CN106831930A - A kind of extractant extracted for ursolic acid and extracting method - Google Patents
A kind of extractant extracted for ursolic acid and extracting method Download PDFInfo
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- CN106831930A CN106831930A CN201710056292.4A CN201710056292A CN106831930A CN 106831930 A CN106831930 A CN 106831930A CN 201710056292 A CN201710056292 A CN 201710056292A CN 106831930 A CN106831930 A CN 106831930A
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- extractant
- ursolic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
- C07J63/008—Expansion of ring D by one atom, e.g. D homo steroids
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Abstract
The invention discloses a kind of extractant that ursolic acid is extracted from the materials such as common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn and the method for extracting ursolic acid, described extractant is counted by weight, and constituent and proportioning are：Tween 80 and/or polysorbate60 and/or TritonX 100：0.1‑4；NaOH 0.01 2；Water is supplemented to 100；PH is 7 14.Described extracting method includes raw material crushing, extraction, filtering, polishing purification, concentration, acidifying, crystallization etc..Extractant of the invention have significantly improve ursolic acid dissolution rate and the function of hydrophobic contaminants dissolution in raw material, the original structure and activity of ursolic acid can be kept, product purity >=60%, extract feed liquid only can need to directly go up resin absorbing column polishing purification by filtering, than the process that organic solvent extractionprocess reduces recycling design, avoid feed liquid to heat repeatedly and cause the change of ursolic acid structure and the decline of activity, it is possible to decrease production cost.
Description
Technical field
The invention belongs to technical field of natural product extraction, and in particular to one kind is used for from common rabdosia leaf, the fruit of glossy privet, loquat
The method that the water base extractant and flooding of ursolic acid are extracted in the materials such as leaf, leaves of Hawthorn.
Background technology
Ursolic acid is a kind of faintly acid pentacyclic triterpenoid, with antitumor, anti-oxidant, enhance immunity, drop blood
The functions such as fat, hypoglycemic, antibacterial, anti-inflammatory, antiviral, liver protection and beauty and skin care.The organic solvents such as conventional ether, ethanol, methyl alcohol
Extract.Organic solvent soaking extraction method process is simple, equipment investment are few, applied widely, but organic solvent is present, and toxicity is big, pollute tight
The shortcomings of weight, difficult solvent recovery.
Surfactant can reduce solid --- and ability is oozed out in the interfacial tension of liquid phase, the dissolving for increasing larger molecular organics matter,
Have the advantages that to shorten infiltrating time in extraction process, improve extraction rate.Emulsion method carries out the extraction of ursolic acid, with water as molten
Agent, adds a small amount of molecules surfactant just can implement, this method avoid organic solvent exist toxicity it is big, seriously polluted,
The shortcomings of difficult solvent recovery, and extraction efficiency is not less than organic solvent extraction, can reduce extraction cost.
The content of the invention
The first object of the present invention is to provide one kind to be extracted from the materials such as common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn
The extractant of ursolic acid, ursolic acid dissolution rate and the function of hydrophobic contaminants dissolution in raw material are extracted with significantly improving.
The second object of the present invention is to provide to extract black bearberry from the materials such as common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn
The method of acid, Solvent Extract methods ursolic acid is substituted with water soaking method, and extraction process is easy, practical, and recovery rate is high, and energy consumption is low,
Production cost is reduced, is remained without extractant in product, it is environmentally safe.
The present invention is achieved through the following technical solutions：One kind is used for from materials such as common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn
The extractant of ursolic acid is extracted in material, it is characterised in that：Count by weight, constituent and proportioning are：
Tween 80 and/or polysorbate60 and/or TritonX-100：0.1-4；NaOH：0.01-2；Water is supplemented to 100；PH is
7-14。
The preparation method of above-mentioned extractant：Tween 80 and/or polysorbate60 and/or TritonX-100, NaOH are pressed into institute
Requirement is dissolved in gauge water.
The material is common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn etc..
The said goods are commercially available prod.
In being embodied at one, described polysorbate60：0.1-4；Tween 80：0.1-4；TritonX-100：0.1-4；Hydrogen
Sodium oxide molybdena：0.01-2；Water is supplemented to 100；PH is 7-14.
