CN106188213B - A kind of Simple Purification method of Tea Saponin - Google Patents
A kind of Simple Purification method of Tea Saponin Download PDFInfo
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- CN106188213B CN106188213B CN201610570369.5A CN201610570369A CN106188213B CN 106188213 B CN106188213 B CN 106188213B CN 201610570369 A CN201610570369 A CN 201610570369A CN 106188213 B CN106188213 B CN 106188213B
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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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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/256—Polyterpene radicals
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Abstract
The invention discloses a kind of Simple Purification method of Tea Saponin, belong to technical field of plant extraction, technical scheme is：1) Tea Saponin crude product is dissolved in the alcoholic solution that volume fraction is 80%, centrifugal treating, takes supernatant；2) supernatant is placed in surname extraction flask, takes cholesterol, wrapped with filter paper, is transferred in soxhlet extraction pipe, after being heated to reflux 6~7h of extraction, be cooled to room temperature, extract is filtered, washed, obtain Tea Saponin cholesterin complex；3) by Tea Saponin cholesterin complex drying to constant weight, wrapped, be fitted into soxhlet extraction pipe with filter paper after cooling, extractant is added into Soxhlet flask, 5~6h of extraction is heated to reflux, after cooling, the Tea Saponin by purification process is obtained from soxhlet extraction pipe, purity is 95%~98%.The present invention is simple to operate, cost is low, and purification efficiency is high (purity is 95%~98%), is adapted to industrial amplification production.
Description
Technical field
The invention belongs to technical field of plant extraction, and in particular to a kind of Simple Purification method of Tea Saponin.
Background technology
Tea Saponin is a kind of glucoside compound extracted from the seed of plant of theaceae, and it belongs to saponin class, is a kind of
Natural nonionic surface active agent, it is accessory substance --- the main active substances of leached tea oil slag after extraction tea-seed oil.Due to Tea Saponin
It can be combined with the cholesterol in cell membrane, form compound, so as to change membrane passage, destroy the knot of cell membrane
Structure, cytoplasm is set to exosmose, so that it is dead.Therefore, although containing a certain amount of reactive protein, polysaccharide etc. in tea seed cake, due to it
In contain a certain amount of Tea Saponin, cause leached tea oil slag to be used as Fertilizer application.
As people are to the continuous understanding of tea-seed oil nutritive value, the tea-seed oil that custom has " title of east olive oil " has turned into
Flavored oils on people's dining table, but because tea seed is difficult to harvest, labor cost is higher, causes tea-seed oil processing cost to rise.
Therefore, active development utilizes other active components in tea seed, realizes tea seed recycling, is produced into for reducing tea-seed oil
This, really has certain meaning as the first-class oil product on popular dining table.
A kind of natural nonionic surfactant of good performance of Tea Saponin, excellent foaming, foam stability energy make its extensive
Applied to fields such as light industry, chemical industry, agricultural chemicals, feed, cultivation, weaving, oil recovery, mining, building materials and expressway constructions, be wash it is clean
Agent, insecticides adjuvant, feed addictive, crab shrimp aquaculture protective agent, textile auxiliary, oilfield foaming agent, mining flotation agent and aerating
The important component of concrete foam stabilizer and concrete admixture --- antifreezing agent.Resources of tea saponin is developed, obtains high-purity
Tea Saponin there is certain realistic meaning.
Because Tea Saponin is insoluble in absolute methanol, ethanol, insoluble in organic solvents such as ether, acetone, benzene, petroleum ethers, easily
It is dissolved in aqueous methanol, hydrous ethanol and glacial acetic acid, aceticanhydride, pyridine etc..Therefore Tea Saponin is typically using aqueous methanol, ethanol as extraction
Agent is taken to be extracted, the Tea Saponin purity that the method obtains is generally 60~80%, pale yellow powder.Someone is with water or low concentration
Ammoniacal liquor is extractant, obtains purity as 40~50%, Tea Saponin of brown-red powder.Someone is used using water as extractant, with second
Alcohol, methanol are flocculant, obtain the of a relatively high Tea Saponin of purity.In general, the purity of Tea Saponin is lower, color and luster is deeper,
Its application surface is narrower.The purity of Tea Saponin is improved, is the major measure for widening Tea Saponin application.
The content of the invention
It is an object of the invention to a kind of Simple Purification method of Tea Saponin, this method is simple to operate, practical, purification
Efficiency high, obtained Tea Saponin purity is high, applied widely.
The present invention is to be achieved through the following technical solutions：
A kind of Simple Purification method of Tea Saponin, comprises the following steps：
1) (10~15) g is pressed：10mL amount ratio, Tea Saponin crude product is dissolved in the alcoholic solution that volume fraction is 80%,
Centrifugal treating, take supernatant；
2) supernatant is placed in surname extraction flask, by Tea Saponin crude product：Cholesterol=(10~15)：(7~12)
Mass ratio, cholesterol is taken, wrapped with filter paper, is transferred in soxhlet extraction pipe, after being heated to reflux 6~7h of extraction, be cooled to room temperature, will
Extract filters, and washing, obtains Tea Saponin-cholesterin complex；
3) by Tea Saponin-cholesterin complex drying to constant weight, wrapped, be fitted into soxhlet extraction pipe with filter paper after cooling,
Extractant is added into Soxhlet flask, is heated to reflux 5~6h of extraction, after cooling, is obtained from soxhlet extraction pipe by purifying
The Tea Saponin of reason, purity are 95%~98%.
In step 1), centrifugal treating is 8~12min of centrifugal treating under 2500~3500r/min.
In step 2), speed control is heated to reflux at 7~8min/ times.
In step 2), washing is cleaned 2~4 times with ethanol.
