CN102229684B - Synthesizing method for separated and purified special resin for assembled flavone of rhizome drynaria - Google Patents
Synthesizing method for separated and purified special resin for assembled flavone of rhizome drynaria Download PDFInfo
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- CN102229684B CN102229684B CN2011101211398A CN201110121139A CN102229684B CN 102229684 B CN102229684 B CN 102229684B CN 2011101211398 A CN2011101211398 A CN 2011101211398A CN 201110121139 A CN201110121139 A CN 201110121139A CN 102229684 B CN102229684 B CN 102229684B
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Abstract
The invention discloses a synthesizing method for a separated and purified special resin for an assembled flavone of rhizome drynaria. in the synthesizing method,: divinylbenzene is taken as a cross-linking agent, GMA (glycidyl methacrylate) and methyl acrylate are taken as monomers, benzoyl peroxide is taken as an initiator, toluene and liquid paraffin wax are taken as a mixed hole-making reagent. The method comprises the following steps: mixing the materials into water and then stirring and aggregating; washing with water; washing with ethanol; repeatedly washing with water; centrifuging; and lastly using a wet column-filling method to fill the centrifuged resin into a resin column and leaching the resin column with an ethanol solution of sodium hydroxide, thereby acquiring the separated and purified special resin for the assembled flavone of rhizome drynaria. The separated and purified special resin for the assembled flavone of rhizome drynaria provided by the invention has the advantages that the stability is higher, the absorption capacity is high, the resin is easily cleaned, and the selectivity is high.
Description
Technical field
The present invention relates to a kind of compound method of resin, the resin dedicated compound method of particularly a kind of separation and purification Rhizome of Fortune's Drynaria total flavones.
Background technology
The Rhizome of Fortune's Drynaria resource is abundanter, have strengthen muscles and bones, the function of supplementing the kidney to control the nocturnal, blood stasis removing analgesic.Be used for that treatment is suffered from a deficiency of the kidney, treating rheumatic ostealgia, wound, dysentery etc.Present Rhizome of Fortune's Drynaria is used for medicine and has caused people's attention; Drug effect is fine; There is poor selectivity in resin in the market aspect the separation Rhizoma Drynariae active principle; The shortcoming that loading capacity decline is fast, the resin of therefore developing a kind of fine separation and purification Rhizome of Fortune's Drynaria total flavones has crucial meaning.
Summary of the invention
The invention provides the resin dedicated compound method of a kind of separation and purification Rhizome of Fortune's Drynaria total flavones.
For solving the problems of the technologies described above, the method steps that the present invention takes is following:
(1) preparation of oil phase
Get 50-60 part industry divinylbenzene, 35-45 part methyl acrylate, 2-8 part GMA by weight; 0.5-2 a part Lucidol mixes; Add the mixing perforating agent that 100-120 part is made up of toluene and whiteruss; Obtain oil phase with mixing under the above-mentioned several kinds of material normal temperature, the mass ratio of toluene and whiteruss is 0.5-1.5:0.5-1.5.
Preferably; At the phase time that makes up oil; Get 55 parts of industrial divinylbenzenes, 40 parts of methyl acrylates, 5 parts of GMA by weight, 1 part of Lucidol mixes, and adds 110 parts of mixing perforating agents of being made up of toluene and whiteruss; Obtain oil phase with mixing under the above-mentioned several kinds of material normal temperature, the mass ratio of toluene and whiteruss is 1:1.
(2) preparation of water
With massfraction is that 0.2% Z 150PH, massfraction are that to join massfraction be to make water in 2.5% sodium chloride aqueous solution to 0.5% gelatin; With above-mentioned water heating in water bath to 45-55 ℃; The mass ratio of said Z 150PH, gelatin and sodium chloride aqueous solution is 1-3:4-6:18-22, and the quality of said water is 3-4 a times of oil phase quality.
Preferably with water heating in water bath to 50 ℃.