A kind of method that ursolic acid is extracted from the materials such as common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn, it is characterised in that
Water logging extracting method is used using extractant, described extractant constituent and proportioning are calculated by weight as：Polysorbate60 and/
Or Tween 80 and/or TritonX-100：0.1-4；NaOH：0.01-2；Water is supplemented to 100；PH is 7--14；
Described extraction step is：
(1) material disintegratings such as dry common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn are crossed into 10-60 mesh；
(2) raw material for obtaining step (1) extracts extraction, extraction temperature for 1: 3-30 (w/w) feeds intake by the ratio between raw material and extractant
30-100 DEG C of degree, is processed -20 hours 1 minute, and during extraction extraction, then intermittent stirring raw material leaves and takes feed liquid；
(3) the feed liquid filtering for obtaining step (2), the impurity gone below 200 mesh, feed liquid is cooled to less than 40 DEG C；
(4) feed liquid that step (3) is obtained is flowed through into resin absorbing column polishing purification, after washing the removal of impurity with water, then with alkalization
5%-95% alcohol flushing resin adsorption column, obtain ethanol eluate；
(5) by ethanol eluate below 50 DEG C, vacuum is concentrated, and reclaims the solvent, obtains ursolic acid concentrate；
(6) the concentrate acidifying for obtaining step (5), black bearberry acid crystal is separated out.
Further, the ratio between described raw material and extractant are 1: 8-24 (w/w).
Further, described vacuum refers to that vacuum is more than 0.08Mpa.
Further, described acidifying refers to be acidified with 1mol/L hydrochloric acid solutions.
In the above-mentioned methods, the resin absorbing column that polishing purification is used is the macroreticular resin to ursolic acid selective absorption
Post.Described ethanol eluate is concentrated under vacuum, and the concentrate acidifying that will finally obtain, black bearberry acid crystal is separated out.
Extractant of the invention has to significantly improve and is extracted ursolic acid dissolution rate and hydrophobic contaminants dissolution in raw material
Function, can keep the original structure and activity of ursolic acid, and consumption is small, extraction yield is high, product purity >=60%, and extracting feed liquid only needs
Resin absorbing column polishing purification can be directly gone up by filtering, than the process that organic solvent extractionprocess reduces recycling design, it is to avoid
Feed liquid is heated and causes the change of ursolic acid structure and the decline of activity repeatedly, and is compared with organic solvent extractionprocess, can
Reduce production cost.
Specific embodiment
Embodiment 1
Composition and proportioning (counting by weight) TritonX-100 of extractant：1.4；Tween 80：0.8；NaOH：0.2；
Water：97.6.
Extraction step：
The common rabdosia leaf 100kg input extractors of 20 mesh will be crushed, extractant 800kg was added, covered and enclosed, extraction temperature was 70
DEG C, pressure：Normal pressure；Stirring and leaching 3 hours, wherein per intermittent stirring 2-5 minutes half an hour.Feed liquid filter centrifugal coarse filtration goes out
The following impurity of 20 mesh, sand filtration machine refined filtration goes out the following impurity of 200 mesh, and is cooled to 40 DEG C.By feed liquid with 500kg/ hours traffic flow
Resin absorbing column is crossed, not adsorbed impurity is then washed down with water, with the alcohol flushing resin adsorption column that content is 85%, obtained
Ethanol eluate, is concentrated in vacuo under 45 DEG C of temperature, vacuum 0.08Mpa, and ethanol eluate is concentrated into original 1/10th, acid
Change, black bearberry acid crystal is separated out, and obtains 0.136kg black bearberry acid products, and its purity reaches 65% or so.
Embodiment 2
Composition and proportioning (counting by weight) TritonX-100 of extractant：1.8；NaOH：0.24；Water：98.
Extraction step：
The fruit of glossy privet 80kg input extractors of 20 mesh will be crushed, extractant 1600kg was added, covered and enclosed, extraction temperature was 70
DEG C, pressure：Normal pressure；Stirring and leaching 3 hours, wherein per intermittent stirring 2-5 minutes half an hour.Feed liquid filter centrifugal coarse filtration goes out
The following impurity of 20 mesh, sand filtration machine refined filtration goes out the following impurity of 200 mesh, and is cooled to 40 DEG C.It is still pure using the resin in embodiment 1
Change, the step such as ethanol elution, concentration, acidifying obtains 0.217kg ursolic acid, and its purity reaches 65% or so.
Embodiment 3
Composition and proportioning (counting by weight) Tween 80 of extractant：0.6；Polysorbate60：0.8；TritonX-100：1.2；
NaOH：0.22；Water：97.2.
Extraction step：
The leaves of Hawthorn 100kg input extractors of 20 mesh will be crushed, extractant 2400kg was added, covered and enclosed, extraction temperature is
70 DEG C, pressure：Normal pressure；Stirring and leaching 4 hours, wherein per intermittent stirring 2-5 minutes half an hour.Feed liquid filter centrifugal coarse filtration
Go out the following impurity of 20 mesh, sand filtration machine refined filtration goes out the following impurity of 200 mesh, and is cooled to 40 DEG C.It is still pure using the resin in embodiment 1
Change, the step such as ethanol elution, concentration, acidifying obtains 0.29kg ursolic acid, and its purity reaches 65% or so.
