CN101690739B - Preparation method of dogbane leaf extractive - Google Patents
Preparation method of dogbane leaf extractive Download PDFInfo
- Publication number
- CN101690739B CN101690739B CN2009100671965A CN200910067196A CN101690739B CN 101690739 B CN101690739 B CN 101690739B CN 2009100671965 A CN2009100671965 A CN 2009100671965A CN 200910067196 A CN200910067196 A CN 200910067196A CN 101690739 B CN101690739 B CN 101690739B
- Authority
- CN
- China
- Prior art keywords
- apocyni veneti
- extract
- ethanol
- herba apocyni
- dogbane leaf
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Cosmetics (AREA)
Abstract
The invention provides a preparation method of dogbane leaf extractive. Acid alcohol solution is utilized to extract dogbane leaf general flavone and contained effective constituents such as hyperoside, iso-quercetin, quercetin and kaempferide. The dogbane leaf extractive in the shape of dry extract can be obtained by the preparation method provided in the invention, the productivity of the extract is 7.0-7.8%, the content of general flavone of the dogbane leaf extractive which is in the shape of dry extract and obtained by the detection of an ultraviolet-visible spectrophotometer is 58-70%. Proved by efficient liquid chromatogram detection, the content of iso-quercetin, hyperoside, quercetin and kaempferide in the dogbane leaf general flavone obtained by the extract method is increased by 5-30 times compared with general extract methods. The method is convenient, efficient, easy in operation and low in cost, can meet the demands of development and utilization of drug and food fields, and has infinite application and development value.
Description
Technical field
The present invention relates to a kind of preparation method of dogbane leaf extractive.
Background technology
The Chinese medicine Folium Apocyni Veneti is the dried leaves of Hypericaceae plant Herba Apocyni veneti Apocynum venetum.Summer, Qiu Erji gather, and dry.The Chinese medicine Folium Apocyni Veneti has the function of suppressing the hyperactive liver pain relieving, nourishing blood for regulating menstruation, astringing YIN to stop sweating, disease such as dizzy, the hypochondriac pain of being usually used in having a headache, stomachache, extremity spasm, blood deficiency and yellow complexion, menoxenia, spontaneous perspiration, night sweat.Flavone is the important active component of Herba Apocyni veneti Ye Zhongyi class, because very low, have important researching value and application prospects so how to find a kind of conveniently extracting method to obtain isoquercitin, Quercetin, the higher total flavones of kaempferide content with component contents such as isoquercitin, Quercetin, kaempferide in the resulting flavones ingredient of general extracting method extraction Folium Apocyni Veneti.
The normal at present method for preparing the Folium Apocyni Veneti total flavones that adopts is direct extraction Folium Apocyni Veneti, the purified again Folium Apocyni Veneti total flavones that makes.Kindir leaf total flavone extract, its preparation and application that Wang Xianrong etc. propose at Chinese patent (application number 200510123187); Li Qingshan etc. are at the extraction separation method of the effective part from dogbane of Chinese patent (application number 02110431) proposition; Yang Xin's ripples etc. are in preparation method and the pharmaceutical preparation and the hepatopathy purposes of a kind of Herba Apocyni veneti extract of Chinese patent (application number 200610083809) proposition.Described several method all extracts raw-material proper constituent with general reagent, can not increase the content of isoquercitin in the extract, Quercetin, kaempferide.
Summary of the invention
The invention provides a kind of preparation method of dogbane leaf extractive.
The invention provides a kind of preparation method of dogbane leaf extractive, its step and condition are as follows: the Herba Apocyni veneti medical material is placed extraction vessel, adding volume ratio is that 30～80% ethanol waters extract, use sulphuric acid, nitric acid, it is 3～6 that hydrochloric acid or acetic acid are regulated pH, the addition ml of ethanol water: the quality g of Herba Apocyni veneti medical material is 5～20, extracting temperature is 95 ℃～300 ℃, each extraction time is 0.5～2 hour, repeat to extract 1～4 time, merge extractive liquid,, extraction solution concentration after will merging behind the recovery ethanol is to 1/4～1/10 of original volume, concentrated solution left standstill 3～24 hours, macroporous resin column on the supernatant, the model of macroporous resin is D101, D130, AB8 or NKA, described exsiccant macroporous resin quality g: the quality g of Herba Apocyni veneti medical material is 1: 0.5～1: 2, elder generation's water eluting, the effluent achromaticity and clarification that is eluted to macroporous resin column is transparent, pH value is 7, the reuse volume ratio is 40%～60% ethanol water eluting, it is transparent to be eluted to the ethanol elution achromaticity and clarification, collects the eluent of ethanol water, reclaims ethanol, drying obtains the Herba Apocyni veneti medicinal substances extract of dry extract shape; Described Herba Apocyni veneti medical material is Folium Apocyni Veneti or Folium Apocyni Veneti powder; This Herba Apocyni veneti medical material contains the Herba Apocyni veneti total flavones, and contain isoquercitin in this total flavones, hyperin, Quercetin and kaempferide.
