and adding a medium-pressure magnesia column and carrying out ethanol dissolution recrystallization to prepare the total saponins. By adopting the process, the content of the total saponins produced reaches 90 percent and the content of the polysaccharide reaches about 80 percent. The process has high raw material utilization rate.

Description

The joint production process of a kind of Herba Phyllanthi Urinariae's total saponins, polysaccharide
Technical field:
The invention belongs to the bioseparation technology field, the joint production process of particularly a kind of Herba Phyllanthi Urinariae's total saponins, polysaccharide.
Background technology:
Tiger eye Herba Phyllanthi Urinariae (Ornithogalum caudatum Ait) has another name called Rhizoma Picrorhizae Herba Phyllanthi Urinariae, Urginea maritima, calabash orchid, for Liliaceae tiger eye Herba Phyllanthi Urinariae, belongs to evergreen perennial bulbous plant, originates in the south, Africa.In northern China cultivation being arranged. among the people being used as medicine with herb or bulb, be mainly used in antiinflammatory and anticancer.Tiger eye Herba Phyllanthi Urinariae has high medical value, pharmaceutical research shows that the tiger eye Herba Phyllanthi Urinariae saponin OSW21 among the tiger eye Herba Phyllanthi Urinariae has tangible active anticancer to pulmonary carcinoma, breast carcinoma, external anti-p338 Lymphocytic leukemia is active result show, OSW21 is common cancer therapy drug camptothecine, Ah mould's rope, paclitaxel active anticancer 10~100 times, and normal cell there is not toxicity, therefore, be a kind of Chinese herbal medicine of great exploitation potential for its.
Mostly existing extraction separation Herba Phyllanthi Urinariae saponin technology is the old technology of tradition.Be that the lixiviate of Herba Phyllanthi Urinariae's leaf water temperature is got, the lead acetate precipitated impurities, activated carbon adsorption, ethanol extracts once more, thick glycosides water dissolution, with Carbon bisulfide, ether washing, chloroform extracts again successively, and the extraction of reuse chloroform alcohol water miscible fluid separates with alumina column, recrystallization obtains three kinds of monomer components, complex process is loaded down with trivial details, and reagent type is various, brings difficulty to recovery.Also have and utilize macroporous resin adsorption prepared saponin, " separation and Extraction of tiger eye Herba Phyllanthi Urinariae saponin " delivered as Xiao Chong etc. adopts ethanol extraction, defat with petroleum ether, AB-8 resin absorption, D-280 resin decolorization.The method of existing patent disclosure is also mostly to be preparations of crude extract, and as patent 200510069273 " Preparation method and use of tiger eye extracting active ingredient of starofbethlehem ", this method adopts ethanol extraction, and resin isolation obtains crude extract.
Existing disclosed Omithogalum caudatum polysaccharide technology, extracting method is simple, product content is lower, as patent 200510017123 " the tiger eye Omithogalum caudatum polysaccharide medicine of treatment hepatocarcinoma ", the method of this patent disclosure is that water is carried, and low alcohol precipitation precipitate discards, high again alcohol precipitation polysaccharide, washing with alcohol gets final product, polyoses content 50%.
Summary of the invention:
The technical problem to be solved in the present invention provides the joint production process of a kind of Herba Phyllanthi Urinariae's total saponins, polysaccharide, and this technology is fit to the separation of Herba Phyllanthi Urinariae's plurality of active ingredients, can improve Herba Phyllanthi Urinariae's utilization ratio of raw materials.
The object of the present invention is achieved like this:
The joint production process of a kind of Herba Phyllanthi Urinariae's total saponins, polysaccharide is characterized in that comprising following step:
1) extract: get Herba Phyllanthi Urinariae's pulverizing medicinal materials, added 5-8 times of water gaging reflux, extract, 1-2 hour, extract 2-3 time, merge extractive liquid, adds the clarifier sedimentation and filtration, collects filtrate;
2) macroporous resin adsorption: above-mentioned filtrate is added macroporous resin adsorption, collect lower column liquid, water-pure gradient elution is collected alcohol eluen;
3) alcohol eluen total saponins purification: with step 2) concentrates small size, adds compression leg in the magnesium oxide, the ethyl acetate-ethanol gradient elution is collected the saponin flow point and is concentrated small size, adds the ether precipitating, the precipitating thing leaches dissolve with ethanol crystallization 2-3 time, is drying to obtain Herba Phyllanthi Urinariae's total saponins;
4) polysaccharide purification: with step 2) lower column liquid is evaporated to density 1.1-1.3, adds ethanol gradient precipitate with ethanol, leaches the precipitate hot water dissolving, the polysaccharide activated carbon column decoloring, destaining solution concentrates and adds the ethanol precipitating, leaches precipitate, and low-temperature vacuum drying promptly gets Omithogalum caudatum polysaccharide.