Claims (7)
1. it is a kind of from common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn material extract ursolic acid extractant, it is characterised in that：Press
Parts by weight meter, constituent and proportioning are：Tween 80 and/or polysorbate60 and/or TritonX-100：0.1-4；NaOH：
0.01-2；Water is supplemented to 100；PH is 7-14.
2. extractant as claimed in claim 1, it is characterised in that：Count by weight, described polysorbate60：0.1-4；Tween
80：0.1-4；TritonX-100：0.1-4；NaOH：0.01-2；Water is supplemented to 100；PH is 7-14.
3. it is a kind of from common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn material extract ursolic acid method, it is characterised in that：Utilize
Extractant uses water logging extracting method, and described extractant constituent and proportioning are calculated by weight as：Polysorbate60 and/or tell
80 and/or TritonX-100 of temperature：0.1-4；NaOH：0.01-2；Water is supplemented to 100；PH is 7--14；
Described extraction step is：
(1) dry common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn material disintegrating are crossed into 10-60 mesh；
(2) raw material for obtaining step (1) extracts extraction, extraction temperature for 1: 3-30 (w/w) feeds intake by the ratio between raw material and extractant
30-100 DEG C of degree, is processed -20 hours 1 minute, and during extraction extraction, then intermittent stirring raw material leaves and takes feed liquid；
(3) the feed liquid filtering for obtaining step (2), the impurity gone below 200 mesh, feed liquid is cooled to less than 40 DEG C；
(4) feed liquid that step (3) is obtained is flowed through into resin absorbing column polishing purification, after washing the removal of impurity with water, then with alkalization
5%-95% alcohol flushing resin adsorption column, obtain ethanol eluate；
(5) by ethanol eluate below 50 DEG C, vacuum is concentrated, and reclaims the solvent, obtains ursolic acid concentrate；
(6) the concentrate acidifying for obtaining step (5), black bearberry acid crystal is separated out.
4. method as claimed in claim 3, it is characterised in that：The ratio between raw material and extractant described in step (2) are 1: 8-24
(w/w)。
5. method as claimed in claim 3, it is characterised in that：The adsorption column that step (4) polishing purification is used is to black bearberry
The macroporous resin column of sour selective absorption.
6. method as claimed in claim 3, it is characterised in that：Vacuum described in step (5) refers to that vacuum is more than
0.08Mpa。
7. method as claimed in claim 3, it is characterised in that：Acidifying described in step (6) refers to use 1mol/L hydrochloric acid solutions
Acidifying.
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| CN201710056292.4A CN106831930B (en) | 2017-01-25 | 2017-01-25 | A kind of extractant and extracting method for ursolic acid extraction |
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| CN201710056292.4A CN106831930B (en) | 2017-01-25 | 2017-01-25 | A kind of extractant and extracting method for ursolic acid extraction |
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| CN106831930A true CN106831930A (en) | 2017-06-13 |
| CN106831930B CN106831930B (en) | 2018-11-20 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108997469A (en) * | 2018-08-28 | 2018-12-14 | 西北大学 | A kind of jujube root extract, extraction separation method and its application |
| CN112409440A (en) * | 2021-01-04 | 2021-02-26 | 湖南德诺健康管理集团有限公司 | Method for producing ursolic acid emulsion by using rosemary ointment as raw material |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022225823A1 (en) * | 2021-04-19 | 2022-10-27 | Life Technologies Corporation | Decontaminant |
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2017
- 2017-01-25 CN CN201710056292.4A patent/CN106831930B/en active Active
Non-Patent Citations (3)
| Title |
|---|
| 于明明等: "熊果酸提取工艺的研究进展", 《氨基酸和生物资源》 * |
| 孟煜嘉等: "熊果酸的提取、分离及分析方法的", 《机电信息》 * |
| 韩嫒嫒等: "熊果酸提取分离方法研究进展", 《中国医药指南》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108997469A (en) * | 2018-08-28 | 2018-12-14 | 西北大学 | A kind of jujube root extract, extraction separation method and its application |
| CN108997469B (en) * | 2018-08-28 | 2021-07-13 | 西北大学 | Jujube root extract, extraction and separation method and application thereof |
| CN112409440A (en) * | 2021-01-04 | 2021-02-26 | 湖南德诺健康管理集团有限公司 | Method for producing ursolic acid emulsion by using rosemary ointment as raw material |
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| CN106831930B (en) | 2018-11-20 |
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Effective date of registration: 20221031 Address after: Room 716, Floor 7, No. 180, Huashen Road, Free Trade Pilot Zone, Pudong New Area, Shanghai, 200000 Patentee after: Shanghai Jiujiantang Food Technology Co.,Ltd. Address before: 235000 Dongshan Road 100, Xiangshan District, Huaibei, Anhui Patentee before: HUAIBEI NORMAL University |
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