CN103330754B - Method for extracting total anthraquinone from fresh rheum officinale - Google Patents
Method for extracting total anthraquinone from fresh rheum officinale Download PDFInfo
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- CN103330754B CN103330754B CN201310243667.XA CN201310243667A CN103330754B CN 103330754 B CN103330754 B CN 103330754B CN 201310243667 A CN201310243667 A CN 201310243667A CN 103330754 B CN103330754 B CN 103330754B
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Abstract
The invention relates to a method for extracting total anthraquinone from fresh rheum officinale. The method comprises the following steps of: (1) preparing freshly ground rheum officinale pulp; (2) degradation of complex enzyme, namely regulating the pH value of the freshly ground rheum officinale pulp with hydrochloric acid or sodium carbonate, adding extraction enzyme for enzymolysis, and then centrifuging to obtain supernate; (3) pretreatment of macroporous resin, namely adsorbing the macroporous resin with an ethanol solution, and then eluting to obtain treated macroporous resin; (4) adsorption of the treated macroporous resin, namely adding the supernate into the treated macroporous resin for adsorbing and separating, eluting with ethanol, and regulating the pH value with hydrochloric acid to obtain an eluent; (5) carrying out decompression concentration on the eluent to obtain an anthraquinone glycoside compound, and carrying out acidolysis and drying on the anthraquinone glycoside compound to constant weight to obtain a free anthraquinone compound; (6) adding chloroform into the free anthraquinone compound for ultrasonic extraction to obtain a water phase and chloroform layer; and (7) carrying out washing, decompression concentration and crystallization on the chloroform layer to obtain coarse yellow anthraquinone product. By virtue of the method, the production cost can be effectively lowered, and the yield can be effectively improved.
Description
Technical field
The present invention relates to Chinese crude drug and extract and separation technology field, relate in particular to a kind of method of extracting general anthraquinone from new fresh Radix et Rhizoma Rhei.
Background technology
Radix Et Rhizoma Rhei bitter in the mouth, cold in nature, has the effect of heat and toxic materials clearing away, clearing away heat-fire, removing pathogenic heat from blood and toxic substance from the body, eliminating blood stasis and inducing menstruation, dampness removing jaundice eliminating, is a kind of natural medicinal plant with valuable pharmacological effect.Modern pharmacology research shows, Radix Et Rhizoma Rhei also has broad-spectrum antiseptic, hepatic cholagogic, heart tonifying, blood pressure lowering, antitumor, hyperlipidemia disease, immunomodulating, removing free radical, accelerates early osteocyte differentiation, diuresis, improves renal function, improves many-sided effects such as immunity.The main effective ingredient of Radix Et Rhizoma Rhei is anthraquinone derivatives; as chrysophanic acid, emodin, chrysophanol, physcione and aloe-emodin etc.; there is physiologically active widely; cardiovascular system, central nervous system, blood circulation etc. are all had to effect, can be used for antiinflammatory, antibacterial, protect Liver and kidney, remove free radical, improve microcirculation etc.Anthraquinone derivative claims general anthraquinone, comprises free fear quinone and combined anthraquinone.Dissociated anthraquinone is insoluble in water, is dissolved in the organic solvents such as ethanol, chloroform, and the organic solvent such as combined anthraquinone hydrophilic is strong, and soluble in water, ethanol, is insoluble in ether, chloroform.At present, Radix Et Rhizoma Rhei has been used to the fields such as medicine, foods and cosmetics.
Traditional Radix Et Rhizoma Rhei preliminary working method for excavating, rossing, section, dry in the sun, takes a lot of work consuming time, workload is very large, Radix Et Rhizoma Rhei collecting season is on the occasion of local rainy season simultaneously, causes the Radix Et Rhizoma Rhei of gathering can not be drying in time, a large amount of moldy metamorphisms, have a strong impact on root yield and quality; Part medicinal herb grower adopts heated kang to dry and consumes a large amount of fire coals, increase cost, consumes the energy, contaminated environment.
And the fresh technology of squeezing the juice is a kind of innovative preliminary working technology, without drying, greatly reduce labor cost, reduce energy consumption, reduce the production cycle, avoid again in drying process the destruction of medicinal ingredient and reduction simultaneously.
Macroporous adsorbent resin has loose structure and very high specific surface area, and optionally adsorb organic compound, has the advantages such as selectivity is good, mechanical strength is high, Regeneration Treatment is convenient, adsorption rate is fast, and aspect the extraction of Chinese medicine, purification, using value is higher.But the macroporous adsorbent resin of different model has different polarity, aperture, specific surface area, pore volume etc., so its separation, concentration effect are also different.Meanwhile, in purge process, be also subject to the impact of the factors such as eluant kind, concentration, volume, program, flow velocity.