Clarifier is the ZTC-II clarifier in the step 1), consumption 1-3 ‰.
Step 2) a kind of among the optional D101 of macroporous resin, AB-8 and the HZ816.Preferred HZ816.
Step 2) water-pure gradient elution is that 6-8 times of column volume washed 5-6 times of column volume 50-70% ethanol elution again in.
The ethyl acetate-ethanol gradient elution is 8-10 times of column volume eluent ethyl acetate 4-8 times of column volume 50-90% ethanol elution again in the step 3).Preferred 85% ethanol.
Crystallization condition is in the step 3): the 90-99% alcohol reflux dissolves, and is recycled to the 1/2-1/3 of original volume, leaves standstill crystallization.
Gradient precipitate with ethanol in the step 4) is three gradients of final concentration of alcohol 90%-70%-50%.
In sum, there is following advantage in the present invention: water refluxes to carry and helps the stripping simultaneously of saponin polysaccharide, and sedimentation agent can be removed macromolecular substances and part tannin, has improved the macroporous resin life-span; The compression leg processing speed is fast, effective in the magnesium oxide, total saponin content is high; Gradient precipitate with ethanol and activated-charcoal column purified polysaccharide, the polyose quality better.
Further specify the present invention below in conjunction with the specific embodiment, but the scope of protection of present invention is not limited to following embodiment.
The specific embodiment:
Embodiment 1:
Get 1kg tiger eye Herba Phyllanthi Urinariae, pulverize, add the 5L deionized water, reflux, extract, 1 hour is extracted 3 times, and merge extractive liquid, adds the 3gZTC-II sedimentation agent and stirs, and fully sedimentation filters to add in the 500mlHZ816 resin column and adsorbs, and lower column liquid is collected standby.Get impurity in the 4L deionized water eluting resin, get the alcoholic solution of 3L50% again, the eluting saponin constituent.
1: total saponins is washed purification: the saponin eluent, the concentrating under reduced pressure small size (concentrate volume must not greater than the magnesium oxide volume 1/5), press the magnesium oxide post in pumping into, earlier 8 times of column volume eluent ethyl acetate impurity, 4 times of column volumes of reuse, 85% ethanol elution total saponins, collect the total saponins flow point and concentrate nothing alcohol, add 20ml ether precipitating, the precipitating thing leaches, 90% dissolve with ethanol refluxes and dissolves, concentrate 1/3 static crystallization, crystallization three times gets total saponins 6g content 90%.
2: polysaccharide purification: lower column liquid is evaporated to density 1.1, emit and add dehydrated alcohol to alcohol 90%, adition process fully stirs, precipitate is 70% and 50% two gradient precipitate with ethanol again, crude polysaccharides leaches dissolving and adds the craboraffin post, collect destaining solution and concentrate adding ethanol to 80% precipitate with ethanol, leach vacuum drying and get polysaccharide 30g content 80%.
Embodiment 2:
Get 1kg tiger eye Herba Phyllanthi Urinariae, pulverize, add the 8L deionized water, reflux, extract, 2 hours is extracted 2 times, and merge extractive liquid, adds the 4gZTC-II sedimentation agent and stirs, and fully sedimentation filters to add in the 500mlAB-8 resin column and adsorbs, and lower column liquid is collected standby.Get impurity in the 3L deionized water eluting resin, get the alcoholic solution of 2.5L70% again, the eluting saponin constituent.
1: total saponins is washed purification: the saponin eluent, the concentrating under reduced pressure small size (concentrate volume must not greater than the magnesium oxide volume 1/5), press the magnesium oxide post in pumping into, 10 times of column volume eluent ethyl acetate impurity of elder generation, 4 times of column volumes of reuse, 90% ethanol elution total saponins is collected the total saponins flow point and is concentrated nothing alcohol, adds 25ml ether precipitating, the precipitating thing leaches, 99% dissolve with ethanol refluxes and dissolves, and concentrates 1/2 static crystallization, crystallization three times, get total saponins 6.2g, content 86%.
