CN103408526A - High-purity chrysosplenetin preparation method - Google Patents
High-purity chrysosplenetin preparation method Download PDFInfo
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- CN103408526A CN103408526A CN201310360127XA CN201310360127A CN103408526A CN 103408526 A CN103408526 A CN 103408526A CN 201310360127X A CN201310360127X A CN 201310360127XA CN 201310360127 A CN201310360127 A CN 201310360127A CN 103408526 A CN103408526 A CN 103408526A
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- ethanolic soln
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Abstract
The invention discloses a high-purity chrysosplenetin preparation method which is simple and convenient in operation and low in pollution. The method comprises the following steps of (1) crushing matricaria chamomilla, adding an appropriate volume of water and an appropriate amount of bio-enzyme, carrying out enzymolysis for 10-40 hours at the temperature of 30-40 DEG C, adding 50-90% ethanol solution of a 5-10-times volume, carrying out reflux extraction, concentrating an extracting solution until no ethanol exists, adding a macroporous resin column for adsorption, carrying out gradient elution by using an ethanol solution, adjusting the ph of an eluent to 1-3 through concentrating the eluent, standing, crystallizing and filtering out crystals; and (2) dissolving the crystals by using an ethanol solution, adding polyamide resin to dry, loading a column, carrying out gradient elution by using an ethanol solution, concentrating and crystallizing an eluent, and re-crystallizing crystals by using a 99% ethanol solution, thereby obtaining high-purity chrysosplenetin. By using the method disclosed by the invention to prepare chrysosplenetin, the extracting efficiency is high, the obtained product is high in purity, and industrial production is easy to realize.
Description
Technical field
The invention belongs to biological technical field, particularly a kind of preparation method of high purity gold waist element.
Background technology
German chamomile is feverfew, and flavor is hot, and micro-hardship is cool in nature, be usually used in cold, fever, swelling and pain in the throat, lung heat cough breathe heavily, gesture numbness swells and ache, sore is swollen etc.Modern study is found to contain a large amount of volatile oil, flavonoid and lactone material in german chamomile, has anti-inflammatory, spasmolysis, bacteriostatic action.Gold waist element is Flavonoid substances in german chamomile, molecular formula C19H18O8, and molecular weight 375.35, have antibiotic, antivirus action, especially has low cytotoxicity, and have very strong anti-EV71 activity.
By literature search, the preparation method of existing high purity gold waist element, adopts silicagel column to separate more, and the method specificity is poor, the method complicated operation, and yield is low, is not suitable for industrialization.
Summary of the invention
The objective of the invention is to solve prior art deficiency and defect, a kind of preparation method of high purity easy and simple to handle gold waist element is provided.
The object of the present invention is achieved like this: a kind of preparation method of high purity gold waist element is characterized in that following steps:
1) getting german chamomile pulverizes, add suitable quantity of water and biological enzyme, 30-40 ℃ of enzymolysis 10-40h, add again 5-10 doubly to measure 50-90% ethanolic soln refluxing extraction, extracting solution is concentrated into without alcohol, adds macroporous resin column absorption, the ethanolic soln gradient elution, the concentrated ph1-3 of adjusting of elutriant places crystallization, and crystallisate leaches;
2) above-mentioned crystallisate adds the polyamide resin drying by the ethanolic soln solution, the dress post, and ethanolic soln gradient elution, elutriant condensing crystal, crystallisate are again with 99% ethanolic soln recrystallization and get final product.
A kind of in the optional cellulase of biological enzyme described in step 1), amylase and polygalacturonase, consumption is the 1-5 ‰ of material quantity.
A kind of in the optional HZ816 of macroporous resin model, ADS-21, AB-8 and HPD400 described in step 1).
Step 1), 2) the ethanolic soln gradient elution described in is: first with 3-5 times of column volume 20-50% ethanolic soln wash-out, more doubly measure 60-90% ethanolic soln wash-out with 5-10.
Adopt the present invention to prepare golden waist element, the hydrolytic process gentleness, product yield is high, and method is simple to operate, pollutes littlely, and energy consumption is low, is easy to suitability for industrialized production.
Embodiment:
Below in conjunction with embodiment, further illustrate the present invention, but the scope of protection of present invention is not limited to following embodiment.
Embodiment 1:
Getting the 10kg german chamomile pulverizes, the aqueous hydrochloric acid and the 30g cellulase that add equal-volume ph4, enzymolysis 20h under 40 ℃ of conditions of temperature, then add 10 times of amount 70% ethanolic soln refluxing extraction 2 times, the extracting solution concentrating under reduced pressure, concentrated solution adds the HZ816 macroporous resin adsorption, first use 5 times of column volumes, 30% ethanolic soln wash-out, measure 70% ethanolic soln wash-outs for 7 times again, the concentrated ph2 of adjusting of elutriant places crystallization, crystallisate leaches with 90% alcohol reflux and dissolves, add the 100g polyamide resin, dry, the dress post, first use 4 times of column volumes, 40% ethanolic soln wash-out, measure 75% ethanolic soln wash-outs for 6 times again, the elutriant condensing crystal, crystallisate refluxes dissolving crystallized with 99% ethanolic soln again, the crystallisate drying, obtain golden waist element 3.2g, through HPLC, detect, content 98.3%.
