CN102688284A - Preparation method of lavender total flavone - Google Patents
Preparation method of lavender total flavone Download PDFInfo
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- CN102688284A CN102688284A CN2011100676059A CN201110067605A CN102688284A CN 102688284 A CN102688284 A CN 102688284A CN 2011100676059 A CN2011100676059 A CN 2011100676059A CN 201110067605 A CN201110067605 A CN 201110067605A CN 102688284 A CN102688284 A CN 102688284A
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Abstract
The invention relates to a preparation method of lavender total flavone, comprising the following steps: 1) that an extract A is obtained by putting lavender in an extraction pot, using deionized water for heated reflux extracting, concentrating an extract solution to a solution specific gravity of 1.1 to 1.2, adding 95% ethanol which is 4-5 times the lavender weight while stirring constantly, allowing the resulting mixture to stand for 12h, and carrying out filtration and pressure-reduced concentration; 2) that an extract B is obtained by using 95% ethanol to carry out heated reflux extracting onherb residues produced instep 1), carrying out reduced pressure concentration on the resulting extract solution, extracting with ethyl acetate, using 95% ethanol for heated dissolution after the extract solution is concentrated to an extract, keeping the solution standing for 24h,filtering, adding the resulting filtrate into an extracted solution, and carrying out pressure-reduced concentration; and 3) that the lavender total flavone is obtained by that the extract A or a mixture of the extract A and the extract B is dissolved with deionized water, added led to a macroporous resin column, eluted with deionized water in 5 times the column volume and 10% ethanol in 5 times the column volume to remove impurities, and eluted with 50-70% alcohol, and that 50-70% ethanol eluate is collected , concentrated and dried.
Description
Technical field
The present invention relates to a kind of method for preparing of total flavones, more particularly relate to the technical field of lavandula angustifolia total flavones method for preparing, belong to the Chinese drug preparation technique field.
Background technology
The fragrant plant lavandula angustifolia belongs to perennial undershrub for the Labiatae lavandula angustifolia; Mainly contain narrow leaf lavandula angustifolia Lavandula angustifola, wide leaf lavandula angustifolia L.spica, three sources of lavandin L.intermedia plant; Originate in the littoral area, Mediterranean of southern foot, Alps, existing extensive cultivating and growing is in all over the world.As the Uygur medicine medicinal herbs most in use; Lavandula angustifolia has dissipation cold, mends the effect of stomach reason brain, dampness pain relieving; Be used for treatment of conditions such as distension and fullness of the chest and abdomen, flu cough with asthma, dizziness headache, shortness of breath and palpitation, joint osteodynia; The history in existing thousands of years of clinical practice is recorded in " Drug Standard of Ministry of Public Health of the Peoples Republic of China-Uigurs medicine fascicle ".At present, the research to lavandula angustifolia both at home and abroad focuses mostly on its quintessence oil, and less to the research of its non-quintessence oil part.The non-quintessence oil part of lavandula angustifolia mainly comprises triterpene, flavone and phenolic acids chemical constituent.Wherein, multiple biological activitys such as flavones ingredient tool antioxidation, antiinflammatory, antitumor and antiviral are widely used among the dietetic food cosmetic field.The medicinal residues of employing HPLC mass spectrometries such as Torras-Claveria L in 2009 after to the purification Herba Lysimachiae foenum-graeci quintessence oil have carried out the research of oxidation-resistant active ingredient; 23 flavone and liposoluble ingredient have therefrom been obtained; And through high-performance liquid chromatogram determination the content of these compositions (J Agric Food Chem.2007,55 (21): 8436-43); Domestic Wu Xia etc. separate from the lavandula angustifolia of Xinjiang and have obtained 7 flavone compounds (CHINA JOURNAL OF CHINESE MATERIA MEDICA, 2007,32 (9): 821-823.); Yang Jie etc. are through obtaining the oxidation resistance that lavandula angustifolia total flavones crude extract has been studied this plant with 50% ethanol extraction, concentrating under reduced pressure and lyophilization; Find that it has the ability (Food Additives Used in China of obvious removing superoxide anion and hydroxy radical; 2010,2:162-165.).
Yet before the present invention, domestic and international various documents only are confined in the laboratory the extraction separation purification of each monomeric compound the research of lavandula angustifolia flavone, and the lavandula angustifolia total flavones of bibliographical information only is a crude extract, i.e. Garden lavender 50% ethanol extraction.Lavandula angustifolia total flavones and preparation method thereof but is not studied, and in suitability for industrialized production, does not use.
