CN102040611A - Method for extracting mulberry root ketone C - Google Patents
Method for extracting mulberry root ketone C Download PDFInfo
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- CN102040611A CN102040611A CN2010102931654A CN201010293165A CN102040611A CN 102040611 A CN102040611 A CN 102040611A CN 2010102931654 A CN2010102931654 A CN 2010102931654A CN 201010293165 A CN201010293165 A CN 201010293165A CN 102040611 A CN102040611 A CN 102040611A
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Abstract
The invention relates to a method for extracting mulberry root ketone C. The process method provided by the invention comprises the following steps: crushing white mulberry root-bark into small grains; carrying out ultrasonic extraction for 2-3 times by utilizing an alkali aqueous solution the pH value of which is 9-11; regulating the pH value to 7-8 by the extraction; absorbing by adding macroporous resin; eluting by an ethanol solution; recycling ethanol after eluting; regulating the acidity, and precipitating; dissolving the precipitates in acetone, and then, adding a silicagel column for separating; carrying out gradient elution by an acetone aqueous solution; concentrating and crystallizing; recrystallizing by a methanol chloroform solution; and drying to obtain a product. The method provided by the invention has the advantage of simple operation and solves the difficulty that the conventional silicagel column separation can not expand the production, and the content of the obtained product is relatively high.
Description
Technical field:
The invention belongs to biological technical field, especially relate to a kind of method of from White Mulberry Root-bark, extracting sanggenon C.
Background technology:
White Mulberry Root-bark is the dry root skin of moraceae plants mulberry Morus alba L..Fall last years of a century in autumn and before the inferior spring germinates, excavate root, scrape off the yellowish brown tertia. vertically cut open. strip the root skin, dry.Lung heat is coughed and is breathed heavily.The property sweet cold falling, main go into lung channel, aqueous vapor in the purging the lung of pathogenic fire of can clear purte the white holding concurrently and relievining asthma.Control lung heat and cough and breathe heavily, hydrosarca, appearance skin edema, turgor is breathed heavily urgency, and dysuria person in addition, also has the merit of removing heat from the liver to lower the high blood pressure hemostasis, can control bleeding from five sense organs or subcutaneous tissue, spitting of blood and the prosperous partially vascular hypertension of liver-yang irascibility.
Contain multiple flavone derivative, Umbelliferone, compositions such as Scopoletin in the modern medicine study White Mulberry Root-bark.Sanggenon C is one of effective constituent in the White Mulberry Root-bark, has tangible hypotensive effect.Nineteen eighty-three, Japanese good fortune richness is at first carried out hypotensive experiment with Cortex Mori extract to rabbit, nineteen ninety-five, in the feed 12-18 week that use original hypertensive rats such as Japan assistant rattan are freely ingested and are mixed with mulberry leaf, also finds that it has the effect that reduces diastolic pressure.Sanggenon C has whitening function in addition.
The sanggenon C Flavonoid substances is dissolved in low molecule organic polar solvents such as methyl alcohol, ethanol, acetone, ether, and is water insoluble, is insoluble in sherwood oil, chloroform.
Extract the method for sanggenon C at present, mostly be organic solvent extraction, again through silica gel column chromatography." from White Mulberry Root-bark, extract the pharmaceutical cpd sanggenon C " as document and adopt the ethanol lixiviate, acetone extract, the benzene washing, ether extracts again, after silicagel column and preparation liquid phase separation obtain the high-content sanggenon C.Though that but this technology has obtained high-content product agents useful for same toxicity is bigger, operator are endangered greatly, technology also is difficult to mass production.Chinese patent " the extraction process for purification and the application thereof of sanggenon C " for another example, the method for this patent disclosure is an alcohol reflux, ethyl acetate extraction adopts silicagel column to separate with preparative chromatography at last again, obtains the product more than 90%.This patent also is to be difficult to relatively large preparation, and cost is also higher.
Summary of the invention:
The present invention wants the technical solution problem to provide a kind of simple to operate, extracting method of being easy to industrialized sanggenon C.
The objective of the invention is to realize by following technical solution:
A kind of extracting method of sanggenon C is characterized in that comprising following steps:
1) the White Mulberry Root-bark raw material pulverizing, add 6-15 and doubly measure the alkaline aqueous solution supersound extraction 2-3 time, extracting solution subtracts regulates pH7-8, add macroporous resin column absorption, wash sugared reaction negative, doubly measure 60-75% ethanolic soln wash-out with 5-8 again, reclaim ethanol, concentrated solution adds acid and transfers pH1-4, places precipitation;
2) throw out leaches with 5-10 and doubly measures the acetone backflow, and filtered while hot adds silicagel column, and the aqueous acetone solution gradient elution is collected effective constituent, reclaims acetone and places crystallization;
3) the coarse crystallization thing leaches with the saturated dissolving of methyl alcohol, adds the 20-30% chloroform and places crystallization, leaches the dry mulberry root C of getting of crystallisate.
