CN105541941A - Method for extracting and separating rhoifolin from exocarpium leaves - Google Patents
Method for extracting and separating rhoifolin from exocarpium leaves Download PDFInfo
- Publication number
- CN105541941A CN105541941A CN201610028881.7A CN201610028881A CN105541941A CN 105541941 A CN105541941 A CN 105541941A CN 201610028881 A CN201610028881 A CN 201610028881A CN 105541941 A CN105541941 A CN 105541941A
- Authority
- CN
- China
- Prior art keywords
- rhoifoloside
- extraction
- pummelo peel
- solution
- extracting
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Saccharide Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention provides a method for extracting and separating rhoifolin from exocarpium leaves. The method comprises the following steps: crushing and filtering exocarpium leaves; extracting the filtered exocarpium leaf powder to obtain an extracting solution; purifying the extracting solution to obtain the rhoifolin. The rhoifolin in the exocarpium leaves accounts for 3.0 to 6.8 percent of dry substances, and the amount is dozens of times that in folium turpiniae or rutaceae exocarpium citri grandis fruits. An extracting solvent is 95% ethyl alcohol, thus entering of water-soluble substances in the extracting solution is reduced; a product with high purity is obtained by extracting a concentrated solution using an n-butyl alcohol and petroleum ether gradient mixed solution; the rhoifolin with the purity of 98% or above is obtained after the product is crystallized and re-crystallized in an aqueous solution. The process flow is simple and applicable to batch production of the rhoifolin.
Description
Technical field
The present invention relates to field of natural medicinal chemistry, be specifically related to a kind of method of extraction and isolation Rhoifoloside from Pummelo Peel leaf.
Background technology
Rhoifoloside Rhoifolin is flavonoids.Rhoifoloside derives from dry leave and the rutaceae of Gu You section Turpinia pomifera(Roxb) D O., for pharmacy, and pharmacological action: antitumor, hypertension, xanthine oxidase inhibitor and antioxidant.
The material of existing extraction Rhoifoloside is mainly leaf of Turpinia pomifera (Roxb) D O. or Rutaceae Citrus grandis Osbeck. Var.tomentosa Hort. fruit, and their content is all lower, only accounts for 0.1 ~ 0.6% of dry-matter.Existing production technique mainly contains solvent extration, supercritical extraction, resin adsorption method and Ultra filtration membrane technology etc.Solvent extration method is simple, but the impurity extracted is also many, the cumbersome of subsequent purification, and supercritical extraction equipment investment is large, and resin adsorption method and Ultra filtration membrane technical matters more complicated, yield is low, and industrialization degree is low.
Summary of the invention
Above-mentioned deficiency is there is for prior art, the invention provides a kind of method of extraction and isolation Rhoifoloside from Pummelo Peel leaf, in the present invention, Extraction solvent is 95% ethanol, water-soluble substances can be reduced and enter extracting solution, extract concentrated solution with propyl carbinol and sherwood oil gradient mixed solution, obtain purity high product, crystallization and recrystallization in aqueous, obtain the Rhoifoloside of purity more than 98%, and technical process of the present invention is simple, is applicable to produce Rhoifoloside in enormous quantities.
Technical scheme of the present invention is, a kind of method of extraction and isolation Rhoifoloside from Pummelo Peel leaf, comprises the following steps:
Pummelo Peel leaf is pulverized and filters;
Pummelo Peel leaf powder after filtration is carried out extraction and obtains extracting solution;
Extracting solution is carried out purifying and obtains Rhoifoloside.
Above-mentioned method, wherein, describedly to pulverize Pummelo Peel leaf and in the step of filtering, wherein said being filtered into is filtered by 40 eye mesh screens.
Above-mentioned method, wherein, described Pummelo Peel leaf powder after filtering is carried out extracting the step obtaining extracting solution and comprises:
Choose the glass chromatography column that diameter is 2.5cm;
By Pummelo Peel leaf powder with 95% ethanol wet sample upper prop and in post soak 1 hour;
Solution after soaking is collected the elutriant of 6 times amount with 95% ethanol elution;
Elutriant concentrating under reduced pressure is obtained extracting solution.
