CN101759738A - Process for extracting cosmos glycoside - Google Patents
Process for extracting cosmos glycoside Download PDFInfo
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- CN101759738A CN101759738A CN200910233834A CN200910233834A CN101759738A CN 101759738 A CN101759738 A CN 101759738A CN 200910233834 A CN200910233834 A CN 200910233834A CN 200910233834 A CN200910233834 A CN 200910233834A CN 101759738 A CN101759738 A CN 101759738A
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- cosmosiin
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- tribute chrysanthemum
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Abstract
A process for extracting cosmos glycoside adopts tribute chrysanthemum as raw material and includes the steps of crushing, soaking, macroporous resin treatment, film concentration, acid adjustment, polyamide treatment and freezing crystallization, so as to obtain the finished products. The invention adopts the separation methods of macroporous, film and polyamide, not only improves the extraction efficiency of cosmos glycoside, but also prevents the decomposition and damage of cosmos glycoside due to heating in preparation method, and also guarantees high purity.
Description
Technical field:
The present invention relates to a kind of technology of extracting cosmosiin, is a kind of technology of extracting cosmosiin from the tribute chrysanthemum.
Background technology:
The tribute chrysanthemum is a conventional Chinese medicine, claims the emblem chrysanthemum again, is grown in high height above sea level mountain region, main product is the medicinal herb tea dual-purpose kind that grows up as the tea chrysanthemum in the Shexian County, Anhui, is listed in tribute during the Ming Dynasty and gains the name, the tribute chrysanthemum brews the back look clear yellow bright, sample sweetly to feel well the effect that has heat-clearing to dispel fire, clear liver and improve vision.Chrysanthemum tea has an effect to dry, hyperactivity of fire, order are puckery, and after the hot drink, panhidrosis feels relief, and is the good medicine of curing flu, also is the nourishing drink that suits the taste of both old and young." Mount Huang tribute chrysanthemum " has wind-dispelling heat-dissipating, nourishes the liver to improve visual acuity, the function of refreshing and detoxicating, and the wind flu that can cure the wound, furuncle swelling toxin, blood pressure is higher and disease such as arteriosclerosis.Can make beverages such as patent medicine such as SUNJU GANMAO PIAN and chrysanthemum crystals with its allotment other medicines.Can make tea, steep in wine, Chang Yinke " peace and quiet the five internal organs, toxin-expelling body-building " has the effect of prolonging the poison beauty treatment.Also can use pillow as after drink exhausted chrysanthemum dries, make the refrigerant fire that falls of people, restoring consciouness makes eye bright.Chrysanthemum always just is described as the flower of long life and anti-ageing, wherein has the decomposition and the excretory composition of anti-ageing composition and promotion cholesterol.Its beauty functions is: sharp qi and blood, profit skin, refresh oneself, " beneficial color ", and can the maintenance hair.Just having in the Yuan Dynasty " Royal drug museum side " with the chrysanthemum is the record that main ingredient is made the hair washing chrysanthemum powder forimproving, cures mainly epilation.The famous physician's Zhang Jingyue of the Ming Dynasty is also controlled freckle with medicine wiping faces such as chrysanthemum, the roots of Dahurain angelica, and is quite powerful.Can strengthen people's physique and the record of promoting longevity as for chrysanthemum, just have a lot from ancient times.The nutritionist thinks that chrysanthemum has physical strength reinforcing both at home and abroad, and antisenility function can improve human body metabolism, relieving fatigue, prevention various diseases and appearance effect.