Basic solution in the described step 1) is sodium hydroxide or the calcium hydroxide aqueous solution of pH9-11, a kind of among the optional AB-8 of macroporous resin model, HPD100 and the HZ818, and used acid is hydrochloric acid or aqueous sulfuric acid.
Described step 2) the aqueous acetone solution gradient elution is 4-5BV10-30% acetone soln → 5-7BV50-70% acetone soln in.
The present invention adopts alkali aqueous solution supersound extraction (document " sanggenon C; the stability study of D in alkali lye ", proved also in the experiment that sanggenon C is stable in basic solution) reduced apolar substance stripping, lower than organic reagent extraction cost, extracting solution also need not to concentrate, can directly go up macroporous resin adsorption, reduced energy consumption, remove polysaccharide and pigment through Amberlyst process post fractionation by adsorption again, obtained the total flavones material, silicagel column on the wet method is used the acetone wash-out of different concns again, operates simple relatively, also amplify easily and produce, solved the little difficult problem of silicagel column treatment capacity.
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:
After the White Mulberry Root-bark drying, pulverize small-particle, get 5kg, add the miniature ultrasonic extractor, the lime aqueous solution of configuration pH9 is measured 75kg, 50kg and 30kg liquid respectively, added the extractor supersound extraction successively 2 hours, 1 hour, 1 hour, open power 2kw, merge No. three times extracting solution, hydrochloric acid is regulated pH8 and is filtered.Get the 7LAB-8 resin resin column (blade diameter length ratio 1: 15) of packing into, use acid-alkali treatment successively, after the washing neutrality, extracting solution is added macroporous resin column, flow velocity 5L/h, after absorption finishes, water-based sugar reaction negative is got the 56L60% ethanol elution again, collects the elutriant decompression recycling ethanol, concentrated solution is placed precipitation regulating pH1, filter throw out 50g.Precipitation is dissolved with the backflow of 500ml acetone, and filtration adds silicagel column, and (blade diameter length ratio 1: 15, silica gel are 200-300 order neutral silica gel, weight 1kg), gets 5kg10% acetone soln wash-out, get 7kg50% acetone wash-out again, collect 50% acetone flow point, reclaim acetone and place crystallization.Leach coarse crystallization with 90% methanol solution backflow dissolving, add 30% chloroformic solution behind the normal temperature, leave standstill crystallization after filtering fast, the vacuum-drying crystallisate obtains sanggenon C 15g, content 91%.
Embodiment 2:
After the White Mulberry Root-bark drying, pulverize small-particle, get 5kg, add the miniature ultrasonic extractor, the lime aqueous solution of configuration pH10 is measured 50kg, 40kg and 30kg liquid respectively, added the extractor supersound extraction successively 1 hour, 1 hour, 1 hour, open power 2kw, merge No. three times extracting solution, hydrochloric acid is regulated pH7 and is filtered.Get the 6L HPD100 resin resin column (blade diameter length ratio 1: 20) of packing into, use acid-alkali treatment successively, after the washing neutrality, extracting solution is added macroporous resin column, flow velocity 8L/h, after absorption finishes, water-based sugar reaction negative is got the 30L75% ethanol elution again, collects the elutriant decompression recycling ethanol, concentrated solution is placed precipitation regulating pH4, filter throw out 65g.Precipitation is dissolved with the backflow of 400ml acetone, and filtration adds silicagel column, and (blade diameter length ratio 1: 15, silica gel are 200-300 order neutral silica gel, weight 1kg), gets 4kg30% acetone soln wash-out, get 5kg70% acetone wash-out again, collect 70% acetone flow point, reclaim acetone and place crystallization.Leach coarse crystallization with 99% methanol solution backflow dissolving, add 20% chloroformic solution behind the normal temperature, leave standstill crystallization after filtering fast, the vacuum-drying crystallisate obtains the 18g sanggenon C, content 85%.
Embodiment 3:
After the White Mulberry Root-bark drying, pulverize small-particle, get 10kg, add the miniature ultrasonic extractor, the lime aqueous solution of configuration pH11 is measured 100kg, 100kg and 60kg liquid respectively, added the extractor supersound extraction successively 1 hour, 1 hour, 1 hour, open power 4kw, merge No. three times extracting solution, sulfuric acid is regulated pH7 and is filtered.Get the 15L HZ818 resin resin column (blade diameter length ratio 1: 15) of packing into, extracting solution is added macroporous resin column, flow velocity 15L/h, after absorption finishes, water-based sugar reaction negative is got the 90L60% ethanol elution again, collects the elutriant decompression recycling ethanol, concentrated solution is placed precipitation regulating pH3, filter throw out 96g.Precipitation is dissolved with the backflow of 700ml acetone, and filtration adds silicagel column, and (blade diameter length ratio 1: 15, silica gel are 200-300 order neutral silica gel, weight 2kg), gets 10kg20% acetone soln wash-out, get 15kg50% acetone wash-out again, collect 50% acetone flow point, reclaim acetone and place crystallization.Leach coarse crystallization with 90% methanol solution backflow dissolving, add 30% chloroformic solution behind the normal temperature, leave standstill crystallization after filtering fast, the vacuum-drying crystallisate obtains sanggenon 21gC, content 92%.