At present, domestic total Radix Et Rhizoma Rhei anthraquinone extraction and separation process adopts organic solvent reflux extraction method more, has no " the fresh technology of squeezing the juice ", " complex enzyme degradation technology ", " macroporous adsorption resin technology " and combines and use the relevant report of extracting purification anthraquinone component.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of general anthraquinone of extracting from new fresh Radix et Rhizoma Rhei that reduces production costs, improves yield.
For addressing the above problem, a kind of method of extracting general anthraquinone from new fresh Radix et Rhizoma Rhei of the present invention, comprises the following steps:
(1) prepare the fresh grinding slurry of Radix Et Rhizoma Rhei:
Roots and stems of rhubarb is cleaned to silt, remove the peel, and cut into the fritter of 1 * 1 cm; Then, the Radix Et Rhizoma Rhei being cut into small pieces is added to water by the solid-liquid ratio of 1kg:5L ~ 20L, with fiberizer, wear into after uniform serosity and cross 10 ~ 300 mesh sieves, obtain the fresh grinding slurry of Radix Et Rhizoma Rhei;
(2) complex enzyme degradation:
The sodium carbonate that the hydrochloric acid that is 2% by mass concentration by the fresh grinding slurry of described Radix Et Rhizoma Rhei or mass concentration are 2% regulates pH value to 2.4 ~ 8.6 o'clock, in the fresh grinding slurry of described Radix Et Rhizoma Rhei, by 20 ~ 125mg/L, add extraction enzyme, enzymolysis 12 ~ 72h at 20 ~ 65 ℃ of temperature, then with centrifugal 5 ~ 25 min of speed of 2000 ~ 4000 rpm, obtain supernatant;
(3) macroporous resin pretreatment:
The alcoholic solution that is 50% ~ 95% by mass concentration by macroporous resin absorption 12 ~ 48 h, the alcoholic solution that is then 10% ~ 95% by mass concentration successively and distilled water eluting, until eluent is without muddiness, without alcohol taste, obtain the macroporous resin after processing;
(4) macroporous resin adsorption:
Described supernatant is joined on the macroporous resin after described processing, at every g resin applied sample amount, be to carry out adsorbing separation under 5 ~ 35ml, the flow velocity condition that is 1 ~ 5VB/h, and the ethanol that is 20 ~ 95% by mass concentration carries out eluting, simultaneously, salt acid for adjusting pH value to 2 ~ 11 that are 2% by mass concentration, obtain eluent after 10 ~ 120min;
Described eluent under the pressure of 0.6 ~ 0.8MPa after concentrating under reduced pressure, obtain anthraquinone glycoside compound, the sulphuric acid that this anthraquinone glycoside compound is 10 ~ 40% by 0.1 ~ 1 times of its volume and mass concentration acidolysis 1 ~ 12 hour under 20 ~ 100 ℃ of conditions, drying obtains dissociated anthraquinone compounds to constant weight;
(6) in described dissociated anthraquinone compounds, add chloroform ultrasonic extraction 5 ~ 60 minutes at ambient temperature, after re-extract 3 ~ 5 times, obtain water and chloroform layer; The volume ratio of described dissociated anthraquinone compounds and described chloroform is 1 ml:2 ml ~ 5 ml;
(7) described chloroform layer is washed till chloroform layer with distilled water and is after neutrality, and under the pressure of 0.6 ~ 0.8MPa, after concentrating under reduced pressure, crystallization at normal temperatures obtains Yellow anthraquinone class crude product.
The extraction enzyme of described step in is (2) the compound enzyme being mixed by the mass ratio of 1g:3g ~ 20g:1g ~ 20g:1g ~ 10g by 1,4 beta-glucanase, cellulase, xylanase and pectase.
The macroporous resin of described step in (3) refers to cation exchange type macroporous adsorbent resin.
The present invention compared with prior art has the following advantages:
1, the present invention is different from the conventional extraction process of traditional Chinese medicine, but being combined to use, " the fresh technology of squeezing the juice ", " complex enzyme degradation technology ", " macroporous adsorption resin technology " extract purification anthraquinone component, pass through impressed pressure, improve the osmotic pressure of cell wall both sides, together with zymolysis technique, under the condition of room temperature, complete extraction, extraction ratio is high, active constituent content and biological activity, compared with the height of traditional handicraft, extract completely mostly.
2, because the direct fresh Radix et Rhizoma Rhei defibrination of the present invention saves the chip drying operation in conventional machining process, therefore, not only reduced production cost, and improved yield.
