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 PDFInfo
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- 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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- polysaccharide
- total saponins
- ethanol
- herba phyllanthi
- phyllanthi urinariae
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- 150000007949 saponins Chemical class 0.000 title claims abstract description 58
- 235000017709 saponins Nutrition 0.000 title claims abstract description 58
- 150000004676 glycans Polymers 0.000 title claims abstract description 42
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 42
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 42
- 150000004804 polysaccharides Polymers 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title abstract description 11
- 241000499865 Ornithogalum Species 0.000 title abstract description 4
- 235000016547 Ornithogalum umbellatum Nutrition 0.000 title abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 112
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000011347 resin Substances 0.000 claims abstract description 22
- 229920005989 resin Polymers 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims description 25
- 239000012141 concentrate Substances 0.000 claims description 23
- XEKOWRVHYACXOJ-UHFFFAOYSA-N acetic acid ethyl ester Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 18
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims description 18
- 238000010828 elution Methods 0.000 claims description 17
- 238000002425 crystallisation Methods 0.000 claims description 16
- 230000005712 crystallization Effects 0.000 claims description 16
- 230000001376 precipitating Effects 0.000 claims description 16
- 238000000746 purification Methods 0.000 claims description 14
- 238000004062 sedimentation Methods 0.000 claims description 13
- 239000003480 eluent Substances 0.000 claims description 12
- 239000000284 extract Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 11
- -1 1-2 hour Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- LJQKCYFTNDAAPC-UHFFFAOYSA-N ethanol;ethyl acetate Chemical compound CCO.CCOC(C)=O LJQKCYFTNDAAPC-UHFFFAOYSA-N 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000007906 compression Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 12
- 239000003795 chemical substances by application Substances 0.000 abstract description 7
- 238000000605 extraction Methods 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 229940023032 Activated Charcoal Drugs 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract description 2
- 238000001953 recrystallisation Methods 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 6
- 229960000935 Dehydrated Alcohol Drugs 0.000 description 5
- 230000001476 alcoholic Effects 0.000 description 5
- 239000000470 constituent Substances 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- 230000003068 static Effects 0.000 description 5
- 230000001093 anti-cancer Effects 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 2
- QGJOPFRUJISHPQ-UHFFFAOYSA-N carbon bisulphide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000000287 crude extract Substances 0.000 description 2
- 238000002481 ethanol extraction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N AI2O3 Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 206010006187 Breast cancer Diseases 0.000 description 1
- VSJKWCGYPAHWDS-FQEVSTJZSA-N Camptothecin Chemical compound C1=CC=C2C=C(CN3C4=CC5=C(C3=O)COC(=O)[C@]5(O)CC)C4=NC2=C1 VSJKWCGYPAHWDS-FQEVSTJZSA-N 0.000 description 1
- 240000009087 Crescentia cujete Species 0.000 description 1
- 235000005983 Crescentia cujete Nutrition 0.000 description 1
- 240000003361 Drimia maritima Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- RCINICONZNJXQF-MZXODVADSA-N Intaxel Chemical compound O([C@@H]1[C@@]2(C[C@@H](C(C)=C(C2(C)C)[C@H](C([C@]2(C)[C@@H](O)C[C@H]3OC[C@]3([C@H]21)OC(C)=O)=O)OC(=O)C)OC(=O)[C@H](O)[C@@H](NC(=O)C=1C=CC=CC=1)C=1C=CC=CC=1)O)C(=O)C1=CC=CC=C1 RCINICONZNJXQF-MZXODVADSA-N 0.000 description 1
- 235000009797 Lagenaria vulgaris Nutrition 0.000 description 1
- GUWSLQUAAYEZAF-UHFFFAOYSA-L Lead(II) acetate Chemical compound O1C(C)=O[Pb]21O=C(C)O2 GUWSLQUAAYEZAF-UHFFFAOYSA-L 0.000 description 1
- 241000234280 Liliaceae Species 0.000 description 1
- 206010058467 Lung neoplasm malignant Diseases 0.000 description 1
- 208000003747 Lymphoid Leukemia Diseases 0.000 description 1
- 229920002521 Macromolecule Polymers 0.000 description 1
- 241000233855 Orchidaceae Species 0.000 description 1
- 240000000654 Ornithogalum longebracteatum Species 0.000 description 1
- 229960001592 Paclitaxel Drugs 0.000 description 1
- VXMKYRQZQXVKGB-CWWHNZPOSA-N Tannin Chemical compound O([C@H]1[C@H]([C@@H]2OC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)O[C@H]([C@H]2O)O1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 VXMKYRQZQXVKGB-CWWHNZPOSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003110 anti-inflammatory Effects 0.000 description 1
- 201000008275 breast carcinoma Diseases 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002026 chloroform extract Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 229940079593 drugs Drugs 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229940046892 lead acetate Drugs 0.000 description 1
- 201000006439 lymphocytic leukemia Diseases 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002965 rope Substances 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 229930003347 taxol Natural products 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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
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).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2010101568428A CN101879265A (en) | 2010-04-27 | 2010-04-27 | Process for co-producing total saponins and polysaccharide from star-of-Bethlehem |
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| CN2010101568428A CN101879265A (en) | 2010-04-27 | 2010-04-27 | Process for co-producing total saponins and polysaccharide from star-of-Bethlehem |
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Cited By (3)
| 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 |
-
2010
- 2010-04-27 CN CN2010101568428A patent/CN101879265A/en active Pending
Cited By (4)
| 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 |