Above-mentioned method, wherein, describedly extracting solution is carried out the step that purifying obtains Rhoifoloside and comprise:
Concentrated extracting solution sherwood oil and propyl carbinol mixed solution are extracted repeatedly;
The subnatant of extraction is concentrated;
Lower floor's concentrated solution cold water is divided three times clean and centrifugal segregation water-soluble impurity obtain the thick product of Rhoifoloside;
Thick for Rhoifoloside product is placed in hot water dissolve, puts refrigerator crystallisation by cooling and recrystallization, obtain the Rhoifoloside of purity more than 98%.
Above-mentioned method, wherein, describedly carries out purifying by extracting solution and obtains in the step of Rhoifoloside: the extraction agent used in described purifying is sherwood oil and propyl carbinol mixed solution.
Above-mentioned method, wherein, the ratio of described sherwood oil and propyl carbinol mixed solution is 8: 2; 6: 4; 4: 6; 2: 8, and the sherwood oil mixed by often kind of proportioning and propyl carbinol mixed solution respectively extract 1 time successively.
The method of a kind of extraction and isolation Rhoifoloside from Pummelo Peel leaf provided by the invention, comprises the following steps: pulverized by Pummelo Peel leaf and filter; Pummelo Peel leaf powder after filtration is carried out extraction and obtains extracting solution; Extracting solution is carried out purifying and obtains Rhoifoloside, open country paint glycosides in the present invention in Pummelo Peel blade accounts for 3.0 ~ 6.8% of dry-matter, it is tens times of leaf of Turpinia pomifera (Roxb) D O. or Rutaceae Citrus grandis Osbeck. Var.tomentosa Hort. fruit, in the present invention, Extraction solvent is 95% ethanol, reduce water-soluble substances and enter extracting solution, concentrated solution is extracted with propyl carbinol and sherwood oil gradient mixed solution, obtain purity high product, crystallization and recrystallization in aqueous, obtain the Rhoifoloside of purity more than 98%, and this technical process is simple, be applicable to produce Rhoifoloside in enormous quantities.
Embodiment
In the following description, a large amount of concrete details is given to provide more thorough understanding of the invention.But, it is obvious to the skilled person that the present invention can be implemented without the need to these details one or more.In other example, in order to avoid obscuring with the present invention, technical characteristics more well known in the art are not described.
In order to thoroughly understand the present invention, detailed step and detailed structure will be proposed in following description, to explain technical scheme of the present invention.Preferred embodiment of the present invention is described in detail as follows, but except these are described in detail, the present invention can also have other embodiments.
The invention provides a kind of method of extraction and isolation Rhoifoloside from Pummelo Peel leaf, comprise the following steps:
Step S1: pulverized by Pummelo Peel leaf and filter, wherein said being filtered into is filtered by 40 eye mesh screens.
Step S2: the Pummelo Peel leaf powder after filtration is carried out extraction and obtains extracting solution, specifically comprise:
Step S2a: choose the glass chromatography column that diameter is 2.5cm.
Step S2b: to be wet sample upper prop soaking 1 hour in post with 95% ethanol by Pummelo Peel leaf powder, such as, gets 200 and digests Exocarpium Citri Rubrum leaf powder 95% ethanol and to wet sample upper prop, immersion 1 hour in post.
Step S2c: solution after soaking is collected the elutriant of 6 times amount with 95% ethanol elution, such as, digest Exocarpium Citri Rubrum leaf powder 95% ethanol to wet sample upper prop when getting 200, soak 1 hour in post, use 95% ethanol elution, collect 6 times amount (V/W) i.e. 300mL elutriant.
Step S2d: elutriant concentrating under reduced pressure is obtained extracting solution, obtains extracting solution concentrating under reduced pressure and is about 10mL.
Step S3: extracting solution is carried out the step that purifying obtains Rhoifoloside and comprise:
Step S3a: concentrated extracting solution sherwood oil and propyl carbinol mixed solution are extracted repeatedly, is specially concentrated solution and uses sherwood oil and propyl carbinol mixed solution (8: 2 successively; 6: 4; 4: 6; 2: 8) 25mL respectively extracts 1 time successively.
Step S3b: concentrated by the subnatant of extraction, be specially, discard upper liquid, subnatant concentrates.