(3) above-mentioned oil phase is joined the aqueous phase in the step (2); Agitator, the control stirring velocity is disperseed oil phase and oil bead diameter is controlled between the 20-60 order; At the uniform velocity be warming up to 67-69 ℃ of insulation with 0.5-1 hour finalized the design in 1.5-2.5 hour; At the uniform velocity be warmed up to 76-78 ℃ of insulation 3-5 hour with 0.5-1 hour again, at the uniform velocity be warmed up to 83-85 ℃ of insulation 1.5-2.5 hour with 0.25-0.75 hour again, at the uniform velocity be warmed up to 89-91 ℃ with 0.2-0.5 hour at last and be incubated 10-14 hour; Make polymerization complete, obtain the resin raw product.
(4) with the above-mentioned resin raw product of 75-85 ℃ water thorough washing, till effluent is limpid.
(5) with above-mentioned resin raw product dress post through water washing, it is not muddy to add water with the abundant extracting of ethanol to effluent.
(6) the resin raw product that step (5) is obtained is used washing, and detecting with Ebullioscope to effluent does not have alcoholic strength to get wet resin.
(7) wet resin of step (6) is carried out centrifugal, centrifugal condition is 1800-2200r/min, centrifugal 5 minutes.
(8) above-mentioned wet resin after centrifugal is packed in internal diameter 0.8-1.0 centimetre the resin column with wet method; Using massfraction is ethanolic soln drip washing 2-3 hour slowly of 2% sodium hydroxide; Flow velocity is 1BV/h, and water is washed till effluent to be that neutrality obtains separation and purification Rhizome of Fortune's Drynaria total flavones resin dedicated then.
The present invention has following remarkable advantage:
This resin is the resin dedicated of a kind of separation and purification Rhizome of Fortune's Drynaria total flavones, and the polarity of resin has very big advantage with the aperture for separating the Rhizome of Fortune's Drynaria flavones, this resin compare with other products on the market stability and selectivity all high.The structural unit that the monomer whose polymerization forms contains hydrophobic benzene rings; Can with the phenyl ring generation hydrophobic interaction in the effective ingredients in plant; On weak hydrophobic framework, add GMA and methacrylate monomer simultaneously; Make resin keep the Rhizome of Fortune's Drynaria flavonoid compound high loading capacity special with synergy adsorption mechanism hydrogen bond to structure with hydrophobic; In the weakening system greatly simple with hydrophobic interaction by the adsorptive power of the impurity of resin absorption, reach and improve the purpose of resin Rhizome of Fortune's Drynaria flavones adsorption selectivity.Consumption comprehensive regulation through adjustment GMA and methyl acrylate resin hydrophobic reactive force intensity and polar big or small.Regulated and control the pore diameter range of resin through the ratio of regulating and control two kinds of pore-creating agents, made it higher separating Rhizome of Fortune's Drynaria flavones selectivity.This resin elution is easy, and kinetics of adsorption is functional.Acid under heat, organic solvent and the average operating, alkali are stablized, so work-ing life is longer.Albumen, carbohydrate, mineral acid, alkali, salt, small molecules hydrophilic organics hydrophilicity are not all adsorbed, thereby can be with Rhizoma Drynariae active principle and these separating substances.
Embodiment:
Embodiment 1
(1) gets 55g industry divinylbenzene, 40g methyl acrylate, 5gGMA, 1g Lucidol and mix, add 55g toluene and 55g whiteruss, obtain oil phase mixing under the above-mentioned several kinds of material normal temperature.
(2) with the 55g massfraction be 0.2% Z 150PH, 137g massfraction be 0.5% gelatin join the 547g massfraction be in 2.5% the sodium chloride aqueous solution as water, heating in water bath to 50 ℃.
(3) oil phase is joined aqueous phase, agitator, control stirring velocity; Make the oil phase dispersion and oil bead diameter is controlled at 60 orders, at the uniform velocity be warming up to 69 ℃ of insulations with 1 hour and finalized the design in 2 hours, at the uniform velocity be warmed up to 78 ℃ with 1 hour again and be incubated 4 hours; At the uniform velocity be warmed up to 85 ℃ with 0.75 hour again and be incubated 2 hours; At the uniform velocity be warmed up to 91 ℃ of insulations 12 hours with 0.5 hour at last, make polymerization complete, obtain the resin raw product.
(4) with the above-mentioned resin raw product of 80 ℃ water thorough washing, till effluent is limpid.