Preparation method provided by the invention got a kind of dogbane leaf extractive of dry extract shape, with the content that contains isoquercitin, hyperin, Quercetin and kaempferide in the Herba Apocyni veneti content of total flavone of this extract of colorimetric method for determining and this total flavones.
A kind of dogbane leaf extractive that preparation method provided by the invention got the dry extract shape is an effective medicinal components, makes the precursor of pharmaceutical preparation with this effective ingredient, is mainly used in the depression of the various degree that a variety of causes causes.
Utilizing ultraviolet-visible spectrophotometer, is external standard drawing standard curve with the standard substance rutin of variable concentrations, as absorbing wavelength, measures in resulting powder flavones content by absorption value with 510nm.And utilize high performance liquid chromatography, come the content of isoquercitin, hyperin, Quercetin, kaempferide in more general extracting method and the resulting total flavones of extracting method of the present invention by chromatographic peak area.High performance liquid chromatograph is: and Waters (Milford, MA, USA) 2690 and be equipped with the diode array monitor, detect wavelength and for the 360nm. high-efficient liquid phase chromatogram condition be: chromatographic column is: Agilent C18,250 * 4.6mm, 5 μ m; Mobile phase consists of 0.2% glacial acetic acid aqueous solution (A) and acetonitrile (B). and type of elution is: 0-20 minute: 13%B; 20-60 minute: 13-40%B; 60-90 minute: the 40-100%B. elution speed was: 0.5ml/min, chromatogram column temperature is: 28 ℃.
Beneficial effect: the invention provides a kind of preparation method of Herba Apocyni veneti extract, obtain a kind of medicinal substances extract of dry extract shape.The weight of extract is for extracting the 7.0-7.8% with Herba Apocyni veneti weight, detects the 58-70% that general flavone content in a kind of dogbane leaf extractive that obtains the dry extract shape accounts for extract through ultraviolet-visible spectrophotometer.Detect proof through high performance liquid chromatography, the content of isoquercitin, hyperin, Quercetin, kaempferide is than having increased by 5～30 times in the general extracting method in the Folium Apocyni Veneti total flavones that this extracting method obtains.The method is convenient, efficient, easy operating, and with low cost, can satisfy the development and utilization of medicine, field of food, uses, develops value greatly.
Description of drawings
Fig. 1 is the chromatogram of the resulting Folium Apocyni Veneti total flavones of general extracting method, and peak 1 is a rutin in the chromatogram of total flavones, and peak 2 is an isoquercitin, and peak 3 is a hyperin, and peak 4 is a Quercetin, and peak 5 is a kaempferide.Rutin content is very high in the chromatogram, and isoquercitin, hyperin, Quercetin, kaempferide content are very low.
Fig. 2 extracts the chromatogram that obtains the Folium Apocyni Veneti total flavones for extracting method embodiment 2 provided by the invention.Same Fig. 1 of the composition at peak 1～5 in the chromatogram.From the chromatogram rutin hydrolysis as can be seen of total flavones, thereby the content of isoquercitin, hyperin, Quercetin, kaempferide is significantly improved.