Step S3c: divided by lower floor's concentrated solution cold water and clean and centrifugal segregation water-soluble impurity for three times, be specially and divide three centrifugal solubility impurities that anhydrate of cleaning with a small amount of cold water, namely the throw out removed after water-soluble impurity is the thick product of Rhoifoloside.
Step S3d: thick for Rhoifoloside product is placed in hot water and dissolves, put refrigerator crystallisation by cooling and recrystallization, obtain the Rhoifoloside of purity more than 98%, be specially and thick product is placed in hot water dissolves, put refrigerator crystallisation by cooling and recrystallization, obtain the Rhoifoloside of purity more than 98%.
In the present invention one preferred embodiment, extracting solution is carried out purifying and obtains in the step of Rhoifoloside: the extraction agent used in described purifying is sherwood oil and propyl carbinol mixed solution, further, the ratio of sherwood oil and propyl carbinol mixed solution is 8: 2; 6: 4; 4: 6; 2: 8, and the sherwood oil mixed by often kind of proportioning and propyl carbinol mixed solution respectively extract 1 time successively.
One specific embodiment is below provided, sets forth the method for a kind of extraction and isolation Rhoifoloside from Pummelo Peel leaf of the present invention further:
Embodiment one, a kind of method of extraction and isolation Rhoifoloside from Pummelo Peel leaf, specifically comprises the following steps, with Pummelo Peel leaf for raw material, pulverize, cross 40 mesh sieves, choose the glass chromatography column that diameter is 2.5cm, 200 digest Exocarpium Citri Rubrum leaf powder 95% ethanol wets sample upper prop, soak 1 hour in post, use 95% ethanol elution equally, collect 6 times amount (V/W) i.e. 300mL elutriant, extracting solution concentrating under reduced pressure is about 10mL, and concentrated solution uses sherwood oil and propyl carbinol mixed solution (8: 2 successively; 6: 4; 4: 6; 2: 8) 25mL respectively extracts 1 time, discard upper liquid, subnatant concentrates, divide with a small amount of cold water and clean the centrifugal solubility impurity that anhydrates three times, namely throw out is the thick product of Rhoifoloside that purity is higher, dissolve in thick product hot water, put refrigerator crystallisation by cooling and recrystallization, obtain the Rhoifoloside of purity more than 98%.
In sum, the method for a kind of extraction and isolation Rhoifoloside from Pummelo Peel leaf provided by the invention, comprises the following steps: pulverized by Pummelo Peel leaf and filter; Pummelo Peel leaf powder after filtration is carried out extraction and obtains extracting solution; Extracting solution is carried out purifying and obtains Rhoifoloside, open country paint glycosides in the present invention in Pummelo Peel blade accounts for 3.0 ~ 6.8% of dry-matter, it is tens times of leaf of Turpinia pomifera (Roxb) D O. or Rutaceae Citrus grandis Osbeck. Var.tomentosa Hort. fruit, in the present invention, Extraction solvent is 95% ethanol, reduce water-soluble substances and enter extracting solution, concentrated solution is extracted with propyl carbinol and sherwood oil gradient mixed solution, obtain purity high product, crystallization and recrystallization in aqueous, obtain the Rhoifoloside of purity more than 98%, and this technical process is simple, be applicable to produce Rhoifoloside in enormous quantities.
Above preferred embodiment of the present invention is described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, the equipment wherein do not described in detail to the greatest extent and structure are construed as to be implemented with the usual manner in this area; Any those of ordinary skill in the art, do not departing under technical solution of the present invention ambit, the Method and Technology content of above-mentioned announcement all can be utilized to make many possible variations and modification to technical solution of the present invention, or being revised as the Equivalent embodiments of equivalent variations, this does not affect flesh and blood of the present invention.Therefore, every content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent variations and modification, all still belongs in the scope of technical solution of the present invention protection.
Claims (6)
1. the method for extraction and isolation Rhoifoloside from Pummelo Peel leaf, is characterized in that, comprise the following steps:
Pummelo Peel leaf is pulverized and filters;
Pummelo Peel leaf powder after filtration is carried out extraction and obtains extracting solution;
Extracting solution is carried out purifying and obtains Rhoifoloside.