(5) with above-mentioned resin raw product dress post through water washing, it is not muddy to add water with the abundant extracting of ethanol to effluent.
(6) the resin raw product that step (5) is obtained is used washing, and detecting with Ebullioscope to effluent does not have alcoholic strength to get wet resin.
(7) wet resin of step (6) is carried out centrifugal, centrifugal condition is 2200r/min, centrifugal 5 minutes.
(8) above-mentioned resin after centrifugal is packed in the resin column of 1.0 centimetres of internal diameters with wet method; Using massfraction is the ethanolic soln drip washing resin 3 hours slowly of 2% sodium hydroxide; Flow velocity is 1BV/h, and water is washed till effluent to be that neutrality obtains separation and purification Rhizome of Fortune's Drynaria total flavones resin dedicated then.
Embodiment 2
(1) gets 55g industry divinylbenzene, 40g methyl acrylate, 5gGMA, 1g Lucidol and mix, add 55g toluene and 55g whiteruss, obtain oil phase mixing under the above-mentioned several kinds of material normal temperature.
(2) with the 47g massfraction be 0.2% Z 150PH, 118g massfraction be 0.5% gelatin join the 469g massfraction be in 2.5% the sodium chloride aqueous solution as water, heating in water bath to 45 ℃.
(3) oil phase is joined aqueous phase, agitator, control stirring velocity; Make the oil phase dispersion and oil bead diameter is controlled at 20 orders, at the uniform velocity be warming up to 67 ℃ of insulations with 0.5 hour and finalized the design in 1.5 hours, at the uniform velocity be warmed up to 76 ℃ with 0.5 hour again and be incubated 3 hours; At the uniform velocity be warmed up to 83 ℃ with 0.25 hour again and be incubated 1.5 hours; At the uniform velocity be warmed up to 89 ℃ of insulations 10 hours with 0.2 hour at last, make polymerization complete, obtain the resin raw product.
(4) with the above-mentioned resin raw product of 75 ℃ water thorough washing, till effluent is limpid.
(5) with above-mentioned resin raw product dress post through water washing, it is not muddy to add water with the abundant extracting of ethanol to effluent.
(6) the resin raw product that step (5) is obtained is used washing, and detecting with Ebullioscope to effluent does not have alcoholic strength to get wet resin.
(7) wet resin of step (6) is carried out centrifugal, centrifugal condition is 1800r/min, centrifugal 5 minutes.
(8) above-mentioned resin after centrifugal is packed in the resin column of 0.8 centimetre of internal diameter with wet method; Using massfraction is the ethanolic soln drip washing resin 2 hours slowly of 2% sodium hydroxide; Flow velocity is 1BV/h, and water is washed till effluent to be that neutrality obtains separation and purification Rhizome of Fortune's Drynaria total flavones resin dedicated then.
Embodiment 3
(1) gets 55g industry divinylbenzene, 40g methyl acrylate, 5gGMA, 1g Lucidol and mix, add 55g toluene and 55g whiteruss, obtain oil phase mixing under the above-mentioned several kinds of material normal temperature.
(2) with the 55g massfraction be 0.2% Z 150PH, 137g massfraction be 0.5% gelatin join the 547g massfraction be in 2.5% the sodium chloride aqueous solution as water, heating in water bath to 55 ℃.
(3) oil phase is joined aqueous phase, agitator, control stirring velocity; Make the oil phase dispersion and oil bead diameter is controlled at 60 orders, at the uniform velocity be warming up to 69 ℃ of insulations with 1 hour and finalized the design in 2.5 hours, at the uniform velocity be warmed up to 78 ℃ with 1 hour again and be incubated 5 hours; At the uniform velocity be warmed up to 85 ℃ with 0.75 hour again and be incubated 2.5 hours; At the uniform velocity be warmed up to 91 ℃ of insulations 14 hours with 0.5 hour at last, make polymerization complete, obtain the resin raw product.
(4) with the above-mentioned resin raw product of 85 ℃ water thorough washing, till effluent is limpid.
(5) with above-mentioned resin raw product dress post through water washing, it is not muddy to add water with the abundant extracting of ethanol to effluent.