2: polysaccharide purification: lower column liquid is evaporated to density 1.2, emit and add dehydrated alcohol to alcohol 90%, adition process fully stirs, precipitate is 70% and 50% two gradient precipitate with ethanol again, crude polysaccharides leaches dissolving and adds the craboraffin post, collect destaining solution and concentrate adding ethanol to 70% precipitate with ethanol, leach vacuum drying and get polysaccharide 28g, content 78%.
Embodiment 3:
Get 1kg tiger eye Herba Phyllanthi Urinariae, pulverize, add the 5L deionized water, reflux, extract, 1 hour is extracted 3 times, and merge extractive liquid, adds the 3gZTC-II sedimentation agent and stirs, and fully sedimentation filters to add in the 500mlD101 resin column and adsorbs, and lower column liquid is collected standby.Get impurity in the 4L deionized water eluting resin, get the alcoholic solution of 3L60% again, the eluting saponin constituent.
1: total saponins is washed purification: the saponin eluent, the concentrating under reduced pressure small size (concentrate volume must not greater than the magnesium oxide volume 1/5), press the magnesium oxide post in pumping into, earlier 10 times of column volume eluent ethyl acetate impurity, 4 times of column volumes of reuse, 50% ethanol elution total saponins, collect the total saponins flow point and concentrate nothing alcohol, add 10ml ether precipitating, the precipitating thing leaches, 95% dissolve with ethanol refluxes and dissolves, concentrate 1/2 static crystallization, crystallization three times gets total saponins 5.5g content 85%.
2: polysaccharide purification: lower column liquid is evaporated to density 1.15, emit and add dehydrated alcohol to alcohol 90%, adition process fully stirs, precipitate is 70% and 50% two gradient precipitate with ethanol again, crude polysaccharides leaches dissolving and adds the craboraffin post, collect destaining solution and concentrate adding ethanol to 80% precipitate with ethanol, leach vacuum drying and get polysaccharide 26g, content 75%.
Embodiment 4:
Get 10kg tiger eye Herba Phyllanthi Urinariae, pulverize, add the 50L deionized water, reflux, extract, 1 hour is extracted 3 times, and merge extractive liquid, adds the 40gZTC-II sedimentation agent and stirs, and fully sedimentation filters to add in the 6LHZ816 resin column and adsorbs, and lower column liquid is collected standby.Get impurity in the 40L deionized water eluting resin, get the alcoholic solution of 30L60% again, the eluting saponin constituent.
1: total saponins is washed purification: the saponin eluent, the concentrating under reduced pressure small size (concentrate volume must not greater than the magnesium oxide volume 1/5), press the magnesium oxide post in pumping into, earlier 10 times of column volume eluent ethyl acetate impurity, 6 times of column volumes of reuse, 85% ethanol elution total saponins, collect the total saponins flow point and concentrate nothing alcohol, add 200ml ether precipitating, the precipitating thing leaches, 90% dissolve with ethanol refluxes and dissolves, concentrate 1/3 static crystallization, crystallization three times gets total saponins 63g content 90%.
2: polysaccharide purification: lower column liquid is evaporated to density 1.2, emit and add dehydrated alcohol to alcohol 90%, adition process fully stirs, precipitate is 70% and 50% two gradient precipitate with ethanol again, crude polysaccharides leaches dissolving and adds the craboraffin post, collect destaining solution and concentrate adding ethanol to 80% precipitate with ethanol, leach vacuum drying and get polysaccharide 310g, content 80%.
Embodiment 5:
Get 10kg tiger eye Herba Phyllanthi Urinariae, pulverize, add the 80L deionized water, reflux, extract, 2 hours is extracted 2 times, and merge extractive liquid, adds the 35gZTC-II sedimentation agent and stirs, and fully sedimentation filters to add in the 6LAB-8 resin column and adsorbs, and lower column liquid is collected standby.Get impurity in the 48L deionized water eluting resin, get the alcoholic solution of 35L65% again, the eluting saponin constituent.
1: total saponins is washed purification: the saponin eluent, the concentrating under reduced pressure small size (concentrate volume must not greater than the magnesium oxide volume 1/5), press the magnesium oxide post in pumping into, earlier 10 times of column volume eluent ethyl acetate impurity, 6 times of column volumes of reuse, 85% ethanol elution total saponins, collect the total saponins flow point and concentrate nothing alcohol, add 200ml ether precipitating, the precipitating thing leaches, 90% dissolve with ethanol refluxes and dissolves, concentrate 1/3 static crystallization, crystallization three times gets total saponins 61g content 85%.