The tribute chrysanthemum is with milli chrysanthemum, Chu chrysanthemum, the Hang Ju quilt " record in the chrysanthemum kind, and former plant is Chrysanthemum morifolium Ramat by Chinese pharmacopoeia version in 2000.Chrysanthemum flavor is sweet, cold nature, and it contains, and chrysanthemum is sweet, VITAMIN B4, choline, also contains a small amount of retinol1, VITMAIN B1, amino acid first, sodium salt etc.Tribute chrysanthemum working method uniqueness is spent best in qualityly, and the medicinal material of processing is grey, the base of a fruit is green, flavor is fragrant, is pleasant to the eye and taste the optimum tea-drinking.Flavones in the chrysanthemum mainly is to exist with the form that is combined into glycosides with sugar.Find after deliberation, because of kind development and place of production difference, the chemical ingredients of chrysanthemum is not quite similar, get 3 flavonoid glycoside compounds from the ethyl acetate extraction position of the ethanol extraction of tribute chrysanthemum, identify that according to physico-chemical property and spectral data its structure is acacetin-7-O-β-D-glucoside (acacetin-7-O-β-D-gluco-side, I), apigenin-7-O-beta-D-glucoside (apigenin-7-O-β-D-glucoside, II), luteolin-7-O-β-D-glucoside (luteolin-7-O-β-D-glucoside, III).Cosmosiin is apigenin-7-O-beta-D-glucoside, and its molecular structure is as follows:
Because have the unique texture of flavonoid, cosmosiin has good oxidation-resistance, and very big potentiality to be exploited is arranged.Extract separately from the tribute chrysanthemum that cosmosiin is domestic still not to have a report.
Summary of the invention:
The objective of the invention is that a kind of production technique is simple, energy consumption is few in order to provide, cost is low, and cosmosiin purity reaches more than 90%, and output is big, and the cycle is short, is easy to realize industrialized cosmosiin extraction process.
The object of the present invention is achieved like this:
The tribute chrysanthemum is pulverized slightly, the sodium carbonate solution that places tribute chrysanthemum weight 10-12 doubly to measure soaked 2-3 hour, the elimination residue, and it is 7～8 that solution is regulated pH, cross macroporous resin column absorption, use the different solvents stepwise elution, it is 2～3 that the cosmosiin elutriant is regulated pH, crosses polyamide column, stepwise elution, cosmosiin elutriant membrane concentration is to small volume, places crystallization, filter the yellow solid finished product.
1) pulverizes: can make it not increasing faster stripping desired substance under the situation of extracting temperature with the tribute inulin is broken, guarantee output when having saved energy.
Above-mentioned crushing process is broken to 40～60 orders with the tribute inulin.
2) stripping: owing to contain the apigenin structure in the cosmosiin, therefore solubleness is better than other compositions in basic solution, can have very high selectivity with sodium carbonate solution when extracting.Regulate pH and make the easier of the cosmosiin that is dissolved in the alkali lye to the weak base performance by macroporous resin adsorption thereafter.
The preferred hydrochloric acid of above-mentioned adjusting pH.
3) macroporous resin adsorption: in order to remove residual salt and organic impurity, cut down the consumption of energy simultaneously, adopt the method for macroporous resin adsorption here.Flavonoid glycoside substance can be by wash-out at alcohol concn about 60%, and the operation of first two steps wash-out can be removed water soluble ion compound and organic impurity respectively.
Above-mentioned macroporous resin column be for can select HPD-100, HPD-300, HPD-400, HPD-600 etc. for use, preferred HPD-100.
Above-mentioned macroporous resin stepwise elution method is: at first with the removal of impurities of 4～6 times of amount column volume deionization washing macroporous resins, then with 10～20% ethanol removal of impurities of 2～3 times of amount column volumes, at last with 4～5 times of amount column volume 60～70% ethanol elution cosmosiins.
4) membrane concentration: the molecular weight of cosmosiin is 432.38, so adopt the aperture to be lower than 400 nanofiltration membrane.
Above-mentioned concentrated employing employing molecular weight cut-off is 300～400 nanofiltration membrane, preferred ESNA1-K1-4040 nanofiltration membrane.
5) polymeric amide absorption: for being further purified cosmosiin, this law adopts the polymeric amide absorption method.Acid adjustment herein can improve adsorption effect.Stepwise elution is removal of impurities once more.
The preferred hydrochloric acid of above-mentioned adjusting pH.
Above-mentioned polymeric amide stepwise elution method is: at first with the removal of impurities of 4～6 times of amount column volume deionization washing polymeric amide, then with 4～5 times of amount column volume 60-70% ethanol elution cosmosiins.
6) membrane concentration: the molecular weight of cosmosiin is 432.38, so adopt the aperture to be lower than 400 nanofiltration membrane.
Above-mentioned concentrated employing employing molecular weight cut-off is 300～400 nanofiltration membrane, preferred ESNA1-K1-4040 nanofiltration membrane.
7) crystallization: for cosmosiin is separated from elutriant, and simplify the operation, ensure the quality of products, adopt the crystallizing process under low temperature.
Above-mentioned crystallisation process carries out at low temperatures.