3, because the present invention utilizes compound enzyme at room temperature, effective degradation of cell wall under normal pressure, therefore, energy savings, performance drug effect.
4, because the present invention utilizes fresh Radix et Rhizoma Rhei defibrination, complex enzyme degradation and resin isolation multiple techniques technique succinct, cost is low, therefore, has both been applicable to large-scale extraction enterprise and has carried out technology upgrading, is conducive to the production of founding the factory of medium and small micro-enterprise, and market popularization value is large.
The specific embodiment
embodiment 1a method of extracting general anthraquinone from new fresh Radix et Rhizoma Rhei, comprises the following steps:
(1) prepare the fresh grinding slurry of Radix Et Rhizoma Rhei:
Roots and stems of rhubarb is cleaned to silt, remove the peel, and cut into the fritter of 1 * 1 cm; Then, the Radix Et Rhizoma Rhei being cut into small pieces is added to water by the solid-liquid ratio of 1kg:5L, with fiberizer, wear into after uniform serosity and cross 10 mesh sieves, obtain the fresh grinding slurry of Radix Et Rhizoma Rhei.
(2) complex enzyme degradation:
Salt acid for adjusting pH value to 2.4 ~ 4.6 o'clock that are 2% by mass concentration by the fresh grinding slurry of Radix Et Rhizoma Rhei add extraction enzyme by 20mg/L in the fresh grinding slurry of Radix Et Rhizoma Rhei, and then enzymolysis 72h at 20 ℃ of temperature with centrifugal 25 min of speed of 2000 rpm, obtains supernatant.
Wherein: extracting enzyme is the compound enzyme being mixed by the mass ratio of 1g:3g:1g:1g by 1,4 beta-glucanase, cellulase, xylanase and pectase.
(3) macroporous resin pretreatment:
Macroporous resin is adsorbed to 48 h with the alcoholic solution that mass concentration is 50%, and the alcoholic solution that is then 10% by mass concentration successively and distilled water eluting, until eluent is without muddiness, without alcohol taste, obtain the macroporous resin after processing.
Wherein: macroporous resin refers to cation exchange type macroporous adsorbent resin.
(4) macroporous resin adsorption:
Supernatant is joined on the macroporous resin after processing, at every g resin applied sample amount, be to carry out adsorbing separation under 5ml, the flow velocity condition that is 1VB/h, and the ethanol that is 20% by mass concentration carry out eluting, simultaneously, salt acid for adjusting pH value to 2 ~ 4 that are 2% by mass concentration, obtain eluent after 10min.
Eluent under the pressure of 0.6MPa after concentrating under reduced pressure, obtain anthraquinone glycoside compound, the sulphuric acid that this anthraquinone glycoside compound is 10% by 0.1 times of its volume and mass concentration acidolysis 12 hours under 20 ℃ of conditions, drying obtains dissociated anthraquinone compounds to constant weight.
(6) in dissociated anthraquinone compounds, add chloroform ultrasonic extraction 5 minutes at ambient temperature, after re-extract 3 ~ 5 times, obtain water and chloroform layer; The volume ratio of dissociated anthraquinone compounds and chloroform is 1 ml:2 ml.
(7) chloroform layer is washed till chloroform layer with distilled water and is after neutrality, and under the pressure of 0.6MPa, after concentrating under reduced pressure, crystallization at normal temperatures obtains Yellow anthraquinone class crude product.
embodiment 2a method of extracting general anthraquinone from new fresh Radix et Rhizoma Rhei, comprises the following steps:
(1) prepare the fresh grinding slurry of Radix Et Rhizoma Rhei:
Roots and stems of rhubarb is cleaned to silt, remove the peel, and cut into the fritter of 1 * 1 cm; Then, the Radix Et Rhizoma Rhei being cut into small pieces is added to water by the solid-liquid ratio of 1kg:20L, with fiberizer, wear into after uniform serosity and cross 300 mesh sieves, obtain the fresh grinding slurry of Radix Et Rhizoma Rhei.
(2) complex enzyme degradation:
The sodium carbonate that is 2% by mass concentration by the fresh grinding slurry of Radix Et Rhizoma Rhei regulates pH value to 4.6 ~ 6.6 o'clock, in the fresh grinding slurry of Radix Et Rhizoma Rhei, by 125mg/L, adds extraction enzyme, and enzymolysis 12h at 65 ℃ of temperature, then, with centrifugal 5 min of speed of 4000 rpm, obtains supernatant.
Wherein: extracting enzyme is the compound enzyme being mixed by the mass ratio of 1g:20g:20g:10g by 1,4 beta-glucanase, cellulase, xylanase and pectase.