(6) the resin raw product that step (5) is obtained is used washing, and detecting with Ebullioscope to effluent does not have alcoholic strength to get wet resin.
(7) wet resin of step (6) is carried out centrifugal, centrifugal condition is 2200r/min, centrifugal 5 minutes.
(8) above-mentioned resin after centrifugal is packed in the resin column of 1.0 centimetres of internal diameters with wet method; Using massfraction is the ethanolic soln drip washing resin 3 hours slowly of 2% sodium hydroxide; Flow velocity is 1BV/h, and water is washed till effluent to be that neutrality obtains separation and purification Rhizome of Fortune's Drynaria total flavones resin dedicated then.
Embodiment 4
(1) gets 55g industry divinylbenzene, 40g methyl acrylate, 5gGMA, 1g Lucidol and mix, add 55g toluene and 55g whiteruss, obtain oil phase mixing under the above-mentioned several kinds of material normal temperature.
(2) with the 62g massfraction be 0.2% Z 150PH, 156g massfraction be 0.5% gelatin join the 625g massfraction be in 2.5% the sodium chloride aqueous solution as water, heating in water bath to 50 ℃.
(3) oil phase is joined aqueous phase, agitator, control stirring velocity; Oil phase is disperseed and oil bead diameter is controlled between 40 orders, at the uniform velocity be warming up to 68 ℃ of insulations typing in 2 hours with 0.75 hour, at the uniform velocity be warmed up to 77 ℃ with 0.75 hour again and be incubated 4 hours; At the uniform velocity be warmed up to 84 ℃ with 0.5 hour again and be incubated 2 hours; At the uniform velocity be warmed up to 90 ℃ of insulations 12 hours with 0.35 hour at last, make polymerization complete, obtain the resin raw product.
(4) with the above-mentioned resin raw product of 80 ℃ water thorough washing, till effluent is limpid.
(5) with above-mentioned resin raw product dress post through water washing, it is not muddy to add water with the abundant extracting of ethanol to effluent.
(6) the resin raw product that step (5) is obtained is used washing, and detecting with Ebullioscope to effluent does not have alcoholic strength to get wet resin.
(7) wet resin of step (6) is carried out centrifugal, centrifugal condition is 2000r/min, centrifugal 5 minutes.
(8) above-mentioned resin after centrifugal is packed in the resin column of 0.9 centimetre of internal diameter with wet method; Using massfraction is the ethanolic soln drip washing resin 2.5 hours slowly of 2% sodium hydroxide; Flow velocity is 1BV/h, and water is washed till effluent to be that neutrality obtains separation and purification Rhizome of Fortune's Drynaria total flavones resin dedicated then.
Embodiment 5
(1) gets 50g industry divinylbenzene, 35g methyl acrylate, 2gGMA, 0.5g Lucidol and mix, add 25g toluene and 75g whiteruss, obtain oil phase mixing under the above-mentioned several kinds of material normal temperature.
(2) with the 26g massfraction be 0.2% Z 150PH, 155g massfraction be 0.5% gelatin join the 569g massfraction be in 2.5% the sodium chloride aqueous solution as water, heating in water bath to 50 ℃.
(3) oil phase is joined aqueous phase, agitator, control stirring velocity; Oil phase is disperseed and oil bead diameter is controlled between 40 orders, at the uniform velocity be warming up to 68 ℃ of insulations typing in 2 hours with 1 hour, at the uniform velocity be warmed up to 77 ℃ with 1 hour again and be incubated 4 hours; At the uniform velocity be warmed up to 84 ℃ with 0.5 hour again and be incubated 2 hours; At the uniform velocity be warmed up to 90 ℃ of insulations 12 hours with 0.5 hour at last, make polymerization complete, obtain the resin raw product.
(4) with the above-mentioned resin raw product of 80 ℃ water thorough washing, till effluent is limpid.
(5) with above-mentioned resin raw product dress post through water washing, it is not muddy to add water with the abundant extracting of ethanol to effluent.
(6) the resin raw product that step (5) is obtained is used washing, and detecting with Ebullioscope to effluent does not have alcoholic strength to get wet resin.
(7) wet resin of step (6) is carried out centrifugal, centrifugal condition is 2000r/min, centrifugal 5 minutes.