In order to address this problem, the invention provides following scheme.
Summary of the invention
The method for preparing that the purpose of this invention is to provide a kind of lavandula angustifolia total flavones, i.e. the method for absorption with macroporous adsorbent resin enrichment lavandula angustifolia total flavones.The preparation technology that the present invention stated has automaticity height, low, the free of contamination advantage of cost, the effective flavones ingredient in the enrichment lavandula angustifolia, and this is that document did not have report in the past.
For realizing above-mentioned purpose, a kind of lavandula angustifolia extractive of general flavone provided by the invention is to prepare through following technical scheme:
(1) raw material is prepared
After gathering the lavandula angustifolia herb, clean, dry or dry, again it is ground into stem length less than 1 centimetre powder.
(2) extract
Lavandula angustifolia medical material with handling well places extraction pot, and the deionized water heating and refluxing extraction of 8 to 12 times of weight of adding 1-3 time is filtered; Merge extractive liquid,, being evaporated to solution proportion is 1.1-1.2, under constantly stirring, adds 95% ethanol (v/v) of 4-5 times of weight; Placed 12 hours, and filtered, filtrate decompression concentrates; Get extractum A, place, subsequent use.
Further above-mentioned steps is extracted the remaining medicinal residues in back, after drying, place extraction pot, 95% ethanol (v/v) heating and refluxing extraction of 6 to 12 times of weight of adding 1-3 time is filtered, and merge extractive liquid, is evaporated to extractum; Extractum with the deionized water suspendible after, with ethyl acetate extraction, after extract is concentrated into extractum,, left standstill 24 hours with 95% ethanol (v/v) heating for dissolving, filter, filtrating is integrated with extraction back solution, concentrating under reduced pressure, extractum B, place, subsequent use.
(3) purification
1. after extractum A being dissolved with the deionized water suspendible; Last macroporous resin column absorption; Earlier,, collect the 50-70% ethanol elution again with 50-70% ethanol (v/v) eluting respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones.
2. extractum A and extractum B are merged; With after the deionized water suspendible dissolving, last macroporous resin column absorption, first respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Again with 50-70% ethanol (v/v) eluting; Collect the 50-70% ethanol elution, concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones.
By the lavandula angustifolia extractive of general flavone of above-mentioned steps preparation, the percentage by weight of its general flavone content is between 50%-70%.
For a better understanding of the present invention, explain that with inventive principle of the present invention and properties of product testing result the present invention is than the excellent part of prior art below.
Principle of the present invention based on:
Macroporous adsorbent resin is a kind of netted opening structure of macromolecule that is polymerized by styrene, stilbene or α-Jia Jibingxisuan ester etc., is the new separation material that combines with adsorptivity and molecular sieve principle.This material absorption affinity in aqueous solution is strong and have a good adsorption selectivity.Its column chromatography is with the method for SPE, guaranteeing that raw medicinal material indicates under the prerequisite of property component content, in absorption effective site with this plant in impurity such as invalid components saccharide and tannin optionally remove.The model commonly used of macroporous resin has D-101, AB-8 and HPD-600 etc., is characterized in that adsorption capacity is big, technological process is short, yield is high, purity is high, resin regeneration is easy, reliable for effect etc.In the present invention, macroporous resin separates impurity such as the invalid components saccharide in the plant, tannin in the absorption flavone to be removed, and under the prerequisite that guarantees flavones ingredient content, effectively enrichment lavandula angustifolia total flavones.
The method for preparing of a kind of lavandula angustifolia extractive of general flavone provided by the invention; Unite extraction through deionized water extraction or deionized water and 95% ethanol (v/v) respectively; Further adopt domestic macroporous adsorbent resin AB-8 type or D101 type or HPD-100 or HPD-400 or HPD-450 or HPD-500 or HPD-600 or HPD-750 enriching and purifying to obtain the lavandula angustifolia total flavones; With the rutin is reference substance, by " percentage by weight of Chinese pharmacopoeia total flavones assay method mensuration general flavone content is 50%-70%.Concrete steps are following:
(1) raw material is prepared
After gathering the lavandula angustifolia herb, clean, dry or dry, again it is ground into stem length less than 1 centimetre powder.
