CN106565803A - Extraction process for oleuropein - Google Patents
Extraction process for oleuropein Download PDFInfo
- Publication number
- CN106565803A CN106565803A CN201610886517.4A CN201610886517A CN106565803A CN 106565803 A CN106565803 A CN 106565803A CN 201610886517 A CN201610886517 A CN 201610886517A CN 106565803 A CN106565803 A CN 106565803A
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- cleupin
- extraction process
- extraction
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- 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
-
- 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
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Medicines Containing Plant Substances (AREA)
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Abstract
The invention discloses an extraction process for oleuropein, belonging to the technical field of separation and extraction of effective components of natural products. The extraction process comprises the following steps: crushing olive leaves into coarse powder, carrying out sieving with a 30-to-40-mesh sieve, carrying out percolation extraction by utilizing ethyl alcohol with a concentration of 80%, subjecting an extracting solution to adsorption through macroporous resin D101, then carrying out elution through ethyl alcohol with a concentration of 65%, concentrating an eluent, then carrying out repeated extraction by utilizing ethyl acetate for 3 to 4 times, and subjecting an ethyl acetate layer solution to concentration and drying so as to prepare the oleuropein with a content of 80 to 88%. The extraction process for the oleuropein disclosed by the invention has the following advantages: used raw materials are low in cost; the process of extraction is simple; the oleuropein with high yield and high purity can be prepared; and the utilization rate of the raw materials is greatly improved.
Description
The invention belongs to the separation and extraction technology field of natural product active ingredient, and in particular to a kind of cleupin is carried
Taking technique.
【Background technology】
The features such as Fructus Canarii albi has high medical value, rich in nutrition content, is the precious medicine-food two-purpose resource of China.Folium olive
In the substantial amounts of cleupin active component that contains, the antibacterium with strength and ntiviral characteristic and extremely strong antioxidation energy
Power, the development and skin care item manufacture view in terms of the new drugs such as anti-bacteria and anti-virus played an important role.In recent years, Fructus Canarii albi kind
Area expanding day is planted, and Folium olive is not utilized substantially, just accumulation generates substantial amounts of Fructus Canarii albi fallen leaves garbage, makes
Into the waste and environmental pollution of resource.It is various from Folium olive with the continuous innovation application of Folium olive hardship glycoside extractive technique
The new method of separation and Extraction Fructus Canarii albi bitter sweet product, new technology emerge in an endless stream, it is intended to improve the yield and purity of Fructus Canarii albi bitter sweet, realize
The effectively utilizes of discarded Folium olive, reach the purpose for turning waste into wealth, and promote company's industrialized production Folium olive hardship glycoside product, improve
Economic benefit, social benefit and environmental benefit.
【The content of the invention】
The extraction process of a kind of cleupin that the present invention is provided, to solve the current Folium olive wasting of resources and environmental pollution
The problems such as, the effectively utilizes of discarded Folium olive are realized, reach the purpose for turning waste into wealth.The extraction process of the present invention, using percolation
The methods such as method extraction, macroporous resin adsorption, ethyl acetate extraction, separation and Extraction process is simple, and raw materials used low cost can be prepared
The cleupin of various different demands component contents, not only product yield is high, purity is high, moreover it is possible to realize the industrialization of cleupin
Production.
To solve above technical problem, the present invention adopts following technical method：
A kind of extraction process of cleupin, comprises the following steps：
S1：It is coarse powder shape that Folium olive is crushed, and 30-40 mesh sieves is crossed, by 1:Ethanol closed of 1 weight than addition 80%
Swollen 1-3h, by the alcohol solvent that the Fructus Canarii albi leaf coarse powder for fully having expanded adds 80% seepage pressure effects are carried out, and extracting solution is obtained；
S2：By the extracting solution in step S1 by D101 macroporous resin adsorption, the ethanol elution of Jing 60%, eluting is obtained
Liquid；
S3：After by the eluent concentration in step S2, extracted 3-4 time repeatedly using the ethyl acetate of equivalent, by acetic acid second
Ester layer liquid carries out concentrate drying, and in the case where temperature is for 55-65 DEG C 2-3h is dried, and the cleupin of 80-88% is obtained.
Preferably, Folium olive submergence all the time in a solvent, impregnates before percolate outflow during seepage pressure effects described in step S1
Folium olive 24-32h.
It is highly preferred that the flow velocity of the percolate is 1-3mL/min.
Preferably, extracting solution described in step S1 is obtained the Fructus Canarii albi hardship of 16-22% by concentrating, settling, separate, be dried
Glycoside.