In sum, there is following advantage in the present invention:
1) utilize this parameter of adjusting solvent pH that extraction efficiency is improved.At first utilize cosmosiin in basic solvent relatively other components preferably solvability selection rate is improved, make thereafter separation not be subjected to the influence of salt by regulating pH again, ion is more easily removal in concentrating also, and is can be when crystallization not residual and cause the reduction of purity.
2) macroporous resin adsorption, membrane sepn, polymeric amide separation, low temperature crystallization all make technological process can guarantee that service temperature is no more than normal temperature, simple to operate, therefore both keep the stability of cosmosiin, also saved a large amount of energy consumptions, also guaranteed production efficiency simultaneously.
3) twice elution process all adopts stepwise elution, and removal of impurities is abundant.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
The tribute chrysanthemum is crushed to 40 orders, get 10kg (cosmosiin content 2.48 ‰), extract at room temperature is 0.5 hour in the adding 40L2% sodium carbonate solution, the elimination residue, regulating pH with hydrochloric acid is 7, cross the HPD-300 macroporous resin column absorption of column volume 5L, earlier with 20L deionized water eluting water solubility impurity, use 10L10% ethanol elution organic impurity again, use 20L60% ethanol elution cosmosiin at last, it is 2 that elutriant is for the third time regulated pH with hydrochloric acid, crosses the polyamide column of column volume 5L, the eccysis of 20L deionized water is assorted, 20L60% ethanol elution cosmosiin, the latter is by ESNA1-K1-4040 nanofiltration membrane simmer down to small volume, and concentrated solution places but crystallization of refrigerator and cooled, filter, finally obtain 17.3g content and be 92.1% cosmosiin finished product.
Embodiment 2:
The tribute chrysanthemum is crushed to 50 orders, get 10kg (cosmosiin content 2.53 ‰), extract at room temperature is 0.75 hour in the adding 45L3% sodium carbonate solution, the elimination residue, regulating pH with hydrochloric acid is 8, cross the HPD-400 macroporous resin column absorption of column volume 5L, earlier with 25L deionized water eluting water solubility impurity, use 10L10% ethanol elution organic impurity again, use 22L60% ethanol elution cosmosiin at last, it is 2 that elutriant is for the third time regulated pH with hydrochloric acid, cross the polyamide column of column volume 5L, the eccysis of 23L deionized water is assorted, 23L65% ethanol elution cosmosiin, and the latter concentrates by the ESNA1-K1-4040 nanofiltration membrane, it is 2 that concentrated solution is regulated pH with hydrochloric acid, cross the polyamide column of column volume 5L, the eccysis of 23L deionized water is assorted, 23L90% ethanol elution cosmosiin, the latter is to small volume, concentrated solution places but crystallization of refrigerator and cooled, filters, and finally obtains 18.6g content and be 94.3% cosmosiin finished product.
Embodiment 3:
The tribute chrysanthemum is crushed to 60 orders, get 10kg (cosmosiin content 2.43 ‰), extract at room temperature is 1 hour in the adding 50L2% sodium carbonate solution, the elimination residue, regulating pH with hydrochloric acid is 7, cross the HPD-100 macroporous resin column absorption of column volume 5L, earlier with 25L deionized water eluting water solubility impurity, use 15L20% ethanol elution organic impurity again, use 25L70% ethanol elution cosmosiin at last, it is 3 that elutriant is for the third time regulated pH with hydrochloric acid, crosses the polyamide column of column volume 5L, the eccysis of 25L deionized water is assorted, 25L60% ethanol elution cosmosiin, the latter is concentrated into small volume by the ESNA1-K1-4040 nanofiltration membrane, and concentrated solution places but crystallization of refrigerator and cooled, filter, finally obtain 18.8g content and be 96.7% cosmosiin finished product.
Embodiment 4:
The tribute chrysanthemum is crushed to 50 orders, get 10kg (cosmosiin content 2.46 ‰), extract at room temperature is 0.75 hour in the adding 40L3% sodium carbonate solution, the elimination residue, regulating pH with hydrochloric acid is 8, cross the HPD-600 macroporous resin column absorption of column volume 5L, earlier with 30L deionized water eluting water solubility impurity, use 10L10% ethanol elution organic impurity again, use 60% ethanol elution cosmosiin at last, it is 3 that elutriant is for the third time regulated pH with hydrochloric acid, crosses the polyamide column of column volume 5L, the eccysis of 25L deionized water is assorted, 20L70% ethanol elution cosmosiin, the latter is concentrated into small volume by the ESNA1-K1-4040 nanofiltration membrane, and concentrated solution places but crystallization of refrigerator and cooled, filter, finally obtain 16.8g content and be 95.0% cosmosiin finished product.