(3) macroporous resin pretreatment:
Macroporous resin is adsorbed to 12 h with the alcoholic solution that mass concentration is 95%, and the alcoholic solution that is then 95% by mass concentration successively and distilled water eluting, until eluent is without muddiness, without alcohol taste, obtain the macroporous resin after processing.
Wherein: macroporous resin refers to cation exchange type macroporous adsorbent resin.
(4) macroporous resin adsorption:
Supernatant is joined on the macroporous resin after processing, at every g resin applied sample amount, be to carry out adsorbing separation under 35ml, the flow velocity condition that is 5VB/h, and the ethanol that is 95% by mass concentration carry out eluting, simultaneously, salt acid for adjusting pH value to 4 ~ 8 that are 2% by mass concentration, obtain eluent after 120min.
Eluent under the pressure of 0.8MPa after concentrating under reduced pressure, obtain anthraquinone glycoside compound, the sulphuric acid that this anthraquinone glycoside compound is 40% by 1 times of its volume and mass concentration acidolysis 1 hour under 100 ℃ of conditions, drying obtains dissociated anthraquinone compounds to constant weight.
(6) in dissociated anthraquinone compounds, add chloroform ultrasonic extraction 60 minutes at ambient temperature, after re-extract 3 ~ 5 times, obtain water and chloroform layer; The volume ratio of dissociated anthraquinone compounds and chloroform is 1 ml:25 ml.
(7) chloroform layer is washed till chloroform layer with distilled water and is after neutrality, and under the pressure of 0.8MPa, after concentrating under reduced pressure, crystallization at normal temperatures obtains Yellow anthraquinone class crude product.
embodiment 3a method of extracting general anthraquinone from new fresh Radix et Rhizoma Rhei, comprises the following steps:
(1) prepare the fresh grinding slurry of Radix Et Rhizoma Rhei:
Roots and stems of rhubarb is cleaned to silt, remove the peel, and cut into the fritter of 1 * 1 cm; Then, the Radix Et Rhizoma Rhei being cut into small pieces is added to water by the solid-liquid ratio of 1kg:13L, with fiberizer, wear into after uniform serosity and cross 150 mesh sieves, obtain the fresh grinding slurry of Radix Et Rhizoma Rhei.
(2) complex enzyme degradation:
Salt acid for adjusting pH value to 6.6 ~ 8.6 o'clock that are 2% by mass concentration by the fresh grinding slurry of Radix Et Rhizoma Rhei add extraction enzyme by 75mg/L in the fresh grinding slurry of Radix Et Rhizoma Rhei, and then enzymolysis 42h at 45 ℃ of temperature with centrifugal 15 min of speed of 3000 rpm, obtains supernatant.
Wherein: extracting enzyme is the compound enzyme being mixed by the mass ratio of 1g:12g:10g:5g by 1,4 beta-glucanase, cellulase, xylanase and pectase.
(3) macroporous resin pretreatment:
Macroporous resin is adsorbed to 30 h with the alcoholic solution that mass concentration is 75%, and the alcoholic solution that is then 65% by mass concentration successively and distilled water eluting, until eluent is without muddiness, without alcohol taste, obtain the macroporous resin after processing.
Wherein: macroporous resin refers to cation exchange type macroporous adsorbent resin.
(4) macroporous resin adsorption:
Supernatant is joined on the macroporous resin after processing, is that 20ml, flow velocity are at every g resin applied sample amount
Under the condition of VB/h, carry out adsorbing separation, and the ethanol that is 65% by mass concentration carries out eluting, meanwhile, salt acid for adjusting pH value to 8 ~ 11 that are 2% by mass concentration, obtain eluent after 60min.
Eluent under the pressure of 0.7MPa after concentrating under reduced pressure, obtain anthraquinone glycoside compound, the sulphuric acid that this anthraquinone glycoside compound is 25% by 0.5 times of its volume and mass concentration acidolysis 6 hours under 60 ℃ of conditions, drying obtains dissociated anthraquinone compounds to constant weight.
(6) in dissociated anthraquinone compounds, add chloroform ultrasonic extraction 35 minutes at ambient temperature, after re-extract 3 ~ 5 times, obtain water and chloroform layer; The volume ratio of dissociated anthraquinone compounds and chloroform is 1 ml:3.5 ml.
(7) chloroform layer is washed till chloroform layer with distilled water and is after neutrality, and under the pressure of 0.7MPa, after concentrating under reduced pressure, crystallization at normal temperatures obtains Yellow anthraquinone class crude product.