It is highly preferred that the temperature of the drying be 55-65 DEG C, when a length of 2-3h.
Preferably, the flow velocity of ethanol elution described in step S2 is 2-3BV/h, a length of 15-30min during eluting.
Preferably, the concentration of eluent described in step S2, dry, the cleupin of prepared 50-58%.
It is highly preferred that the temperature of the drying be 55-65 DEG C, when a length of 2-3h.
The invention has the advantages that：
(1) cleupin extraction process operating process of the invention is simple, raw materials used low cost；
(2) extraction process that the present invention is provided is isolated and purified using macroporous adsorbent resin, to improve obtaining for extract
Rate and purity, realize the high-recovery and high-purity of cleupin product；
(3) process provided by the present invention can prepare the cleupin product of various different demands component contents, easily
In the industrialization production for realizing cleupin.
【Specific embodiment】
It is specifically described with reference to specific embodiment.
Embodiment 1
S1：It is coarse powder shape that Folium olive is crushed, and 30 mesh sieves is crossed, by 1:Than adding, 80% ethanol is closed to swell 1 weight
1h, the Fructus Canarii albi leaf coarse powder for fully having expanded is fitted in percolation bucket, and uniform compaction, the alcohol solvent for plus 80% carries out percolation and carries
Take.When carrying out seepage pressure effects, should constantly add solvent makes the submergence all the time of Fructus Canarii albi leaf coarse powder in a solvent, and before percolate flows out
Dipping coarse powder 24h.When percolate flows out, the rate of outflow should be controlled in 1mL/min；It is intended to the 75% of preparation amount and oozes when collects
Filter liquid when, stop percolation, squeezing medicinal residues simultaneously merge pressed liquor with percolate, the required extracting solution of acquisition.Extracting solution is by dense
Contracting, sedimentation, is put into centrifugation in the centrifuge of 1000r/min, and gained centrifugal liquid is dried 2h at 60 DEG C, Fructus Canarii albi is obtained bitter
Glycoside.Jing chromatographs detect that the content of cleupin is 18% in product；
S2：By the extracting solution obtained by step S1 after D101 macroporous resin adsorption, eluting is carried out using 60% ethanol,
Elution flow rate is 2BV/h, when a length of 30min, after eluting is complete, then eluent is concentrated, gained concentrated solution at 60 DEG C be dried
2h, is obtained cleupin.Jing chromatographs detect that the content of cleupin is 51% in product；
S3：After by the eluent concentration in step S2, extracted repeatedly 3 times using the ethyl acetate of equivalent, take ethyl acetate
Layer liquid is concentrated, and is dried 2h at 60 DEG C, and cleupin is obtained.The detection of Jing chromatographs, the content of cleupin in product
For 82%.
Embodiment 2
S1：It is coarse powder shape that Folium olive is crushed, and 40 mesh sieves is crossed, by 1:Than adding, 80% ethanol is closed to swell 1 weight
2h, the Fructus Canarii albi leaf coarse powder for fully having expanded is fitted in percolation bucket, and uniform compaction, the alcohol solvent for plus 80% carries out percolation and carries
Take.When carrying out seepage pressure effects, should constantly add solvent makes the submergence all the time of Fructus Canarii albi leaf coarse powder in a solvent, and before percolate flows out
Dipping coarse powder 28h.When percolate flows out, the rate of outflow should be controlled in 2mL/min；It is intended to the 75% of preparation amount and oozes when collects
Filter liquid when, stop percolation, squeezing medicinal residues simultaneously merge pressed liquor with percolate, the required extracting solution of acquisition.Extracting solution is by dense
Contracting, sedimentation, is put into centrifugation in the centrifuge of 1000r/min, and gained centrifugal liquid is dried 3h at 62 DEG C, Fructus Canarii albi is obtained bitter
Glycoside.Jing chromatographs detect that the content of cleupin is 19% in product；
S2：By the extracting solution obtained by step S1 after D101 macroporous resin adsorption, eluting is carried out using 60% ethanol,
Elution flow rate is 3BV/h, when a length of 25min, after eluting is complete, then eluent is concentrated, gained concentrated solution at 62 DEG C be dried
3h, is obtained cleupin.Jing chromatographs detect that the content of cleupin is 53% in product；
S3：After by the eluent concentration in step S2, extracted repeatedly 4 times using the ethyl acetate of equivalent, take ethyl acetate
Layer liquid is concentrated, and is dried 3h at 62 DEG C, and cleupin is obtained.The detection of Jing chromatographs, the content of cleupin in product
For 81%.
