CN106831930B - A kind of extractant and extracting method for ursolic acid extraction - Google Patents
A kind of extractant and extracting method for ursolic acid extraction Download PDFInfo
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- CN106831930B CN106831930B CN201710056292.4A CN201710056292A CN106831930B CN 106831930 B CN106831930 B CN 106831930B CN 201710056292 A CN201710056292 A CN 201710056292A CN 106831930 B CN106831930 B CN 106831930B
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- extractant
- ursolic acid
- feed liquid
- extraction
- raw material
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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
Abstract
The method that the invention discloses a kind of to extract the extractant of ursolic acid from the materials such as common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn and extract ursolic acid, according to parts by weight, constituent and proportion are the extractant：Tween 80 and/or polysorbate60 and/or TritonX-100：0.1-4；Sodium hydroxide 0.01-2；Water is supplemented to 100；PH is 7-14.The extracting method includes raw material crushing, extraction, filtering, polishing purification, concentration, acidification, crystallization etc..Extractant of the invention has the function of significantly improving ursolic acid dissolution rate and hydrophobic contaminants dissolution in raw material, it can keep the original structure and activity of ursolic acid, product purity >=60%, extracting 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, change and active decline that feed liquid heats repeatedly and causes ursolic acid structure are avoided, production cost can be reduced.
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 of the water base extractant and flooding of ursolic acid is extracted in the materials such as leaf, leaves of Hawthorn.
Background technique
Ursolic acid is a kind of faintly acid pentacyclic triterpenoid, has antitumor, anti-oxidant, raising immunity, drop blood
The functions such as rouge, hypoglycemic, antibacterial, anti-inflammatory, antiviral, liver protection and beauty and skin care.The organic solvents such as common ether, ethyl alcohol, methanol
It extracts.Organic solvent soaking extraction method simple process, equipment investment are few, applied widely, but that there are toxicity is big, pollution is tight for organic solvent
The disadvantages of weight, difficult solvent recovery.
Surfactant can reduce solid --- and the interfacial tension of liquid phase increases the dissolution exudation ability of larger molecular organics matter,
Have many advantages, such as to shorten infiltrating time during the extraction process, improve extraction rate.Emulsion method carries out the extraction of ursolic acid, is molten with water
Agent, a small amount of molecules surfactant, which is added, to be implemented, that there are toxicity is big, seriously polluted this method avoid organic solvent,
The disadvantages of difficult solvent recovery, and extraction efficiency is not less than organic solvent extraction, can reduce extraction cost.
Summary of the invention
The first object of the present invention is that provide one kind extracts from the materials such as common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn
The extractant of ursolic acid, has the function of significantly improving and is extracted ursolic acid dissolution rate and hydrophobic contaminants dissolution in raw material.
The second object of the present invention, which is to provide, extracts black bearberry from the materials such as common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn
The method of acid extracts ursolic acid with water soaking method substitution organic solvent, and extraction process is easy, practical, and recovery rate is high, and low energy consumption,
Production cost is reduced, is remained in product without extractant, no pollution to the environment.
The invention is realized by the following technical scheme：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：According to parts by weight, constituent and proportion are：
Tween 80 and/or polysorbate60 and/or TritonX-100：0.1-4；Sodium hydroxide：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, sodium hydroxide 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 commercial product.
A method of extracting ursolic acid 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, the extractant constituent and proportion are calculated by weight as：Polysorbate60 and/
Or Tween 80 and/or TritonX-100：0.1-4；Sodium hydroxide：0.01-2；Water is supplemented to 100；PH is 7- 14；
The 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 that step (1) obtains is fed intake by the ratio between raw material and extractant for 1: 3-30 (w/w) and extracts extraction, leaching
30-100 DEG C of temperature raising degree is handled -20 hours 1 minute, and when extraction extracts, then intermittent stirring raw material leaves and takes feed liquid；
(3) feed liquid for obtaining step (2) filters, and removes 200 mesh impurity below, feed liquid is cooled to 40 DEG C or less；
(4) feed liquid that step (3) obtains is flowed through into resin absorbing column polishing purification, after removal impurity is washed with water, then used
The alcohol flushing resin adsorption column of the 5%-95% of alkalization, obtains ethanol eluate；
(5) by ethanol eluate at 50 DEG C hereinafter, vacuum is concentrated, recycle the solvent, obtain ursolic acid concentration
Liquid；
(6) concentrate for obtaining step (5) is acidified, and black bearberry acid crystal is precipitated.
Further, the ratio between the raw material and extractant are 1: 8-24 (w/w).
Further, the vacuum refers to that vacuum degree is greater than 0.08Mpa.
Further, the acidification refers to is acidified with 1mol/L hydrochloric acid solution.
In the above-mentioned methods, resin absorbing column used in polishing purification is the macroreticular resin to ursolic acid selective absorption
Column.The ethanol eluate is concentrated under vacuum conditions, is finally acidified obtained concentrate, and black bearberry acid crystal is precipitated.
Extractant of the invention, which has to significantly improve, is extracted what ursolic acid dissolution rate and hydrophobic contaminants in raw material dissolved out
Function can keep the original structure and activity of ursolic acid, and dosage 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 to avoid than the process that organic solvent extractionprocess reduces recycling design
Feed liquid heats repeatedly and causes the change and active decline of ursolic acid structure, and compared with organic solvent extractionprocess, can
Reduce production cost.
Specific embodiment
The ingredient and proportion (according to parts by weight) TritonX-100 of 1 extractant of embodiment：1.4；Tween 80：0.8；
Sodium hydroxide：0.2；Water：97.6.