Claims (3)
1. from new fresh Radix et Rhizoma Rhei, extract a method for general anthraquinone, comprise the following steps:
(1) prepare the fresh grinding slurry of Radix Et Rhizoma Rhei:
Roots and stems of rhubarb is cleaned to silt, remove the peel, and cut into the fritter of 1 * 1 cm; Then, the Radix Et Rhizoma Rhei being cut into small pieces is added to water by the solid-liquid ratio of 1kg:5L ~ 20L, with fiberizer, wear into after uniform serosity and cross 10 ~ 300 mesh sieves, obtain the fresh grinding slurry of Radix Et Rhizoma Rhei;
(2) complex enzyme degradation:
The sodium carbonate that the hydrochloric acid that is 2% by mass concentration by the fresh grinding slurry of described Radix Et Rhizoma Rhei or mass concentration are 2% regulates pH value to 2.4 ~ 8.6 o'clock, in the fresh grinding slurry of described Radix Et Rhizoma Rhei, by 20 ~ 125mg/L, add extraction enzyme, enzymolysis 12 ~ 72h at 20 ~ 65 ℃ of temperature, then with centrifugal 5 ~ 25 min of speed of 2000 ~ 4000 rpm, obtain supernatant;
(3) macroporous resin pretreatment:
The alcoholic solution that is 50% ~ 95% by mass concentration by macroporous resin absorption 12 ~ 48 h, the alcoholic solution that is then 10% ~ 95% by mass concentration successively and distilled water eluting, until eluent is without muddiness, without alcohol taste, obtain the macroporous resin after processing;
(4) macroporous resin adsorption:
Described supernatant is joined on the macroporous resin after described processing, at every g resin applied sample amount, be to carry out adsorbing separation under 5 ~ 35ml, the flow velocity condition that is 1 ~ 5VB/h, and the ethanol that is 20 ~ 95% by mass concentration carries out eluting, simultaneously, salt acid for adjusting pH value to 2 ~ 11 that are 2% by mass concentration, obtain eluent after 10 ~ 120min;
Described eluent under the pressure of 0.6 ~ 0.8MPa after concentrating under reduced pressure, obtain anthraquinone glycoside compound, the sulphuric acid that this anthraquinone glycoside compound is 10 ~ 40% by 0.1 ~ 1 times of its volume and mass concentration acidolysis 1 ~ 12 hour under 20 ~ 100 ℃ of conditions, drying obtains dissociated anthraquinone compounds to constant weight;
(6) in described dissociated anthraquinone compounds, add chloroform ultrasonic extraction 5 ~ 60 minutes at ambient temperature, after re-extract 3 ~ 5 times, obtain water and chloroform layer; The volume ratio of described dissociated anthraquinone compounds and described chloroform is 1 ml:2 ml ~ 5 ml;
(7) described chloroform layer is washed till chloroform layer with distilled water and is after neutrality, and under the pressure of 0.6 ~ 0.8MPa, after concentrating under reduced pressure, crystallization at normal temperatures obtains Yellow anthraquinone class crude product.
2. a kind of method of extracting general anthraquinone from new fresh Radix et Rhizoma Rhei as claimed in claim 1, is characterized in that: the extraction enzyme of described step in is (2) the compound enzyme being mixed by the mass ratio of 1g:3g ~ 20g:1g ~ 20g:1g ~ 10g by 1,4 beta-glucanase, cellulase, xylanase and pectase.
3. a kind of method of extracting general anthraquinone from new fresh Radix et Rhizoma Rhei as claimed in claim 1, is characterized in that: the macroporous resin of described step in (3) refers to cation exchange type macroporous adsorbent resin.
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| CN105123789B (en) * | 2015-09-25 | 2017-10-20 | 兰州大学 | A kind of free anthraquinones extracted from rheum nano-emulsion preparation for being used to prevent and treat plant red spider disease |
| CN107582647A (en) * | 2017-10-31 | 2018-01-16 | 桂林纽泰生物科技有限公司 | The extracting method of fleece-flower root total anthraquinone |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101181363A (en) * | 2007-11-19 | 2008-05-21 | 北京诚创康韵医药科技有限公司 | Ginseng rhubarb injection and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101181363A (en) * | 2007-11-19 | 2008-05-21 | 北京诚创康韵医药科技有限公司 | Ginseng rhubarb injection and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 周天林等.效应面法优化酶法提取大黄总蒽醌类成分的工艺研究.《中药材》.2012,第35卷(第10期),第1668-1674页. * |
| 效应面法优化酶法提取大黄总蒽醌类成分的工艺研究;周天林等;《中药材》;20121031;第35卷(第10期);第1668-1674页 * |
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