Embodiment 2:
Getting the 10kg german chamomile pulverizes, the aqueous sulfuric acid and the 40g amylase that add equal-volume p4.5, enzymolysis 18h under the temperature 50 C condition, then add 6 times of amount 80% ethanolic soln refluxing extraction 3 times, the extracting solution concentrating under reduced pressure, concentrated solution adds the ADS-21 macroporous resin adsorption, first use 5 times of column volumes, 40% ethanolic soln wash-out, measure 75% ethanolic soln wash-outs for 10 times again, the concentrated ph3 of adjusting of elutriant places crystallization, crystallisate leaches with 95% alcohol reflux and dissolves, add the 150g polyamide resin, dry, the dress post, first use 5 times of column volumes, 35% ethanolic soln wash-out, measure 70% ethanolic soln wash-outs for 7 times again, the elutriant condensing crystal, crystallisate refluxes dissolving crystallized with 99% ethanolic soln again, the crystallisate drying, obtain golden waist element 3.6g, through HPLC, detect, content 98.5%.
Embodiment 3:
Getting the 10kg german chamomile pulverizes, the aqueous hydrochloric acid and the 50g polygalacturonase that add equal-volume ph5, enzymolysis 25h under the temperature 45 C condition, then add 10 times of amount 50% ethanolic soln refluxing extraction 2 times, the extracting solution concentrating under reduced pressure, concentrated solution adds the AB-8 macroporous resin adsorption, first use 5 times of column volumes, 20% ethanolic soln wash-out, measure 60% ethanolic soln wash-outs for 7 times again, the concentrated ph1 of adjusting of elutriant places crystallization, crystallisate leaches with 95% alcohol reflux and dissolves, add the 130g polyamide resin, dry, the dress post, first use 5 times of column volumes, 20% ethanolic soln wash-out, measure 60% ethanolic soln wash-outs for 8 times again, the elutriant condensing crystal, crystallisate refluxes dissolving crystallized with 99% ethanolic soln again, the crystallisate drying, obtain golden waist element 3.6g, through HPLC, detect, content 96.9%.
Embodiment 4:
Getting the 10kg german chamomile pulverizes, the aqueous hydrochloric acid and the 40g cellulase that add equal-volume ph3, enzymolysis 15h under the temperature 45 C condition, then add 8 times of amount 90% ethanolic soln refluxing extraction 2 times, the extracting solution concentrating under reduced pressure, concentrated solution adds the HPD400 macroporous resin adsorption, first use 4 times of column volumes, 40% ethanolic soln wash-out, measure 90% ethanolic soln wash-outs for 5 times again, the concentrated ph3 of adjusting of elutriant places crystallization, crystallisate leaches with 95% alcohol reflux and dissolves, add the 150g polyamide resin, dry, the dress post, first use 3 times of column volumes, 50% ethanolic soln wash-out, measure 90% ethanolic soln wash-outs for 5 times again, the elutriant condensing crystal, crystallisate refluxes dissolving crystallized with 99% ethanolic soln again, the crystallisate drying, obtain golden waist element 3.5g, through HPLC, detect, content 97.4%.
Claims (4)
1. the preparation method of high purity gold waist element is characterized in that following steps:
1) getting german chamomile pulverizes, add suitable quantity of water and biological enzyme, 30-40 ℃ of enzymolysis 10-40h, add again 5-10 doubly to measure 50-90% ethanolic soln refluxing extraction, extracting solution is concentrated into without alcohol, adds macroporous resin column absorption, the ethanolic soln gradient elution, the concentrated ph1-3 of adjusting of elutriant places crystallization, and crystallisate leaches;
2) above-mentioned crystallisate adds the polyamide resin drying by the ethanolic soln solution, the dress post, and ethanolic soln gradient elution, elutriant condensing crystal, crystallisate are again with 99% ethanolic soln recrystallization and get final product.
2. the preparation method of high purity gold waist element according to claim 1, it is characterized in that the optional cellulase of biological enzyme described in step 1), amylase and polygalacturonase in a kind of, consumption is the 1-5 ‰ of material quantity.
3. the preparation method of high purity gold waist element according to claim 1, is characterized in that a kind of in the optional HZ816 of macroporous resin model, ADS-21, AB-8 and the HPD400 described in step 1).
4. the preparation method of high purity gold waist element according to claim 1, is characterized in that step 1), 2) described in the ethanolic soln gradient elution be: first with 3-5 times of column volume 20-50% ethanolic soln wash-out, more doubly measure 60-90% ethanolic soln wash-out with 5-10.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310360127XA CN103408526A (en) | 2013-08-19 | 2013-08-19 | High-purity chrysosplenetin preparation method |
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| CN201310360127XA CN103408526A (en) | 2013-08-19 | 2013-08-19 | High-purity chrysosplenetin preparation method |
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Application publication date: 20131127 |