CN102311445A - Method for preparing high purity sanggenon D - Google Patents
Method for preparing high purity sanggenon D Download PDFInfo
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- CN102311445A CN102311445A CN201110186579A CN201110186579A CN102311445A CN 102311445 A CN102311445 A CN 102311445A CN 201110186579 A CN201110186579 A CN 201110186579A CN 201110186579 A CN201110186579 A CN 201110186579A CN 102311445 A CN102311445 A CN 102311445A
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- sanggenon
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- polyamide resin
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Abstract
The invention belongs to the technical field of biology, and discloses a method for preparing high purity sanggenon D. The method comprises steps that 1) a medicinal material of the root bark of white mulberry is crushed, added with 6-10 times of 80-90% ethanol solution and treated with refluxing extraction 2-3 times; an extract is concentrated, treated with acidity adjusting, and precipitated; precipitate is dissolved by acetone, added with polyamide resin, blended, dried and loaded into a polyamide resin column; the polyamide resin column is treated with gradient elution, thin layer detection; an object component is collected, and treated with acidity adjusting and crystallization to obtain a coarse crystallization; 2) the coarse crystallization is separated by high speed counter current chromatography, monitored by an ultraviolet detector; the objective component is collected according to a spectrum, and reagents are recovered through fraction pressure reduction; and the high purity sanggenon D is obtained after drying. The method has advantages of simply operated technology, high yield, large preparation amount, and a content of the obtained sanggenon D higher than 96%.
Description
Technical field
The invention belongs to biological technical field, particularly relate to a kind of method for preparing high purity sanggenon D.
Background technology
Sanggenon D is a Flavonoid substances, molecular formula C
40H
36O
12, molecular weight 708.7, molecular structural formula:
Sanggenon D, yellow powder, fusing point 175-185 ℃.Be soluble in methyl alcohol, ethanol, acetone etc., water insoluble, chloroform, methylene dichloride, normal hexane, benzene etc. are slightly soluble in ether, ETHYLE ACETATE.That sanggenon D has is hypotensive, antibacterial, anticancer, treatment heart trouble and atherosclerosis effect.
Mostly the existing high purity sanggenon D method that from White Mulberry Root-bark, prepares is to adopt silicagel column, polyamide column or preparation liquid phase separation.Like " from White Mulberry Root-bark, extracting pharmaceutical cpd sanggenon D " that the red people of grade of road direction delivers, the method that the document adopts is: acetone extraction, and the normal hexane washing, extracted with diethyl ether, twice silicagel column separates.But traditional column chromatography for separation can cause product extremely to adsorb, and product yield is low, and complicated operation, and preparation liquid phase separation preparation amount is little.
Summary of the invention:
The object of the invention overcomes the deficiency of prior art, and a kind of method for preparing high purity sanggenon D is provided, and this method utilizes high speed adverse current chromatogram to separate, and is simple to operate, and yield is high.
The objective of the invention is to realize through following technical scheme:
A kind of method for preparing high purity sanggenon D is characterized in that comprising following steps:
1) get the White Mulberry Root-bark pulverizing medicinal materials, add 6-10 and doubly measure 80-90% ethanolic soln refluxing extraction 2-3 time, extracting solution concentrates the acid adjustment deposition; Throw out adds polyamide resin with acetone solution and mixes the appearance oven dry; The polyamide resin column of packing into, the methanol solution gradient elution, thin layer detects; Collect target component acid adjustment crystallization, get coarse crystallization;
2) adopt high speed adverse current chromatogram to separate above-mentioned coarse crystallization, the UV-detector monitoring is collected target component according to collection of illustrative plates, and flow point reclaim under reduced pressure reagent is drying to obtain high purity sanggenon D.
Methanol aqueous solution gradient in the said step 1) is got 60-70% methyl alcohol effective constituent again for getting 4-6BV30-50% methanol-eluted fractions impurity earlier.