Embodiment 4:
After the White Mulberry Root-bark drying, pulverize small-particle, get 20kg, add medium-sized supersound extraction jar, the sodium hydroxide solution of configuration pH9 is measured 150kg, 150kg and 120kg liquid respectively, added the extractor supersound extraction successively 1 hour, 1 hour, 1 hour, open power 5kw, merge No. three times extracting solution, sulfuric acid is regulated pH7 and is filtered.Get the 30L AB-8 resin resin column (blade diameter length ratio 1: 15) of packing into, extracting solution is added macroporous resin column, flow velocity 30L/h, after absorption finishes, water-based sugar reaction negative is got the 180L60% ethanol elution again, collects the elutriant decompression recycling ethanol, concentrated solution is placed precipitation regulating pH2, filter throw out 205g.Precipitation is dissolved with the backflow of 2000ml acetone, and filtration adds silicagel column, and (blade diameter length ratio 1: 15, silica gel are 200-300 order neutral silica gel, weight 4kg), gets 20kg20% acetone soln wash-out, get 25kg60% acetone wash-out again, collect 60% acetone flow point, reclaim acetone and place crystallization.Leach coarse crystallization with 90% methanol solution backflow dissolving, add 30% chloroformic solution behind the normal temperature, leave standstill crystallization after filtering fast, the vacuum-drying crystallisate obtains sanggenon 45gC, content 89%.
Claims (3)
1. the extracting method of a sanggenon C is characterized in that comprising following steps:
1) the White Mulberry Root-bark raw material pulverizing, add 6-15 and doubly measure the alkaline aqueous solution supersound extraction 2-3 time, extracting solution subtracts regulates pH7-8, add macroporous resin column absorption, wash sugared reaction negative, doubly measure 60-75% ethanolic soln wash-out with 5-8 again, reclaim ethanol, concentrated solution adds acid and transfers pH1-4, places precipitation;
2) throw out leaches with 5-10 and doubly measures the acetone backflow, and filtered while hot adds silicagel column, and the aqueous acetone solution gradient elution is collected effective constituent, reclaims acetone and places crystallization;
3) the coarse crystallization thing leaches with the saturated dissolving of methyl alcohol, adds the 20-30% chloroform and places crystallization, leaches the dry mulberry root C of getting of crystallisate.
2. the extracting method of sanggenon C according to claim 1, it is characterized in that the basic solution in the described step 1) is sodium hydroxide or the calcium hydroxide aqueous solution of pH9-11, a kind of among the optional AB-8 of macroporous resin model, HPD100 and the HZ818, used acid is hydrochloric acid or aqueous sulfuric acid.
3. the extracting method of sanggenon C according to claim 1 is characterized in that described step 2) in the aqueous acetone solution gradient elution be 4-5BV20-30% acetone soln → 5-7BV50-70% acetone soln.
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| CN2010102931654A CN102040611A (en) | 2010-09-27 | 2010-09-27 | Method for extracting mulberry root ketone C |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103027951A (en) * | 2011-10-09 | 2013-04-10 | 贵州大学 | Purification method of cortex mori total flavonoids |
| CN103876988A (en) * | 2014-04-04 | 2014-06-25 | 广州丹奇日用化工厂有限公司 | Method for extracting flavone from lithospermum stems and leaves and application thereof in cosmetics |
| CN108261346A (en) * | 2018-03-01 | 2018-07-10 | 森知（上海）国际贸易有限公司 | A kind of lightening compositions and preparation method thereof |
| CN113633592A (en) * | 2021-09-10 | 2021-11-12 | 武汉知归堂创新医药研究有限公司 | Whitening and freckle-removing functional additive, whitening and freckle-removing cream and preparation method thereof |
-
2010
- 2010-09-27 CN CN2010102931654A patent/CN102040611A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103027951A (en) * | 2011-10-09 | 2013-04-10 | 贵州大学 | Purification method of cortex mori total flavonoids |
| CN103876988A (en) * | 2014-04-04 | 2014-06-25 | 广州丹奇日用化工厂有限公司 | Method for extracting flavone from lithospermum stems and leaves and application thereof in cosmetics |
| CN103876988B (en) * | 2014-04-04 | 2016-08-17 | 松泽化妆品（深圳）有限公司 | A kind of Radix Arnebiae (Radix Lithospermi) stem and leaf extracts the method for flavone and the application in cosmetics thereof |
| CN108261346A (en) * | 2018-03-01 | 2018-07-10 | 森知（上海）国际贸易有限公司 | A kind of lightening compositions and preparation method thereof |
| CN108261346B (en) * | 2018-03-01 | 2020-12-29 | 上海科颜生物科技有限公司 | Whitening composition and preparation method thereof |
| CN113633592A (en) * | 2021-09-10 | 2021-11-12 | 武汉知归堂创新医药研究有限公司 | Whitening and freckle-removing functional additive, whitening and freckle-removing cream and preparation method thereof |
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Application publication date: 20110504 |