2. the method for a kind of extraction and isolation Rhoifoloside from Pummelo Peel leaf as claimed in claim 1, is characterized in that, describedly to be pulverized by Pummelo Peel leaf and in the step of filtering, wherein said being filtered into is filtered by 40 eye mesh screens.
3. the method for a kind of extraction and isolation Rhoifoloside from Pummelo Peel leaf as claimed in claim 2, is characterized in that, describedly Pummelo Peel leaf powder after filtering is carried out extracting the step obtaining extracting solution comprises:
Choose the glass chromatography column that diameter is 2.5cm;
By Pummelo Peel leaf powder with 95% ethanol wet sample upper prop and in post soak 1 hour;
Solution after soaking is collected the elutriant of 6 times amount with 95% ethanol elution;
Elutriant concentrating under reduced pressure is obtained extracting solution.
4. the method for a kind of extraction and isolation Rhoifoloside from Pummelo Peel leaf as claimed in claim 3, is characterized in that, describedly extracting solution is carried out the step that purifying obtains Rhoifoloside and comprises:
Concentrated extracting solution sherwood oil and propyl carbinol mixed solution are extracted repeatedly;
The subnatant of extraction is concentrated;
Lower floor's concentrated solution cold water is divided three times clean and centrifugal segregation water-soluble impurity obtain the thick product of Rhoifoloside;
Thick for Rhoifoloside product is placed in hot water dissolve, puts refrigerator crystallisation by cooling and recrystallization, obtain the Rhoifoloside of purity more than 98%.
5. the method for a kind of extraction and isolation Rhoifoloside from Pummelo Peel leaf as described in as arbitrary in claim 1-4, it is characterized in that, describedly extracting solution is carried out purifying obtain in the step of Rhoifoloside: the extraction agent used in described purifying is sherwood oil and propyl carbinol mixed solution.
6. the method for a kind of extraction and isolation Rhoifoloside from Pummelo Peel leaf as claimed in claim 5, it is characterized in that, the ratio of described sherwood oil and propyl carbinol mixed solution is 8: 2; 6: 4; 4: 6; 2: 8, and the sherwood oil mixed by often kind of proportioning and propyl carbinol mixed solution respectively extract 1 time successively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610028881.7A CN105541941A (en) | 2016-01-07 | 2016-01-07 | Method for extracting and separating rhoifolin from exocarpium leaves |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610028881.7A CN105541941A (en) | 2016-01-07 | 2016-01-07 | Method for extracting and separating rhoifolin from exocarpium leaves |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105541941A true CN105541941A (en) | 2016-05-04 |
Family
ID=55821544
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610028881.7A Pending CN105541941A (en) | 2016-01-07 | 2016-01-07 | Method for extracting and separating rhoifolin from exocarpium leaves |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105541941A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106632546A (en) * | 2016-11-16 | 2017-05-10 | 广东石油化工学院 | Method for preparing two chemical reference substances of Rhoifolin and naringin simultaneously |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1676159A (en) * | 2004-08-26 | 2005-10-05 | 林励 | Total flavone of citrus grandis osbeckvar tomentosa hort peridium, and its extracting method and use |
| CN101279001A (en) * | 2007-04-03 | 2008-10-08 | 化州市绿色生命有限公司 | Pummelo peel extract and preparation method and application thereof |
| CN101906122A (en) * | 2010-08-16 | 2010-12-08 | 江西山香药业有限公司 | Method for extracting rhoifolin and prepared medicament application thereof |
| WO2012022223A1 (en) * | 2010-08-16 | 2012-02-23 | 江西山香药业有限公司 | Composition comprising ligustroflavone, rhoifolin and hyperin, and use thereof in the preparation of a medicament |
| CN102391337A (en) * | 2011-10-10 | 2012-03-28 | 南京泽朗医药科技有限公司 | Method for extracting rhoifolin from turpinia formosana leaves |