Said step 2) the optional chloroform of high speed adverse current chromatogram solvent systems in, methyl alcohol, water solvent system, ratio of mixture 5-10:3-7:2-5 gets and does moving phase mutually, and phase mutually fixes down.
Advantage of the present invention is to adopt high-speed countercurrent chromatography, and this method is a liquid liquid distribution chromatography, does not produce dead absorption, and the sepn process product does not lose, and cooperates the UV-detector on-line monitoring, and is simple to operate, and preparation cycle is short, and preparation amount is bigger, can be continuously produced.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment
Embodiment 1:
Get the White Mulberry Root-bark pulverizing medicinal materials, weighing 5kg drops into 200L stainless steel extractor, adds 10 times of amount 80% ethanolic soln refluxing extraction 2 hours; Extract 2 times, extracting solution concentrates no pure acid adjustment deposition, and throw out adds the 200g polyamide resin with acetone solution and mixes appearance oven dry, the polyamide resin column of packing into; Get 6BV30% methanol-eluted fractions impurity earlier, get 70% methyl alcohol effective constituent again, thin layer detects; Collect the high density flow point, transfer the pH3 crystallization, leach coarse crystallization 12g.Get chloroform, methyl alcohol, water,, take off mutually with being full of the phase that fixes in the high speed adverse current chromatogram post, the rotation main frame in 5: 3: 2 ratios thorough mixing in separating funnel; Speed adjustment is 700rpm, pumps into to do moving phase mutually, and after waiting to set up running balance, flow rate regulation is 2ml/min; Get moving phase dissolving coarse crystallization simultaneously,,, collect target component according to the UV-detector collection of illustrative plates by the sampling valve sample introduction; Reclaim reagent, drying obtains 2.1g sanggenon D, detects content 98.2% through HPLC.
Embodiment 2:
Get the White Mulberry Root-bark pulverizing medicinal materials, weighing 5kg drops into 200L stainless steel extractor, adds 6 times of amount 90% ethanolic soln refluxing extraction 2 hours; Extract 3 times, extracting solution concentrates no pure acid adjustment deposition, and throw out adds the 300g polyamide resin with acetone solution and mixes appearance oven dry, the polyamide resin column of packing into; Get 4BV50% methanol-eluted fractions impurity earlier, get 60% methyl alcohol effective constituent again, thin layer detects; Collect the high density flow point, transfer the pH4 crystallization, leach coarse crystallization 9g.Get chloroform, methyl alcohol, water,, take off mutually with being full of the phase that fixes in the high speed adverse current chromatogram post, the rotation main frame in 7: 5: 3 ratios thorough mixing in separating funnel; Speed adjustment is 850rpm, pumps into to do moving phase mutually, and after waiting to set up running balance, flow rate regulation is 3ml/min; Get moving phase dissolving coarse crystallization simultaneously,,, collect target component according to the UV-detector collection of illustrative plates by the sampling valve sample introduction; Reclaim reagent, drying obtains 2.3g sanggenon D, detects content 95.9% through HPLC.
Embodiment 3:
Get the White Mulberry Root-bark pulverizing medicinal materials, weighing 10kg drops into 200L stainless steel extractor, adds 8 times of amount 80% ethanolic soln refluxing extraction 2 hours; Extract 2 times, extracting solution concentrates no pure acid adjustment deposition, and throw out adds the 400g polyamide resin with acetone solution and mixes appearance oven dry, the polyamide resin column of packing into; Get 4BV50% methanol-eluted fractions impurity earlier, get 70% methyl alcohol effective constituent again, thin layer detects; Collect the high density flow point, transfer the pH3 crystallization, leach coarse crystallization 25g.Get chloroform, methyl alcohol, water,, take off mutually with being full of the phase that fixes in the high speed adverse current chromatogram post, the rotation main frame in 10: 7: 5 ratios thorough mixing in separating funnel; Speed adjustment is 900rpm, pumps into to do moving phase mutually, and after waiting to set up running balance, flow rate regulation is 2ml/min; Get moving phase dissolving coarse crystallization simultaneously,,, collect target component according to the UV-detector collection of illustrative plates by the sampling valve sample introduction; Reclaim reagent, drying obtains 4.5g sanggenon D, detects content 96.8% through HPLC.