Embodiment 3
S1：It is coarse powder shape that Folium olive is crushed, and 40 mesh sieves is crossed, by 1:Than adding, 80% ethanol is closed to swell 1 weight
3h, the Fructus Canarii albi leaf coarse powder for fully having expanded is fitted in percolation bucket, and uniform compaction, the alcohol solvent for plus 80% carries out percolation and carries
Take.When carrying out seepage pressure effects, should constantly add solvent makes the submergence all the time of Fructus Canarii albi leaf coarse powder in a solvent, and before percolate flows out
Dipping coarse powder 32h.When percolate flows out, the rate of outflow should be controlled in 3mL/min；It is intended to the 75% of preparation amount and oozes when collects
Filter liquid when, stop percolation, squeezing medicinal residues simultaneously merge pressed liquor with percolate, the required extracting solution of acquisition.Extracting solution is by dense
Contracting, sedimentation, is put into centrifugation in the centrifuge of 1000r/min, and gained centrifugal liquid is dried 2h at 65 DEG C, Fructus Canarii albi is obtained bitter
Glycoside.Jing chromatographs detect that the content of cleupin is 17% in product；
S2：By the extracting solution obtained by step S1 after D101 macroporous resin adsorption, eluting is carried out using 60% ethanol,
Elution flow rate is 3BV/h, when a length of 15min, after eluting is complete, then eluent is concentrated, gained concentrated solution at 65 DEG C be dried
2h, is obtained cleupin.Jing chromatographs detect that the content of cleupin is 50% in product；
S3：After by the eluent concentration in step S2, extracted repeatedly 4 times using the ethyl acetate of equivalent, take ethyl acetate
Layer liquid is concentrated, and is dried 2h at 65 DEG C, and cleupin is obtained.The detection of Jing chromatographs, the content of cleupin in product
For 81%.
Embodiment 4
S1：It is coarse powder shape that Folium olive is crushed, and 30 mesh sieves is crossed, by 1:Than adding, 80% ethanol is closed to swell 1 weight
3h, the Fructus Canarii albi leaf coarse powder for fully having expanded is fitted in percolation bucket, and uniform compaction, the alcohol solvent for plus 80% carries out percolation and carries
Take.When carrying out seepage pressure effects, should constantly add solvent makes the submergence all the time of Fructus Canarii albi leaf coarse powder in a solvent, and before percolate flows out
Dipping coarse powder 32h.When percolate flows out, the rate of outflow should be controlled in 2mL/min；It is intended to the 75% of preparation amount and oozes when collects
Filter liquid when, stop percolation, squeezing medicinal residues simultaneously merge pressed liquor with percolate, the required extracting solution of acquisition.Extracting solution is by dense
Contracting, sedimentation, is put into centrifugation in the centrifuge of 1000r/min, and gained centrifugal liquid is dried 2h at 65 DEG C, Fructus Canarii albi is obtained bitter
Glycoside.Jing chromatographs detect that the content of cleupin is 18% in product；
S2：By the extracting solution obtained by step S1 after D101 macroporous resin adsorption, eluting is carried out using 60% ethanol,
Elution flow rate is 3BV/h, when a length of 25min, after eluting is complete, then eluent is concentrated, gained concentrated solution at 63 DEG C be dried
3h, is obtained cleupin.Jing chromatographs detect that the content of cleupin is 56% in product；
S3：After by the eluent concentration in step S2, extracted repeatedly 4 times using the ethyl acetate of equivalent, take ethyl acetate
Layer liquid is concentrated, and is dried 2h at 65 DEG C, and cleupin is obtained.The detection of Jing chromatographs, the content of cleupin in product
For 84%.
Above content is to combine specific preferred implementation further description made for the present invention, it is impossible to assert
The present invention be embodied as be confined to these explanation, for person of an ordinary skill in the technical field, without departing from
On the premise of present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention by being submitted to
Claims determine scope of patent protection.
Claims (8)
1. a kind of extraction process of cleupin, it is characterised in that comprise the following steps：
S1：It is coarse powder shape that Folium olive is crushed, and 30-40 mesh sieves is crossed, by 1:1 weight swell 1- more closed than the ethanol of addition 80%
3h, by the alcohol solvent that the Fructus Canarii albi leaf coarse powder for fully having expanded adds 80% seepage pressure effects are carried out, and extracting solution is obtained；
S2：By the extracting solution in step S1 by D101 macroporous resin adsorption, the ethanol elution of Jing 60%, eluent is obtained；
S3：After by the eluent concentration in step S2, extracted 3-4 time repeatedly using the ethyl acetate of equivalent, by ethyl acetate layer
Liquid carries out concentrate drying, and in the case where temperature is for 55-65 DEG C 2-3h is dried, and the cleupin of 80-88% is obtained.