The specific embodiment
Embodiment 1
With the Folium Apocyni Veneti pulverizing medicinal materials, take by weighing 100g, put in the extraction vessel, adding the 1000ml volume ratio is 50% ethanol water, regulates PH to 3 with sulphuric acid, extract with 100 ℃ temperature, extract 4 times, each 1 hour, merge extractive liquid,, reclaim ethanol, be concentrated into 1/4 of original volume, static 10 hours of concentrated solution, the exsiccant macroporous resin column of 100g on the supernatant, elder generation's water eluting, the effluent achromaticity and clarification that is eluted to macroporous resin column is transparent, and pH value is 7, and the reuse volume ratio is that 50% ethanol water carries out eluting, it is transparent to be eluted to the alcoholic solution achromaticity and clarification, about 5 times of column volumes, the eluent of collection ethanol water reclaims ethanol, drying obtains a kind of dogbane leaf extractive of dry extract shape.The weight of extract is for extracting with 7.2% of Herba Apocyni veneti weight, and detecting a kind of dogbane leaf extractive general flavone content that obtains the dry extract shape through ultraviolet-visible spectrophotometer is 62%
With the Folium Apocyni Veneti pulverizing medicinal materials, take by weighing 200g, put in the extraction vessel, adding the 2000ml volume ratio is 60% ethanol water, regulates PH to 4 with hydrochloric acid, extract with 120 ℃ temperature, extract 3 times, each 1.5 hours, merge extractive liquid,, reclaim ethanol, be concentrated into 1/5 of original volume, static 20 hours of concentrated solution, the exsiccant macroporous resin column of 200g on the supernatant, elder generation's water eluting, the effluent achromaticity and clarification that is eluted to macroporous resin column is transparent, and pH value is 7, and the reuse volume ratio is that 60% ethanol water carries out eluting, it is transparent to be eluted to the alcoholic solution achromaticity and clarification, about 5 times of column volumes, the eluent of collection ethanol water reclaims ethanol, drying obtains a kind of dogbane leaf extractive of dry extract shape.The weight of extract is for extracting with 7.0% of Herba Apocyni veneti weight, and detecting a kind of dogbane leaf extractive general flavone content that obtains the dry extract shape through ultraviolet-visible spectrophotometer is 68%.
With the Folium Apocyni Veneti pulverizing medicinal materials, take by weighing 150g, put in the extraction vessel, adding the 2000ml volume ratio is 80% ethanol water, regulates PH to 6 with sulphuric acid, extract with 150 ℃ temperature, extract 4 times, each 1 hour, merge extractive liquid,, reclaim ethanol, be concentrated into 1/4 of original volume, static 15 hours of concentrated solution, the exsiccant macroporous resin column of 150g on the supernatant, elder generation's water eluting, the effluent achromaticity and clarification that is eluted to macroporous resin column is transparent, and pH value is 7, and the reuse volume ratio is that 50% ethanol water carries out eluting, it is transparent to be eluted to the alcoholic solution achromaticity and clarification, about 5 times of column volumes, the eluent of collection ethanol water reclaims ethanol, drying obtains a kind of dogbane leaf extractive of dry extract shape.The weight of extract is for extracting with 7.5% of Herba Apocyni veneti weight, and detecting a kind of dogbane leaf extractive general flavone content that obtains the dry extract shape through ultraviolet-visible spectrophotometer is 58%.
With the Folium Apocyni Veneti pulverizing medicinal materials, take by weighing 100g, put in the extraction vessel, adding the 1500ml volume ratio is 50% ethanol water, regulates PH to 5 with hydrochloric acid, extract with 180 ℃ temperature, extract 3 times, each 2 hours, merge extractive liquid,, reclaim ethanol, be concentrated into 1/4 of original volume, static 20 hours of concentrated solution, the exsiccant macroporous resin column of 150g on the supernatant, elder generation's water eluting, the effluent achromaticity and clarification that is eluted to macroporous resin column is transparent, and pH value is 7, and the reuse volume ratio is that 55% ethanol water carries out eluting, it is transparent to be eluted to the alcoholic solution achromaticity and clarification, about 5 times of column volumes, the eluent of collection ethanol water reclaims ethanol, drying obtains a kind of dogbane leaf extractive of dry extract shape.The weight of extract is for extracting with 7.3% of Herba Apocyni veneti weight, and detecting a kind of dogbane leaf extractive general flavone content that obtains the dry extract shape through ultraviolet-visible spectrophotometer is 68%.
With the Folium Apocyni Veneti pulverizing medicinal materials, take by weighing 250g, put in the extraction vessel, adding the 3000ml volume ratio is 50% ethanol water, regulates PH to 6 with sulphuric acid, extract with 200 ℃ temperature, extract 4 times, each 2 hours, merge extractive liquid,, reclaim ethanol, be concentrated into 1/4 of original volume, static 24 hours of concentrated solution, the exsiccant macroporous resin column of 300g on the supernatant, elder generation's water eluting, the effluent achromaticity and clarification that is eluted to macroporous resin column is transparent, and pH value is 7, and the reuse volume ratio is that 60% ethanol water carries out eluting, it is transparent to be eluted to the alcoholic solution achromaticity and clarification, about 5 times of column volumes, the eluent of collection ethanol water reclaims ethanol, drying obtains a kind of dogbane leaf extractive of dry extract shape.The weight of extract is for extracting with 7.8% of Herba Apocyni veneti weight, and detecting a kind of dogbane leaf extractive general flavone content that obtains the dry extract shape through ultraviolet-visible spectrophotometer is 70%.