(8) above-mentioned resin after centrifugal is packed in the resin column of 1.0 centimetres of internal diameters with wet method; Using massfraction is the ethanolic soln drip washing resin 2.5 hours slowly of 2% sodium hydroxide; Flow velocity is 1BV/h, and water is washed till effluent to be that neutrality obtains separation and purification Rhizome of Fortune's Drynaria total flavones resin dedicated then.
Embodiment 6
(1) gets 60g industry divinylbenzene, 45g methyl acrylate, 8gGMA, 2g Lucidol and mix, add 90g toluene and 30g whiteruss, obtain oil phase mixing under the above-mentioned several kinds of material normal temperature.
(2) with the 113g massfraction be 0.2% Z 150PH, 150g massfraction be 0.5% gelatin join the 677g massfraction be in 2.5% the sodium chloride aqueous solution as water, heating in water bath to 50 ℃.
(3) oil phase is joined aqueous phase, agitator, control stirring velocity; Oil phase is disperseed and oil bead diameter is controlled between 40 orders, at the uniform velocity be warming up to 68 ℃ of insulations typing in 2 hours with 0.75 hour, at the uniform velocity be warmed up to 77 ℃ with 0.75 hour again and be incubated 4 hours; At the uniform velocity be warmed up to 84 ℃ with 0.5 hour again and be incubated 2 hours; At the uniform velocity be warmed up to 90 ℃ of insulations 12 hours with 0.35 hour at last, make polymerization complete, obtain the resin raw product.
(4) with the above-mentioned resin raw product of 80 ℃ water thorough washing, till effluent is limpid.
(5) with above-mentioned resin raw product dress post through water washing, it is not muddy to add water with the abundant extracting of ethanol to effluent.
(6) the resin raw product that step (5) is obtained is used washing, and detecting with Ebullioscope to effluent does not have alcoholic strength to get wet resin.
(7) wet resin of step (6) is carried out centrifugal, centrifugal condition is 2000r/min, centrifugal 5 minutes.
(8) above-mentioned resin after centrifugal is packed in the resin column of 0.9 centimetre of internal diameter with wet method; Using massfraction is the ethanolic soln drip washing resin 2.5 hours slowly of 2% sodium hydroxide; Flow velocity is 1BV/h, and water is washed till effluent to be that neutrality obtains separation and purification Rhizome of Fortune's Drynaria total flavones resin dedicated then.
Embodiment 7
Take by weighing a certain amount of Rhizome of Fortune's Drynaria medicinal material, add the process water (through the water of reverse-osmosis treated) of 10 times of amounts, boil and extract 1h, extract altogether 3 times, merge No. 3 times extracting solution, vacuum filtration.The control pH value is that resin and the commercial resins of utilizing embodiment 1 to prepare under the condition of 4.0-4.5 are extracted, and the flow velocity of control extracting solution is 2-3BV/h; Use deionized water rinsing then, flow velocity is 2-3BV/h; Carry out desorb with 50% ethanol; Light absorption value according to spectrophotometry desorb thing, calculate dried cream yield and general flavone content, data such as table 1:
The resin that the application makes selectivity and stable aspect higher than commercial resins.