Extraction step：
The common rabdosia leaf 100kg that crushed 20 mesh is put into extractor, extractant 800kg, covered and enclosed, extraction temperature is added
It is 70 DEG C, pressure：Normal pressure；Stirring and leaching 3 hours, wherein per half an hour intermittent stirring 2-5 minutes.Feed liquid filter centrifugal is thick
The following impurity of 20 mesh is filtered out, sand filtration machine refined filtration goes out the following impurity of 200 mesh, and is cooled to 40 DEG C.Feed liquid was flowed with 500kg/ hours
Amount flows through resin absorbing column, and the impurity not being adsorbed then is washed with water down, the alcohol flushing resin adsorption column for being 85% with content,
Ethanol eluate is obtained, is concentrated in vacuo at 45 DEG C of temperature, vacuum degree 0.08Mpa, ethanol eluate is concentrated original ten/
One, acidification, black bearberry acid crystal is precipitated, and obtains 0.136kg black bearberry acid product, purity reaches 65% or so.
The ingredient and proportion (according to parts by weight) TritonX-100 of 2 extractant of embodiment：1.8；Sodium hydroxide：0.24；
Water：98.
Extraction step：
The fruit of glossy privet 80kg that crushed 20 mesh is put into extractor, extractant 1600kg, covered and enclosed, extraction temperature is added
It is 70 DEG C, pressure：Normal pressure；Stirring and leaching 3 hours, wherein per half an hour intermittent stirring 2-5 minutes.Feed liquid filter centrifugal is thick
The following impurity of 20 mesh is filtered out, sand filtration machine refined filtration goes out the following impurity of 200 mesh, and is cooled to 40 DEG C.Still using the resin in embodiment 1
Purifying, ethanol elution, concentration, acidification, obtains 0.217kg ursolic acid, purity reaches 65% or so.
The ingredient and proportion (according to parts by weight) Tween 80 of 3 extractant of embodiment：0.6；Polysorbate60：0.8；
TritonX-100：1.2；Sodium hydroxide：0.22；Water：97.2.
Extraction step：
The leaves of Hawthorn 100kg that crushed 20 mesh is put into extractor, extractant 2400kg, covered and enclosed, extraction temperature is added
Degree is 70 DEG C, pressure：Normal pressure；Stirring and leaching 4 hours, wherein per half an hour intermittent stirring 2-5 minutes.Feed liquid filter centrifugal
Coarse filtration goes out the following impurity of 20 mesh, and sand filtration machine refined filtration goes out the following impurity of 200 mesh, and is cooled to 40 DEG C.Still using the tree in embodiment 1
Rouge purifying, ethanol elution, concentration, acidification obtain 0.29kg ursolic acid, purity reaches 65% or so.
Claims (6)
1. a kind of extractant for extracting ursolic acid from common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn material, it is characterised in that：It presses
Parts by weight meter, constituent and proportion are：Tween 80 and/or polysorbate60 and/or TritonX-100：0.1-4；Sodium hydroxide：
0.01-2；Water is supplemented to 100；PH is 7-14.
2. a kind of method for extracting ursolic acid from common rabdosia leaf, the fruit of glossy privet, loguat leaf, leaves of Hawthorn material, it is characterised in that：It utilizes
Extractant uses water logging extracting method, and the extractant constituent and proportion are calculated by weight as：It polysorbate60 and/or spits
80 and/or TritonX-100 of temperature：0.1-4；Sodium hydroxide：0.01-2；Water is supplemented to 100；PH is 7- 14；
The 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 that step (1) obtains is fed intake by the ratio between raw material and extractant for 1: 3-30 (w/w) and extracts extraction, extraction temperature
30-100 DEG C of degree is handled -20 hours 1 minute, and when extraction extracts, then intermittent stirring raw material leaves and takes feed liquid；
(3) feed liquid for obtaining step (2) filters, and removes 200 mesh impurity below, feed liquid is cooled to 40 DEG C or less；
(4) feed liquid that step (3) obtains is flowed through into resin absorbing column polishing purification, be washed with water removal impurity after, then with alkalize
5%-95% alcohol flushing resin adsorption column, obtain ethanol eluate；
(5) by ethanol eluate at 50 DEG C hereinafter, vacuum is concentrated, recycle the solvent, obtain ursolic acid concentrate；
(6) concentrate for obtaining step (5) is acidified, and black bearberry acid crystal is precipitated.
3. method according to claim 2, it is characterised in that：The ratio between raw material and extractant described in step (2) are 1: 8-24
(w/w)。
4. method according to claim 2, it is characterised in that：Adsorption column used in step (4) polishing purification is to black bearberry
The macroporous resin column of sour selective absorption.
5. method according to claim 2, it is characterised in that：Vacuum described in step (5) refers to that vacuum degree is greater than
0.08Mpa。
6. method according to claim 2, it is characterised in that：Acidification described in step (6) refers to 1mol/L hydrochloric acid solution
Acidification.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022225823A1 (en) * | 2021-04-19 | 2022-10-27 | Life Technologies Corporation | Decontaminant |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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- 2017-01-25 CN CN201710056292.4A patent/CN106831930B/en active Active
Non-Patent Citations (3)
| Title |
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| 熊果酸提取分离方法研究进展;韩嫒嫒等;《中国医药指南》;20121231;第10卷(第35期);第433-435页 * |
| 熊果酸提取工艺的研究进展;于明明等;《氨基酸和生物资源》;20091231;第31卷(第1期);第33-36，39页 * |
| 熊果酸的提取、分离及分析方法的;孟煜嘉等;《机电信息》;20160115(第2期);第45-51页 * |
Cited By (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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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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