Claims (1)
1. preparation method of dogbane leaf extractive, its step and condition are as follows: the Herba Apocyni veneti medical material is placed extraction vessel, adding volume ratio is that 30～80% ethanol waters extract, use sulphuric acid, nitric acid, it is 3～6 that hydrochloric acid or acetic acid are regulated pH, the addition ml of ethanol water: the quality g of Herba Apocyni veneti medical material is 5～20, extracting temperature is 95 ℃～300 ℃, each extraction time is 0.5～2 hour, repeat to extract 1～4 time, merge extractive liquid,, extraction solution concentration after will merging behind the recovery ethanol is to 1/4～1/10 of original volume, concentrated solution left standstill 3～24 hours, macroporous resin column on the supernatant, the model of macroporous resin is D101, D130, AB8 or NKA, described exsiccant macroporous resin quality g: the quality g of Herba Apocyni veneti medical material is 1: 0.5～1: 2, elder generation's water eluting, the effluent achromaticity and clarification that is eluted to macroporous resin column is transparent, pH value is 7, the reuse volume ratio is 40%～60% ethanol water eluting, it is transparent to be eluted to the ethanol elution achromaticity and clarification, collects the eluent of ethanol water, reclaims ethanol, drying obtains the Herba Apocyni veneti medicinal substances extract of dry extract shape; Described Herba Apocyni veneti medical material is Folium Apocyni Veneti or Folium Apocyni Veneti powder; This Herba Apocyni veneti medical material contains the Herba Apocyni veneti total flavones, and contain isoquercitin in this total flavones, hyperin, Quercetin and kaempferide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100671965A CN101690739B (en) | 2009-06-30 | 2009-06-30 | Preparation method of dogbane leaf extractive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100671965A CN101690739B (en) | 2009-06-30 | 2009-06-30 | Preparation method of dogbane leaf extractive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101690739A CN101690739A (en) | 2010-04-07 |
| CN101690739B true CN101690739B (en) | 2011-07-13 |
Family
ID=42079489
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100671965A Active CN101690739B (en) | 2009-06-30 | 2009-06-30 | Preparation method of dogbane leaf extractive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101690739B (en) |
Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966139B (en) * | 2010-10-26 | 2015-06-10 | 戈宝绿业(深圳)有限公司 | Apocynum venetum extract, preparation method thereof and application thereof to cosmetics |
| CN102190693B (en) * | 2011-03-29 | 2013-10-09 | 江苏省中医院 | Method for preparing hyperin from Dogbane leaves |
| CN102197887B (en) * | 2011-05-23 | 2013-04-17 | 新疆戈宝红麻有限公司 | Health-care brassiere made of Apocynum venetum Linn |
| CN102659740B (en) * | 2012-04-26 | 2014-04-02 | 西安医学院 | Method for extracting quercetin from eucommia leaves |
| CN103830292A (en) * | 2014-03-05 | 2014-06-04 | 吉林化工学院 | Apocynum flavonoid extract and preparation method thereof |
| CN104644707A (en) * | 2014-06-26 | 2015-05-27 | 钟延华 | Method for extracting total flavonoids from dogbane leaves |
| CN104490961A (en) * | 2014-12-25 | 2015-04-08 | 长春师范大学 | Preparation method and application of folium apocyni veneti extract |
| CN105663190B (en) * | 2016-02-22 | 2019-04-26 | 廊坊师范学院 | Apocynum extract and its purification process |
| CN105699557A (en) * | 2016-04-25 | 2016-06-22 | 广西壮族自治区梧州食品药品检验所 | Method for measuring content of kaempferide in momordica grosvenori fruit tea through high performance liquid chromatography |
| CN109908162B (en) * | 2017-12-12 | 2022-10-28 | 广州白云山和记黄埔中药有限公司 | Pharmaceutical composition for treating depression, preparation and medical application thereof |
| CN108542929A (en) * | 2018-07-05 | 2018-09-18 | 吉林化工学院 | Bluish dogbane total polyphenol extract and preparation method thereof |
| CN108926506B (en) * | 2018-09-27 | 2022-02-25 | 中国农业科学院麻类研究所 | Method for extracting flavonol components in jute leaves, extract and application thereof |