(2) extract
Lavandula angustifolia medical material with handling well places extraction pot, and the deionized water heating and refluxing extraction of 8 to 12 times of weight of adding 1-3 time is filtered; Merge extractive liquid,, being evaporated to solution proportion is 1.1-1.2, under constantly stirring, adds 95% ethanol (v/v) of 4-5 times of weight; Placed 12 hours, and filtered, filtrate decompression concentrates; Get extractum A, place, subsequent use.
Further above-mentioned steps is extracted the remaining medicinal residues in back, after drying, place extraction pot, 95% ethanol (v/v) heating and refluxing extraction of 6 to 12 times of weight of adding 1-3 time is filtered, and merge extractive liquid, is evaporated to extractum; Extractum with the deionized water suspendible after, with ethyl acetate extraction, after extract is concentrated into extractum,, left standstill 24 hours with 95% ethanol (v/v) heating for dissolving, filter, filtrating is integrated with extraction back solution, concentrating under reduced pressure, extractum B, place, subsequent use.
(3) purification
1. after extractum A being dissolved with the deionized water suspendible; Last macroporous resin column absorption; Earlier,, collect the 50-70% ethanol elution again with 50-70% ethanol (v/v) eluting respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones.
2. extractum A and extractum B are merged; With after the deionized water suspendible dissolving, last macroporous resin column absorption, first respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Again with 50-70% ethanol (v/v) eluting; Collect the 50-70% ethanol elution, concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones.
In order to understand the present invention better, further specify essentiality content of the present invention below in conjunction with embodiments of the invention, but content of the present invention is not limited thereto.
The specific embodiment
Embodiment 1
(1) takes by weighing narrow leaf lavandula angustifolia 10kg, be ground into powder, place extraction pot, the deionized water heating and refluxing extraction of 8 times of weight of adding 3 times less than 1cm; Filter, merge extractive liquid,, being evaporated to solution proportion is 1.1, under constantly stirring, adds 95% (v/v) ethanol of 4 times of weight; Placed 12 hours, and filtered, filtrate decompression concentrates; Get extractum A, place, subsequent use.
(2) above-mentioned steps is extracted the remaining medicinal residues in back, after drying, place extraction pot, 95% (v/v) alcohol heating reflux that adds 10 times of weight extracts 2 times, filters, and merge extractive liquid, is evaporated to extractum; Behind the extractum water suspendible, with ethyl acetate extraction, after extract is concentrated into extractum, with 95% ethanol (v/v) heating for dissolving, left standstill 24 hours, filter, filtrating is integrated with in the solution of extraction back, and concentrating under reduced pressure gets extractum B, places, and is subsequent use.
Embodiment 2
With the extractum A in the instance 1 with deionized water suspendible dissolving, last AB-8 macroporous resin column absorption, first respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Again with 70% (v/v) ethanol elution; Collect the ethanol elution of 70% (v/v), concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones; The percentage by weight of flavones content is 62.35%, and yield is 4.54%.
Embodiment 3
With the extractum A in the instance 1 with deionized water suspendible dissolving, last D101 macroporous resin column absorption, first respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Again with 70% (v/v) ethanol elution; Collect the ethanol elution of 70% (v/v), concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones; The percentage by weight of flavones content is 56.12%, and yield is 4.27%.
Embodiment 4
With after the deionized water suspendible dissolving, the absorption of HPD600 macroporous resin column is earlier respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes with the extractum A in the instance 1; Again with 50% (v/v) ethanol elution; Collect the ethanol elution of 50% (v/v), concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones; The percentage ratio of flavones content is 50.21%, and yield is 3.01%.
Embodiment 5
With the extractum A in the instance 1 with after the deionized water suspendible dissolving, last HPD500 macroporous resin column absorption, first respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Again with 70% (v/v) ethanol elution; Collect the ethanol elution of 70% (v/v), concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones; Content is 53.81%, and yield is 3.57%.
Embodiment 6
With the extractum A in the instance 1 with after the deionized water suspendible dissolving, last HPD100 macroporous resin column absorption, first respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Again with 70% (v/v) ethanol elution; Collect the ethanol elution of 70% (v/v), concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones; Content is 56.68%, and yield is 3.73%.
