CN104825586A - Method of extracting flavones from waste liquid after extraction of rose essential oil - Google Patents
Method of extracting flavones from waste liquid after extraction of rose essential oil Download PDFInfo
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- CN104825586A CN104825586A CN201410340940.5A CN201410340940A CN104825586A CN 104825586 A CN104825586 A CN 104825586A CN 201410340940 A CN201410340940 A CN 201410340940A CN 104825586 A CN104825586 A CN 104825586A
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Abstract
The invention discloses a method of extracting flavones from a waste liquid after extraction of rose essential oil through a water vapor distillation method. The method includes following steps: (1) after solid residue of the waste liquid after the extraction of the rose essential oil removed, feeding 100 ml of the waste liquid to macro-porous resin column; (2) performing gradient-elution with an ethanol/water 0-100% solution; (3) performing pressure-reduced concentration and feeding the liquid to a polyamide column and performing gradient-elution with an ethanol/water 0-100% solution; (4) performing concentration and feeding the liquid to an MCI column; and (5) performing gradient-elution with an ethanol/water 0-100% solution to obtain a total flavonoid extract of rose waste liquid after the of the essential oil. The invention can perform advanced development to the natural product, rose flowers, to fully extract the effective components from the rose flowers, so that problems of waste of the effective components from the rose flowers and environmental pollution in the prior art are avoided. The method is simpler in processes, is carried out with toxic-free and harmless solvents and can be used for preparing a high-content flavones product.
Description
Technical field
The present invention relates to a kind of method of the waste liquid after natural product process being carried out to reprocessing, the present invention is exactly a kind of method utilizing the pulp thickening flavone after extraction by steam distillation Flos Rosae Rugosae quintessence oil.
Background technology
Extraction by steam distillation Flos Rosae Rugosae quintessence oil is in Flos Rosae Rugosae, add 4-5 water doubly, then heats at 100 DEG C and boils and carry out extraction of essential oil in 2-3 hour.Liquid in prior art after extraction by steam distillation Flos Rosae Rugosae quintessence oil and waste residue are just simply used as feed additive or are regarded soil fertility quality, or directly discharge abandons, and under latter event, waste liquid also may become a kind of pollutant.
Relevant research shows to there is flavone compound in Flos Rosae Rugosae.It is raw material with Flos Rosae Rugosae that Chinese invention patent application 201210317876.X discloses a kind of, by extractum extraction, silica gel column chromatography chloroform-methanol gradient elution, silica gel column chromatography petroleum ether-ethyl acetate gradient elution, eventually pass high-efficient liquid phase chromatogram purification, obtain a kind of flavone.Obviously, prior art is not suitable for and extracts flavone from extracting the waste liquid after Flos Rosae Rugosae quintessence oil.
Summary of the invention
The invention provides a kind of method utilizing the pulp thickening total flavones after extraction by steam distillation Flos Rosae Rugosae quintessence oil.
The method of flavone is extracted from the waste liquid after extraction Flos Rosae Rugosae quintessence oil, upper macroporous resin column after the waste liquid extracted after Flos Rosae Rugosae quintessence oil is removed solid residue, after ethanol/water 0%-100% solution gradient eluting, upper polyamide column after concentrating under reduced pressure, after ethanol/water 0%-100% solution gradient eluting, upper MCI post after concentrated again, after ethanol/water 0%-100% solution gradient eluting, must extract Flos Rosae Rugosae waste liquid extractive of general flavone after quintessence oil.
The method for optimizing extracting flavone from the waste liquid after extraction Flos Rosae Rugosae quintessence oil of the present invention is: will extract the waste liquid 100mL after Flos Rosae Rugosae quintessence oil, cross D-101 type macroporous resin, first with the distilled water of 4-6 times of column volume, again with 15% alcoholic solution eluting of 4-6 times of column volume, then with 30% ethanol elution of 4-6 times of column volume, reclaim eluent and boil off solvent.Polyamide column on gained sample, first with 4-6 times of column volume distilled water eluting, then with 15% alcoholic solution eluting of 4-6 times of column volume, more then with 30% alcoholic solution eluting of 4-6 times of column volume, reclaim eluent and boil off solvent, the thick product that general flavone content is more than 50% can be obtained.Gained crude product is crossed 100gMCI chromatographic column, first uses 4 times of column volume distilled water eluting, then use 4 times of column volume 15% alcoholic solution eluting, then use 4 times of column volume 30% alcoholic solution eluting, reclaim eluent.Product can be obtained and be about 15mg, general flavone content about 80%.
The present invention can carry out the exploitation of the degree of depth to natural product-Flos Rosae Rugosae, fully extract useful component wherein, avoids waste and the environmental pollution of active ingredient in the Flos Rosae Rugosae that prior art causes.It is relatively more simple that method of the present invention also has method, and the nontoxic solvent used is harmless, can obtain the advantage of high-load flavone product.
detailed description of the invention
A concrete extracting method of the present invention is as follows:
Solid residue is removed by by the waste liquid centrifuging after extraction by steam distillation Flos Rosae Rugosae quintessence oil.Get waste liquid 100mL, cross D-101 type macroporous resin, first with the distilled water eluting of 4-6 times of column volume, then with 15% alcoholic solution eluting of 4-6 times of column volume, then with 30% ethanol elution of 4-6 times of column volume, reclaim eluent and boil off solvent.Polyamide column on gained sample, first with 4-6 times of column volume distilled water eluting, then with 15% alcoholic solution eluting of 4-6 times of column volume, more then with 30% alcoholic solution eluting of 4-6 times of column volume, reclaim eluent and boil off solvent, the thick product that general flavone content is more than 50% can be obtained.Gained crude product is crossed 100g MCI chromatographic column, first use 4 times of column volume distilled water eluting, then use 4 times of column volume 15% alcoholic solution eluting, then use 4 times of column volume 30% alcoholic solution eluting, reclaim eluent.Product can be obtained and be about 15mg, general flavone content about 80%.