Embodiment 4:
Get the White Mulberry Root-bark pulverizing medicinal materials, weighing 10kg drops into 200L stainless steel extractor, adds 8 times of amount 80% ethanolic soln refluxing extraction 2 hours; Extract 2 times, extracting solution concentrates no pure acid adjustment deposition, and throw out adds the 500g polyamide resin with acetone solution and mixes appearance oven dry, the polyamide resin column of packing into; Get 4BV50% methanol-eluted fractions impurity earlier, get 65% methyl alcohol effective constituent again, thin layer detects; Collect the high density flow point, transfer the pH4 crystallization, leach coarse crystallization 20g.Get chloroform, methyl alcohol, water,, take off mutually with being full of the phase that fixes in the high speed adverse current chromatogram post, the rotation main frame in 7: 6: 4 ratios thorough mixing in separating funnel; Speed adjustment is 800rpm, pumps into to do moving phase mutually, and after waiting to set up running balance, flow rate regulation is 3ml/min; Get moving phase dissolving coarse crystallization simultaneously,,, collect target component according to the UV-detector collection of illustrative plates by the sampling valve sample introduction; Reclaim reagent, drying obtains 4.7g sanggenon D, detects content 97.6% through HPLC.
Claims (3)
1. method for preparing high purity sanggenon D is characterized in that comprising following steps:
1) get the White Mulberry Root-bark pulverizing medicinal materials, add 6-10 and doubly measure 80-90% ethanolic soln refluxing extraction 2-3 time, extracting solution concentrates the acid adjustment deposition; Throw out adds polyamide resin with acetone solution and mixes the appearance oven dry; The polyamide resin column of packing into, the methanol solution gradient elution, thin layer detects; Collect target component acid adjustment crystallization, get coarse crystallization;
2) adopt high speed adverse current chromatogram to separate above-mentioned coarse crystallization, the UV-detector monitoring is collected target component according to collection of illustrative plates, and flow point reclaim under reduced pressure reagent is drying to obtain high purity sanggenon D.
2. the method for preparing high purity sanggenon D according to claim 1 is characterized in that the methanol aqueous solution gradient in the said step 1) is: get 4-6BV30-50% methanol-eluted fractions impurity earlier and get 60-70% methyl alcohol effective constituent again.
3. the method for preparing high purity sanggenon D according to claim 1; It is characterized in that said step 2) in the optional chloroform of high speed adverse current chromatogram solvent systems, methyl alcohol, water solvent system; Ratio of mixture 5-10:3-7:2-5 gets and does moving phase mutually, and phase mutually fixes down.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110186579A CN102311445A (en) | 2011-07-05 | 2011-07-05 | Method for preparing high purity sanggenon D |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110186579A CN102311445A (en) | 2011-07-05 | 2011-07-05 | Method for preparing high purity sanggenon D |
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| CN102311445A true CN102311445A (en) | 2012-01-11 |
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| CN201110186579A Pending CN102311445A (en) | 2011-07-05 | 2011-07-05 | Method for preparing high purity sanggenon D |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108703966A (en) * | 2018-07-26 | 2018-10-26 | 大连天星本草生物科技有限公司 | A kind of application of Saliggenon D in the drug or pharmaceutical composition for preparing treatment hyperlipidemia and/or obesity |
-
2011
- 2011-07-05 CN CN201110186579A patent/CN102311445A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108703966A (en) * | 2018-07-26 | 2018-10-26 | 大连天星本草生物科技有限公司 | A kind of application of Saliggenon D in the drug or pharmaceutical composition for preparing treatment hyperlipidemia and/or obesity |
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Application publication date: 20120111 |