Claims (3)
1. resin dedicated compound method of separation and purification Rhizome of Fortune's Drynaria total flavones is characterized in that may further comprise the steps:
(1) preparation of oil phase
Get 50-60 part industry divinylbenzene, 35-45 part methyl acrylate, 2-8 part GMA by weight; 0.5-2 a part Lucidol mixes; Add the mixing perforating agent that 100-120 part is made up of toluene and whiteruss; Obtain oil phase with mixing under the above-mentioned several kinds of material normal temperature, the mass ratio of toluene and whiteruss is 0.5-1.5:0.5-1.5;
(2) preparation of water
With massfraction is that 0.2% Z 150PH, massfraction are that to join massfraction be to make water in 2.5% sodium chloride aqueous solution to 0.5% gelatin; With above-mentioned water heating in water bath to 45-55 ℃; The mass ratio of said Z 150PH, gelatin and sodium chloride aqueous solution is 1-3:4-6:18-22, and the quality of said water is 3-4 a times of oil phase quality;
(3) above-mentioned oil phase is joined the aqueous phase in the step (2); Agitator, the control stirring velocity is disperseed oil phase and oil bead diameter is controlled between the 20-60 order; At the uniform velocity be warming up to 67-69 ℃ of insulation with 0.5-1 hour finalized the design in 1.5-2.5 hour; At the uniform velocity be warmed up to 76-78 ℃ of insulation 3-5 hour with 0.5-1 hour again, at the uniform velocity be warmed up to 83-85 ℃ of insulation 1.5-2.5 hour with 0.25-0.75 hour again, at the uniform velocity be warmed up to 89-91 ℃ with 0.2-0.5 hour at last and be incubated 10-14 hour; Make polymerization complete, obtain the resin raw product;
(4) with the above-mentioned resin raw product of 75-85 ℃ water thorough washing, till effluent is limpid;
(5) with above-mentioned resin raw product dress post through water washing, it is not muddy to add water with the abundant extracting of ethanol to effluent;
(6) the resin raw product that step (5) is obtained is used washing, and detecting with Ebullioscope to effluent does not have alcoholic strength to get wet resin;
(7) wet resin of step (6) is carried out centrifugal, centrifugal condition is 1800-2200r/min, centrifugal 5 minutes;
(8) above-mentioned wet resin after centrifugal is packed in internal diameter 0.8-1.0 centimetre the resin column with wet method; Using massfraction is ethanolic soln drip washing 2-3 hour slowly of 2% sodium hydroxide; Flow velocity is 1BV/h, and water is washed till effluent to be that neutrality obtains separation and purification Rhizome of Fortune's Drynaria total flavones resin dedicated then.
2. the resin dedicated compound method of a kind of according to claim 1 separation and purification Rhizome of Fortune's Drynaria total flavones is characterized in that, with water heating in water bath to 50 ℃.
3. the resin dedicated compound method of a kind of according to claim 1 separation and purification Rhizome of Fortune's Drynaria total flavones; It is characterized in that,, get 55 parts of industrial divinylbenzenes, 40 parts of methyl acrylates, 5 parts of GMA by weight at the phase time that makes up oil; 1 part of Lucidol mixes; Add 110 parts of mixing perforating agents of being made up of toluene and whiteruss, obtain oil phase with mixing under the above-mentioned several kinds of material normal temperature, the mass ratio of toluene and whiteruss is 1:1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101211398A CN102229684B (en) | 2011-05-11 | 2011-05-11 | Synthesizing method for separated and purified special resin for assembled flavone of rhizome drynaria |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101211398A CN102229684B (en) | 2011-05-11 | 2011-05-11 | Synthesizing method for separated and purified special resin for assembled flavone of rhizome drynaria |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148486A (en) * | 2007-10-25 | 2008-03-26 | 刘文韬 | Micro/nano level mesoporous structure substance with biological affinity and forming method thereof |
| CN101200516A (en) * | 2007-11-30 | 2008-06-18 | 天津市中宝制药有限公司 | Polar macroporous adsorption resin and method for synthesizing the same |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100849253B1 (en) * | 2000-12-29 | 2008-07-29 | 키후앙 파마슈티컬 테크놀러지 앤드 인베스트먼트 씨오.,엘티디 | Drynaria extractions for treating osteoporosis and their extraction process |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148486A (en) * | 2007-10-25 | 2008-03-26 | 刘文韬 | Micro/nano level mesoporous structure substance with biological affinity and forming method thereof |
| CN101200516A (en) * | 2007-11-30 | 2008-06-18 | 天津市中宝制药有限公司 | Polar macroporous adsorption resin and method for synthesizing the same |
Non-Patent Citations (1)
| Title |
|---|
| 张全香 等.大孔吸附树脂纯化骨碎补总黄酮的研究.《中草药》.2011,第42卷(第4期),第708-709页. * |
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Denomination of invention: Synthesizing method for separated and purified special resin for assembled flavone of rhizome drynaria Effective date of registration: 20160823 Granted publication date: 20120801 Pledgee: Xianxian County Hebei rural commercial bank Limited by Share Ltd Pledgor: Cangzhou Bon Adsorber Technology Co.,Ltd. Registration number: 2016990000727 |
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