2. the extraction process of cleupin according to claim 1, it is characterised in that：Described in step S1 during seepage pressure effects
, it is ensured that Folium olive submergence all the time is in a solvent, percolate should impregnate Folium olive 24-32h before flowing out.
3. the extraction process of cleupin according to claim 2, it is characterised in that：The flow velocity of the percolate is 1-
3mL/min。
4. the extraction process of cleupin according to claim 1, it is characterised in that：Extracting solution passes through described in step S1
Concentration, sedimentation, separation, dry, the cleupin of prepared 16-22%.
5. the extraction process of cleupin according to claim 4, it is characterised in that：The temperature of the drying is 55-65
DEG C, when a length of 2-3h.
6. the extraction process of cleupin according to claim 1, it is characterised in that：Ethanol elution described in step S2
Flow velocity is 2-3BV/h, a length of 15-30min during eluting.
7. the extraction process of cleupin according to claim 1, it is characterised in that：Eluent passes through described in step S2
Concentration, dry, the cleupin of prepared 50-58%.
8. the extraction process of cleupin according to claim 7, it is characterised in that：The temperature of the drying is 55-65
DEG C, when a length of 2-3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610886517.4A CN106565803A (en) | 2016-10-10 | 2016-10-10 | Extraction process for oleuropein |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610886517.4A CN106565803A (en) | 2016-10-10 | 2016-10-10 | Extraction process for oleuropein |
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| CN106565803A true CN106565803A (en) | 2017-04-19 |
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ID=58532738
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| CN201610886517.4A Pending CN106565803A (en) | 2016-10-10 | 2016-10-10 | Extraction process for oleuropein |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109021042A (en) * | 2018-09-13 | 2018-12-18 | 四川奇格曼药业有限公司 | A method of extracting high-purity oleuropein from olive growing leaves |
| CN109125182A (en) * | 2018-10-16 | 2019-01-04 | 阿谷巴科技（唐山）有限公司 | A kind of Cleupin cold cream and preparation method thereof with bacteriostasis |
| EP3818837A1 (en) | 2019-11-07 | 2021-05-12 | Michel Rumiz | Method for reducing the concentration of oleuropein and for formation and preservation of the concentration of hydroxytyrosol and tyrosol in olives |
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| CN102228514A (en) * | 2011-05-05 | 2011-11-02 | 陕西禾博天然产物有限公司 | Method for extracting oleuropein from olive leaves |
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| CN102731592A (en) * | 2012-06-25 | 2012-10-17 | 向华 | Method for extracting cleupin and amentoflavone from olive leaf |
| CN102850416A (en) * | 2012-09-07 | 2013-01-02 | 中国林业科学研究院林产化学工业研究所 | Method and apparatus used for preparing olive leaf extract |
| CN103333213A (en) * | 2013-07-24 | 2013-10-02 | 桂林茗兴生物科技有限公司 | Method for extracting oleuropein from olive leaves |
| CN104311613A (en) * | 2014-09-30 | 2015-01-28 | 桂林三宝药业有限公司 | Method for extracting oleuropein from olive leaves |
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| CN102451235A (en) * | 2010-10-27 | 2012-05-16 | 深圳劲创生物技术有限公司 | Preparation method of olive leaf extract |
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| CN102731592A (en) * | 2012-06-25 | 2012-10-17 | 向华 | Method for extracting cleupin and amentoflavone from olive leaf |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109021042A (en) * | 2018-09-13 | 2018-12-18 | 四川奇格曼药业有限公司 | A method of extracting high-purity oleuropein from olive growing leaves |
| CN109021042B (en) * | 2018-09-13 | 2022-04-12 | 四川奇格曼药业有限公司 | Method for extracting high-purity oleuropein from olive leaves |
| CN109125182A (en) * | 2018-10-16 | 2019-01-04 | 阿谷巴科技（唐山）有限公司 | A kind of Cleupin cold cream and preparation method thereof with bacteriostasis |
| EP3818837A1 (en) | 2019-11-07 | 2021-05-12 | Michel Rumiz | Method for reducing the concentration of oleuropein and for formation and preservation of the concentration of hydroxytyrosol and tyrosol in olives |
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