2: polysaccharide purification: lower column liquid is evaporated to density 1.2, emit and add dehydrated alcohol to alcohol 90%, adition process fully stirs, precipitate is 70% and 50% two gradient precipitate with ethanol again, crude polysaccharides leaches dissolving and adds the craboraffin post, collect destaining solution and concentrate adding ethanol to 80% precipitate with ethanol, leach vacuum drying and get polysaccharide 305g, content 75%.

Claims (7)

1. the joint production process of Herba Phyllanthi Urinariae's total saponins, polysaccharide is characterized in that comprising following step:
1) extract: get Herba Phyllanthi Urinariae's pulverizing medicinal materials, added 5-8 times of water gaging reflux, extract, 1-2 hour, extract 2-3 time, merge extractive liquid, adds the clarifier sedimentation and filtration, collects filtrate;
2) macroporous resin adsorption: above-mentioned filtrate is added macroporous resin adsorption, collect lower column liquid, water-pure gradient elution is collected alcohol eluen;
3) alcohol eluen total saponins purification: with step 2) concentrates small size, adds compression leg in the magnesium oxide, the ethyl acetate-ethanol gradient elution is collected the saponin flow point and is concentrated small size, adds the ether precipitating, the precipitating thing leaches dissolve with ethanol crystallization 2-3 time, is drying to obtain Herba Phyllanthi Urinariae's total saponins;
4) polysaccharide purification: with step 2) lower column liquid is evaporated to density 1.1-1.3, adds ethanol gradient precipitate with ethanol, leaches the precipitate hot water dissolving, the polysaccharide activated carbon column decoloring, destaining solution concentrates and adds the ethanol precipitating, leaches precipitate, and low-temperature vacuum drying promptly gets Omithogalum caudatum polysaccharide.
2. according to the joint production process of the described Herba Phyllanthi Urinariae's total saponins of claim 1, polysaccharide, it is characterized in that clarifier is the ZTC-II clarifier in the step 1), consumption 1-3 ‰.
3. according to the joint production process of the described Herba Phyllanthi Urinariae's total saponins of claim 1, polysaccharide, it is characterized in that step 2) in a kind of among the optional D101 of macroporous resin, AB-8 and the HP100.
4. according to the joint production process of the described Herba Phyllanthi Urinariae's total saponins of claim 1, polysaccharide, it is characterized in that step 2) it is middle that water-pure gradient elution is that 6-8 times of column volume washed 5-6 times of column volume 50-70% ethanol elution again.
5. according to the joint production process of the described Herba Phyllanthi Urinariae's total saponins of claim 1, polysaccharide, it is characterized in that the ethyl acetate-ethanol gradient elution is 8-10 times of column volume eluent ethyl acetate 4-8 times of column volume 50-90% ethanol elution again in the step 3).
6. according to the joint production process of the described Herba Phyllanthi Urinariae's total saponins of claim 1, polysaccharide, it is characterized in that crystallization condition is in the step 3): the 90-99% alcohol reflux dissolves, and is recycled to the 1/2-1/3 of original volume, leaves standstill crystallization.
7. according to the joint production process of the described Herba Phyllanthi Urinariae's total saponins of claim 1, polysaccharide, it is characterized in that the gradient precipitate with ethanol is three gradients of final concentration of alcohol 90%-70%-50% in the step 4).
CN2010101568428A 2010-04-27 2010-04-27 Process for co-producing total saponins and polysaccharide from star-of-Bethlehem Pending CN101879265A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102911282A (en) * 2012-11-02 2013-02-06 龙岩嘉麒生物科技有限公司 Decolorization and deproteinization process of mesona chinensis benth polysaccharide solution
CN104188030A (en) * 2014-07-24 2014-12-10 刘山玉 Health drink
CN112299810A (en) * 2019-07-25 2021-02-02 孔德奎 Assembled building heat-insulation wallboard and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102911282A (en) * 2012-11-02 2013-02-06 龙岩嘉麒生物科技有限公司 Decolorization and deproteinization process of mesona chinensis benth polysaccharide solution
CN102911282B (en) * 2012-11-02 2014-12-17 龙岩嘉麒生物科技有限公司 Decolorization and deproteinization process of mesona chinensis benth polysaccharide solution
CN104188030A (en) * 2014-07-24 2014-12-10 刘山玉 Health drink
CN112299810A (en) * 2019-07-25 2021-02-02 孔德奎 Assembled building heat-insulation wallboard and preparation method thereof

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Application publication date: 20101110