| CN110057931A (en) * | 2019-04-10 | 2019-07-26 | 长春师范大学 | The detection method of reversed-phased high performace liquid chromatographic detection osmund ketone standard substance |
| CN116077542A (en) * | 2023-02-01 | 2023-05-09 | 西藏天虹科技股份有限责任公司 | Preparation method of apocynum venetum extract |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1931205A (en) * | 2005-12-16 | 2007-03-21 | 周亚球 | Kindir leaf total flavone extract and its prepn and application |
-
2009
- 2009-06-30 CN CN2009100671965A patent/CN101690739B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1931205A (en) * | 2005-12-16 | 2007-03-21 | 周亚球 | Kindir leaf total flavone extract and its prepn and application |
Non-Patent Citations (1)
| Title |
|---|
| 张素琼，等.大孔树脂同步分离纯化罗布麻叶总黄酮和总鞣质的研究.《中国中药杂志》.2008,第33卷(第10期),1141-1144. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101690739A (en) | 2010-04-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101690739B (en) | Preparation method of dogbane leaf extractive | |
| CN102451235B (en) | Preparation method of olive leaf extract | |
| CN101336987B (en) | Preparation method of total flavone of Hovenia dulcisThunb | |
| CN101985421A (en) | Method for simultaneously preparing chlorogenic acid and luteoloside from honeysuckle flower | |
| CN103110670A (en) | Preparation method for efficiently extracting separating high-purity flavone components from ginkgo leaf | |
| CN100484948C (en) | Method for separating derivative of vitexin | |
| CN104173221A (en) | Novel application of prunus mume extract | |
| CN106266262A (en) | A kind of Callicarpa nudiflora extract with antiinflammatory action | |
| CN105732250A (en) | Preparing method for high-purity grifola frondosa polyphenol component | |
| CN101524458B (en) | Extract of smilax glabra saponins and flavonoid and preparation method thereof | |
| CN103191041A (en) | Chinese yew branch and leaf extractive with anti-oxidative effect as well as extraction method and application of yew branch and leaf extractive | |
| CN102526127B (en) | Flash type extraction method for active constituents in cordyceps militaris | |
| CN102233013A (en) | Preparation method for total saponins of pulsatilla chinensis | |
| CN104940280A (en) | Method for extracting total flavones from radix puerariae employing enzyme preparation | |
| CN104610401B (en) | A kind of method for extracting baicalin, baicalin and wogonin from Radix Scutellariae simultaneously | |
| CN100368421C (en) | Method for picking up and separating compound of flavone being as effective content of cinquefoil, and application | |
| CN101234147A (en) | Method of preparing total flavones of tropaeolum for injections | |
| CN112999274A (en) | Rose polyphenol extract and preparation method and application thereof | |
| CN101732421A (en) | Method for preparing total flavonoids, total tannins and galic acid compounds of polygonum capitatum | |
| CN111595972A (en) | Preparation method and quality detection method of lithocarpus polystachyus rehd total flavone extract | |
| CN106038828A (en) | Callicarpa nudiflora extract containing rich verbascoside and preparation method of callicarpa nudiflora extract | |
| CN109394609A (en) | A kind of Waxberry leaf extract and preparation method thereof and the application in cosmetics | |
| CN102000125B (en) | Ginkgo flavone extraction method | |
| CN108126000A (en) | Arasaponin extracts preparation method in fresh Radix Notoginseng | |
| CN102659740B (en) | Method for extracting quercetin from eucommia leaves |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: SHANXI YABAO PHARMACEUTICAL GROUP CORP. Free format text: FORMER OWNER: CHANGCHUN NORMAL COLLEGE Effective date: 20130718 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 130012 CHANGCHUN, JILIN PROVINCE TO: 044600 YUNCHENG, SHAANXI PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20130718 Address after: 044600 Fumin Road, Ruicheng County, Shanxi, China, No. 43, No. Patentee after: Shanxi Yabao Pharmaceutical Group Corp. Address before: 130012 Jilin province Changchun Changji City Road No. 677 Patentee before: Changchun Normal University |