Claims (9)
1. technology of from the tribute chrysanthemum, extracting cosmosiin, it is characterized in that comprising following steps: the tribute chrysanthemum is pulverized slightly, and the sodium carbonate solution that places tribute chrysanthemum weight 10-12 doubly to measure soaked 2-3 hour, the elimination residue, it is 7～8 that solution is regulated pH, crosses macroporous resin column absorption, uses the different solvents stepwise elution, it is 2～3 that the cosmosiin elutriant is regulated pH, cross polyamide column, stepwise elution, cosmosiin elutriant membrane concentration is to small volume, place crystallization, filter the yellow solid finished product.
2. extract the technology of cosmosiin as claim 1 from the tribute chrysanthemum, it is characterized in that described crushing process is broken to the 10-20 order with the tribute inulin, sodium carbonate solution concentration is 2-3%.
3. from the tribute chrysanthemum, extract the technology of cosmosiin as claim 1, it is characterized in that the preferred hydrochloric acid of described adjusting pH.
4. from the tribute chrysanthemum, extract the technology of cosmosiin as claim 1, it is characterized in that described macroporous resin column, preferred HPD-100 for can select HPD-100, HPD-300, HPD-400, HPD-600 etc. for use.
5. from the tribute chrysanthemum, extract the technology of cosmosiin as claim 1, it is characterized in that described macroporous resin stepwise elution method is: at first with the removal of impurities of 4～6 times of amount column volume deionization washing macroporous resins, then with 10～20% ethanol removal of impurities of 2～3 times of amount column volumes, at last with 4～5 times of amount column volume 60～70% ethanol elution cosmosiins.
6. from the tribute chrysanthemum, extract the technology of cosmosiin as claim 1, it is characterized in that described concentration operation employing molecular weight cut-off is 300～400 nanofiltration membrane, preferred ESNA1-K1-4040 nanofiltration membrane.
7. from the tribute chrysanthemum, extract the technology of cosmosiin as claim 1, it is characterized in that described polymeric amide stepwise elution method is: at first with the removal of impurities of 4～6 times of amount column volume deionization washing polyamide columns, again with 20～30% ethanol removal of impurities of 2～3 times of amount column volumes, at last with 4～5 times of amount column volume 60-70% ethanol elution cosmosiins.
8. from the tribute chrysanthemum, extract the technology of cosmosiin as claim 1, it is characterized in that described concentration operation employing molecular weight cut-off is 300～400 nanofiltration membrane.
9. from the tribute chrysanthemum, extract the technology of cosmosiin as claim 1, it is characterized in that described crystallisation process carries out at low temperatures.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910233834A CN101759738A (en) | 2009-10-22 | 2009-10-22 | Process for extracting cosmos glycoside |
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| CN200910233834A CN101759738A (en) | 2009-10-22 | 2009-10-22 | Process for extracting cosmos glycoside |
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| CN101759738A true CN101759738A (en) | 2010-06-30 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329354A (en) * | 2011-05-31 | 2012-01-25 | 苏州派腾生物医药科技有限公司 | Method for extracting cosmosiin from agrimony |
| CN109717445A (en) * | 2019-01-30 | 2019-05-07 | 湖南绿蔓生物科技股份有限公司 | Sweetener composition and its preparation method and application |
-
2009
- 2009-10-22 CN CN200910233834A patent/CN101759738A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329354A (en) * | 2011-05-31 | 2012-01-25 | 苏州派腾生物医药科技有限公司 | Method for extracting cosmosiin from agrimony |
| CN109717445A (en) * | 2019-01-30 | 2019-05-07 | 湖南绿蔓生物科技股份有限公司 | Sweetener composition and its preparation method and application |
| CN109717445B (en) * | 2019-01-30 | 2022-10-18 | 湖南绿蔓生物科技股份有限公司 | Sweet taste composition and preparation method and application thereof |
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Application publication date: 20100630 |