Embodiment 7
With the extractum A in the instance 1 with after the deionized water suspendible dissolving, last HPD400 macroporous resin column absorption, first respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Again with 70% (v/v) ethanol elution; Collect the ethanol elution of 70% (v/v), concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones; Content is 59.70%, and yield is 3.92%.
Embodiment 8
With the extractum A in the instance 1 with after the deionized water suspendible dissolving, last HPD450 macroporous resin column absorption, first respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Again with 70% (v/v) ethanol elution; Collect the ethanol elution of 70% (v/v), concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones; Content is 58.60%, and yield is 3.59%.
Embodiment 9
With the extractum A in the instance 1 with after the deionized water suspendible dissolving, last HPD750 macroporous resin column absorption, first respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Again with 70% (v/v) ethanol elution; Collect the ethanol elution of 70% (v/v), concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones; Content is 56.38%, and yield is 3.52%.
Embodiment 10
Extractum A in the instance 1 and extractum B are merged the back with the dissolving of deionized water suspendible, last AB-8 macroporous resin column absorption, elder generation is respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Again with 70% (v/v) ethanol elution; Collect the ethanol elution of 70% (v/v), concentrate drying gets pale brown toner end, promptly gets the lavandula angustifolia total flavones; Content is 69.31%, and yield is 4.49%.
Embodiment 11
(1) takes by weighing wide leaf lavandula angustifolia 0.5kg, be ground into powder, place extraction pot, the deionized water heating and refluxing extraction of 12 times of weight of adding 2 times less than 1cm; Filter, merge extractive liquid,, being evaporated to solution proportion is 1.2; Under constantly stirring, add 95% (v/v) ethanol of 4 times of weight, placed 12 hours, filter; Filtrate decompression concentrates, and gets extractum A, and is subsequent use; (2) step (1) is extracted the remaining medicinal residues in back, after drying, place extraction pot, 95% (v/v) alcohol heating reflux that adds 6 times of weight extracts 3 times, filters, and merge extractive liquid, is evaporated to extractum; Behind the extractum water suspendible, with ethyl acetate extraction; After extract is concentrated into extractum, with 95% ethanol (v/v) heating for dissolving, left standstill 24 hours, filter, filtrating is integrated with in the solution of extraction back, and concentrating under reduced pressure gets extractum B, and is subsequent use; (3) extractum A and extractum B are merged, with the dissolving of deionized water suspendible, last AB-8 type macroporous resin column absorption; Earlier,, collect the ethanol elution of 70% (v/v) again with 70% (v/v) ethanol elution respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Concentrate drying gets pale brown toner end; Be the lavandula angustifolia total flavones, content is 62.62%, and yield is 4.41%.
Embodiment 12
(1) takes by weighing lavandin 0.5kg, be ground into powder, place extraction pot, the deionized water heating and refluxing extraction of 12 times of weight of adding 1 time less than 1cm; Filter, merge extractive liquid,, being evaporated to solution proportion is 1.2; Under constantly stirring, add 95% (v/v) ethanol of 5 times of weight, placed 12 hours, filter; Filtrate decompression concentrates, and gets extractum A, and is subsequent use; (2) step (1) is extracted the remaining medicinal residues in back, after drying, place extraction pot, 95% (v/v) alcohol heating reflux that adds 12 times of weight extracts 1 time, filters, and merge extractive liquid, is evaporated to extractum; Behind the extractum water suspendible, with ethyl acetate extraction; After extract is concentrated into extractum, with 95% ethanol (v/v) heating for dissolving, left standstill 12 hours, filter, filtrating is integrated with in the solution of extraction back, and concentrating under reduced pressure gets extractum B, and is subsequent use; (3) extractum A and extractum B are merged, with the dissolving of deionized water suspendible, last D101 type macroporous resin column absorption; Earlier,, collect the ethanol elution of 60% (v/v) again with 60% (v/v) ethanol elution respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Concentrate drying gets pale brown toner end; Promptly get the lavandula angustifolia total flavones, content is 56.33%, and yield is 4.08%.
Claims (4)
1. the method for preparing of a lavandula angustifolia total flavones is characterized in that adopting following steps to carry out:
(1) the lavandula angustifolia herb is ground into the powder less than 1cm, places extraction pot, the deionized water heating and refluxing extraction of 8 to 12 times of weight of adding 1-3 time is filtered; Merge extractive liquid,, being evaporated to solution proportion is 1.1-1.2, under constantly stirring, adds 95% ethanol (v/v) of 4-5 times of weight; Placed 12 hours, and filtered, filtrate decompression concentrates; Get extractum A, place, subsequent use.