The assay method of products obtained therefrom general flavone content of the present invention is as follows:
The preparation of standard solution
Accurately take the rutin mark product 6.6mg that 120 DEG C are dried to constant weight, with the dissolve with ethanol of 60%, transfer in the volumetric flask of 10mL, with 60% ethanol standardize solution, shake up, mother liquid concentration is 0. 66mg/ mL.The above-mentioned solution 0. 2,0. 4,0. 6,0. 8 and 1. 0 of accurate absorption is placed in the volumetric flask of 10mL respectively, adds 0. 3mL 5% NaNO respectively
2solution, shakes up, and after placing 6min, adds 0. 3mL 10% Al (NO respectively under the condition of room temperature
2)
3solution, shakes up, and places 6min, then adds 4% NaOH solution 4mL respectively, finally complement to 10mL with 60% alcoholic solution, shake up, place 15min in the condition of room temperature, take blank reagent as contrast, surveys absorbance y at 510nm place.Take sample size as abscissa, absorbance is that vertical coordinate carries out linear regression, obtains the standard curve of reference substance, and regression equation is y=13.75x-0.0015, R
2=0.9987.Show that the linear relationship of the amount of reference substance and absorbance is good.
Sample tests
Accurately take sample 6.0mg, use 60% dissolve with ethanol, be transferred in 10mL volumetric flask, and with 60% ethanol standardize solution, as test liquid.Survey absorbance y according to the aluminum salt development process of standard solution at 510nm place, calculated the content of flavone by Regression Equations.
Claims (3)
1. from the waste liquid after extraction Flos Rosae Rugosae quintessence oil, extract the method for flavone, upper macroporous resin column after the waste liquid extracted after Flos Rosae Rugosae quintessence oil is removed solid residue, after ethanol/water 0%-100% solution gradient eluting, upper polyamide column after concentrating under reduced pressure, after ethanol/water 0%-100% solution gradient eluting, upper MCI post after concentrated again, after ethanol/water 0%-100% solution gradient eluting, must extract Flos Rosae Rugosae waste liquid extractive of general flavone after quintessence oil.
2. the method extracting flavone from the waste liquid after extraction Flos Rosae Rugosae quintessence oil according to claim 1, it is characterized in that waste liquid 100mL, cross D-101 type macroporous resin, first with the distilled water eluting of 4-6 times of column volume, again with 15% alcoholic solution eluting of 4-6 times of column volume, then with 30% ethanol elution of 4-6 times of column volume, reclaim eluent and boil off solvent, polyamide column on gained sample, first with 4-6 times of column volume distilled water eluting, again with 15% alcoholic solution eluting of 4-6 times of column volume, again then with 30% alcoholic solution eluting of 4-6 times of column volume, reclaim eluent and boil off solvent, the thick product that general flavone content is more than 50% can be obtained.
3. the method extracting flavone from the waste liquid after extraction Flos Rosae Rugosae quintessence oil according to claim 2, claim 1 products obtained therefrom is it is characterized in that to cross 100g MCI chromatographic column, first use 4 times of column volume distilled water eluting, use 4 times of column volume 15% alcoholic solution eluting again, then 4 times of column volume 30% alcoholic solution eluting are used, reclaim eluent, obtain the product of general flavone content about 80%.
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| CN201410340940.5A CN104825586A (en) | 2014-07-17 | 2014-07-17 | Method of extracting flavones from waste liquid after extraction of rose essential oil |
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| CN201410340940.5A CN104825586A (en) | 2014-07-17 | 2014-07-17 | Method of extracting flavones from waste liquid after extraction of rose essential oil |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106377582A (en) * | 2016-08-31 | 2017-02-08 | 上海新亚药业高邮有限公司 | Comprehensive extraction method of peony volatile oil and general flavone |
| CN106668234A (en) * | 2016-12-30 | 2017-05-17 | 成都普思生物科技股份有限公司 | Process for extracting and purifying total flavone from rose flower |
| WO2019233158A1 (en) * | 2018-06-08 | 2019-12-12 | 苏州思源天然产物研发有限公司 | Traditional chinese medicine gel composition, preparation method and use thereof |
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| CN1687053A (en) * | 2005-03-23 | 2005-10-26 | 中国科学院西北高原生物研究所 | Technique for extracting general flavonoid from seeds of nitraria |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106377582A (en) * | 2016-08-31 | 2017-02-08 | 上海新亚药业高邮有限公司 | Comprehensive extraction method of peony volatile oil and general flavone |
| CN106668234A (en) * | 2016-12-30 | 2017-05-17 | 成都普思生物科技股份有限公司 | Process for extracting and purifying total flavone from rose flower |
| CN106668234B (en) * | 2016-12-30 | 2019-10-18 | 成都普思生物科技股份有限公司 | Rose extraction and purification process for total flavonoids |
| WO2019233158A1 (en) * | 2018-06-08 | 2019-12-12 | 苏州思源天然产物研发有限公司 | Traditional chinese medicine gel composition, preparation method and use thereof |
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