| CN102633850A (en) * | 2010-08-16 | 2012-08-15 | 江西山香药业有限公司 | Rhoifolin extraction method and usage of drug prepared by rhoifolin |
-
2016
- 2016-01-07 CN CN201610028881.7A patent/CN105541941A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1676159A (en) * | 2004-08-26 | 2005-10-05 | 林励 | Total flavone of citrus grandis osbeckvar tomentosa hort peridium, and its extracting method and use |
| CN101279001A (en) * | 2007-04-03 | 2008-10-08 | 化州市绿色生命有限公司 | Pummelo peel extract and preparation method and application thereof |
| CN101906122A (en) * | 2010-08-16 | 2010-12-08 | 江西山香药业有限公司 | Method for extracting rhoifolin and prepared medicament application thereof |
| WO2012022223A1 (en) * | 2010-08-16 | 2012-02-23 | 江西山香药业有限公司 | Composition comprising ligustroflavone, rhoifolin and hyperin, and use thereof in the preparation of a medicament |
| CN102633850A (en) * | 2010-08-16 | 2012-08-15 | 江西山香药业有限公司 | Rhoifolin extraction method and usage of drug prepared by rhoifolin |
| CN102391337A (en) * | 2011-10-10 | 2012-03-28 | 南京泽朗医药科技有限公司 | Method for extracting rhoifolin from turpinia formosana leaves |
Non-Patent Citations (3)
| Title |
|---|
| 孔令义: "《天然药物化学 第2版》", 31 August 2015 * |
| 沈彤，等: "《天然药物化学》", 31 July 2010 * |
| 陈健，等: "《食品化学原理》", 28 February 2015 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106632546A (en) * | 2016-11-16 | 2017-05-10 | 广东石油化工学院 | Method for preparing two chemical reference substances of Rhoifolin and naringin simultaneously |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102924240B (en) | Method for extracting total magnolol according to alcoholic-alkaline method | |
| CN104086425A (en) | Method for simultaneously extracting and separating chlorogenic acid, solanesol, alkaloid and rutin in tobacco | |
| CN106220698A (en) | A kind of method of separating high-purity Hesperidin, neohesperidin, naringin and Neosynephrine from Fructus Aurantii Immaturus | |
| CN101463027B (en) | Method for extracting and separating flavone and anthocyanidin from elder fruit | |
| CN111978158A (en) | Method for extracting purified hypocannabidiol from industrial cannabis sativa | |
| CN102106928B (en) | Method for preparing high-purity oil tea saponins | |
| CN107266400B (en) | Method for extracting lactuca sativa bitter principle from chicory | |
| CN102660137B (en) | Method for high-efficiency preparation of natural pigment of Ziziphus jujuba Mill. | |
| CN103601775A (en) | Method for extracting hesperidin from orange peels | |
| CN107098942B (en) | Method for subcritical water extraction of kaempferitrin in radish leaves | |
| CN111072618A (en) | Method for conveniently and rapidly purifying dihydromyricetin from Ampelopsis grossedentata leaves | |
| CN111116323A (en) | Microwave-assisted subcritical technology for extracting cannabidiol and preparation method thereof | |
| CN109021046B (en) | Method for simultaneously extracting quercetin and kaempferitrin from stem and leaf of momordica grosvenori | |
| CN100422205C (en) | Method for preparing oleanolic acid from wrinkled papaya | |
| CN105541941A (en) | Method for extracting and separating rhoifolin from exocarpium leaves | |
| CN108042590A (en) | A kind of residual extract of Radix Ginseng stem and leaf of low agriculture and preparation method thereof | |
| CN107382943B (en) | Method for subcritical water extraction of dihydroquercetin in sorghum bran | |
| CN106905339B (en) | Method for purifying phillygenin from forsythia suspense leaves | |
| CN105712965B (en) | A kind of method that orange peel element and Nobiletin are separated in the extract from tangeritin | |
| CN105254563B (en) | A kind of preparation method of Lotus Leafextract | |
| CN102285954B (en) | Method for extracting epicatechin from red bayberry fruit residues | |
| CN101879265A (en) | Process for co-producing total saponins and polysaccharide from star-of-Bethlehem | |
| CN102391219A (en) | Method for preparing blinin from golden Chinese gentian | |
| CN111763188A (en) | Refining method of nobiletin in immature bitter orange flavone | |
| CN105777922A (en) | Pilose asiabell root polysaccharide extraction method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160504 |