(2) step (1) is extracted the remaining medicinal residues in back, after drying, place extraction pot, 95% ethanol (v/v) heating and refluxing extraction of 6 to 12 times of weight of adding 1-3 time is filtered, merge extractive liquid,, and being evaporated to does not have the alcohol flavor, with ethyl acetate extraction; After extract is concentrated into extractum, with 95% ethanol (v/v) heating for dissolving, left standstill 24 hours, filter, filtrating is integrated with in the solution of extraction back, and concentrating under reduced pressure gets extractum B, places, and is subsequent use.
(3) with extractum A with after the deionized water suspendible dissolving; Last macroporous resin column absorption; Earlier,, collect 50-70% ethanol (v/v) eluent again with 50-70% ethanol (v/v) eluting respectively with 10% ethanol (v/v) the eluting remove impurity of deionized water and 5 times of column volumes of 5 times of column volumes; Concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones.
Or with extractum A and extractum B merging; After the dissolving of deionized water suspendible, last macroporous resin column absorption is earlier respectively with the deionized water of 5 times of column volumes and 10% ethanol (v/v) eluting of 5 times of column volumes; Again with 50-70% ethanol (v/v) eluting; Collect 50-70% ethanol (v/v) eluent, concentrate drying gets pale brown toner end, is the lavandula angustifolia total flavones.
2. the method for preparing of lavandula angustifolia total flavones according to claim 1 is characterized in that resulting lavandula angustifolia total flavones is pale brown toner end, and the percentage by weight of general flavone content is between 50% to 70%.
3. the method for preparing of lavandula angustifolia total flavones according to claim 1 is characterized in that its source plant is respectively the herb of narrow leaf lavandula angustifolia Lavandula angustifolia, wide leaf lavandula angustifolia Lavandula spica, lavandin Lavandula intermedia.
4. the method for preparing of lavandula angustifolia total flavones according to claim 2 is characterized in that employed macroporous adsorbent resin is domestic macroporous adsorbent resin AB-8 type or D101 type or HPD-100 or HPD-400 or HPD-450 or HPD-500 or HPD-600 or HPD-750.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104825538A (en) * | 2015-05-18 | 2015-08-12 | 江苏耐雀生物工程技术有限公司 | Extraction method of lavender total flavone |
| CN105949249A (en) * | 2016-06-27 | 2016-09-21 | 赣州华汉生物科技有限公司 | Method for extracting lavandula angustifolia flavone from lavandula angustifolia pulp water |
| CN107569527A (en) * | 2017-10-31 | 2018-01-12 | 桂林纽泰生物科技有限公司 | The method that general flavone is extracted from hyperici,herba |
| CN107582593A (en) * | 2017-10-31 | 2018-01-16 | 桂林纽泰生物科技有限公司 | The method that general flavone is extracted from beggar-ticks |
| CN114795992A (en) * | 2022-05-16 | 2022-07-29 | 新疆维吾尔自治区药物研究所 | Composition for preventing and treating skin photodamage and preparation method thereof |
-
2011
- 2011-03-21 CN CN2011100676059A patent/CN102688284A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104825538A (en) * | 2015-05-18 | 2015-08-12 | 江苏耐雀生物工程技术有限公司 | Extraction method of lavender total flavone |
| CN104825538B (en) * | 2015-05-18 | 2019-11-08 | 江苏耐雀生物工程技术有限公司 | A kind of extracting method of lavender total flavone |
| CN105949249A (en) * | 2016-06-27 | 2016-09-21 | 赣州华汉生物科技有限公司 | Method for extracting lavandula angustifolia flavone from lavandula angustifolia pulp water |
| CN107569527A (en) * | 2017-10-31 | 2018-01-12 | 桂林纽泰生物科技有限公司 | The method that general flavone is extracted from hyperici,herba |
| CN107582593A (en) * | 2017-10-31 | 2018-01-16 | 桂林纽泰生物科技有限公司 | The method that general flavone is extracted from beggar-ticks |
| CN114795992A (en) * | 2022-05-16 | 2022-07-29 | 新疆维吾尔自治区药物研究所 | Composition for preventing and treating skin photodamage and preparation method thereof |
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Application publication date: 20120926 |