It is to dry Tea Saponin-cholesterin complex at 55~60 DEG C in step 3).
Extractant used in step 3) is ether, toluene or petroleum ether.
In step 3), speed control is heated to reflux at 8~10min/ times.
Also include the step of recovery intermediate product recycles after step 3), be specially：
The extract for being heated to reflux extraction is collected, concentration volume to 1/3~2/3, then cools down, obtains cholesterol crystal,
Filtering, drying, obtain cholesterol.
Compared with prior art, the present invention has technique effect beneficial below：
The Simple Purification method of Tea Saponin disclosed by the invention, because Tea Saponin is soluble in aqueous methanol/ethanol, therefore with
80v/v ethanol dissolves, and is fitted into Soxhlet flask.Though cholesterol is dissolved in ethanol, at 20~50 DEG C, solubility with temperature becomes
Change little, but during more than 50 DEG C, solubility raises suddenly, and Soxhlet method of purification is exactly to utilize the progress of this principle.Tea Saponin exists
Tea Saponin-cholesterin complex is easily combined to form in liquid phase with cholesterol, Tea Saponin-cholesterin complex does not dissolve in aqueous second
Alcohol/methanol, it is easy to separated with extractant (aqueous ethanol/methanol).Again because Tea Saponin does not dissolve in ether/toluene/oil
The organic solvents such as ether, and cholesterol is soluble in the organic solvents such as ether/toluene/petroleum ether, is according to this extractant, can be by tea soap
Element, cholesterol are separated.Cholesterol used in the inventive method does not lose in the purge process of Tea Saponin, can be repeatedly sharp
With, the purifying cost of Tea Saponin will not be dramatically increased, the purifying cost of Tea Saponin is mainly derived from the energy resource consumption of extraction process,
Can also solve the problems, such as difficult solvent recovery in the prior art, it is simple to operate, cost is low, purification efficiency it is high (purity is 95%~
98%), it is adapted to industrial amplification production.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
The present invention reaction principle be：It is compound that Tea Saponin easily combines to form Tea Saponin-cholesterol with cholesterol in the liquid phase
Thing, Tea Saponin-cholesterin complex do not dissolve in aqueous ethanol/methanol, it is easy to extractant (aqueous ethanol/methanol) point
From.Again because Tea Saponin is insoluble in organic solvents such as ether/toluene/petroleum ethers, and cholesterol is soluble in ether/toluene/oil
The organic solvents such as ether, are followed successively by extractant, can be separated Tea Saponin, cholesterol.
Using 80v/v methanol/ethanol as solvent, taking 10~15g thick Tea Saponin, to be dissolved in 100mL volume fractions be 80v/v
Methanol/ethanol in, in 3000 revs/min of lower centrifugal treating 10min, supernatant is fitted into 150mL surname extraction flask, claim
7.0-12g cholesterol is taken, is wrapped with filter paper, is transferred in soxhlet extraction pipe, soxhlet extraction device is installed, cooling water is opened and opens
Close, open heater and heated, it is 1 time/7~8min to control back-flow velocity, 6~7h of continuous extraction, powers off switch,
After being cooled to room temperature, Soxhlet extraction device of dismantling.By extract centrifugal filtration, Tea Saponin-cholesterin complex is obtained, uses 50mL
Methanol point 3 lotions, obtain the pure white Tea Saponin compound of color and luster.
Tea Saponin compound is dried to constant weight in 55~60 DEG C of baking oven, wrapped after cooling with filter paper, loads Soxhlet extraction
Take in pipe, extractant ether/toluene/100~150mL of petroleum ether is moved into Soxhlet flask, open cooling water system, open electricity
Source is heated, and it is 1 time/8~10min, 5~6h of continuous extraction to control back-flow velocity, after cooling, soxhlet extraction device is removed, from rope
What is removed in family name's pipe is the Tea Saponin by purification process, and its purity is 95~98%, and color and luster is pure white, and its aqueous solution is looked for
It is bright.Contain cholesterol in extract, withdraw 1/3~2/3 ether/toluene/petroleum ether extraction liquid, cooling obtains cholesterol knot
Crystalline substance, filtering, drying obtain cholesterol.
Solubility of the cholesterol in methanol/ethanol is 10~12g/100mL, but variation with temperature, especially tea soap
Element is in ethanol before 55 DEG C, and solubility with temperature change is little, but when temperature rises to 55~65 DEG C, solubility drastically increases
Add, more than 2 times of almost dissolved solution degree.The present invention just make use of this property of cholesterol, and cholesterol is placed in
In soxhlet extraction pipe, because being cooled down by the condensed device of thermal evaporation methanol/ethanol in soxhlet extraction device, its temperature it is more 55 DEG C with
On, the now solubility rise of cholesterol quickly, is dissolved in the cholesterol in methanol/ethanol through flowing back and the tea in Soxhlet flask
Saponin combines to form cholesterol-Tea Saponin compound.This process simplify Tea Saponin purifying technique, avoids mixed solvent recovery
Difficult technical problem.
Embodiment 1
A kind of Simple Purification method of Tea Saponin, comprises the following steps：
1) 10g Tea Saponin crude products are dissolved in the alcoholic solution that 100mL volume fractions are 80%, centrifuged under 3000 revs/min
10min is handled, takes supernatant；
2) supernatant is placed in surname extraction flask, takes 7g cholesterol, wrapped with filter paper, be transferred in soxhlet extraction pipe,
Install soxhlet extraction device, open cooling water switch, open heater heated, control back-flow velocity be 1 time/7~
8min, after being heated to reflux 6~7h of extraction, switch is powered off, is cooled to room temperature, extract is filtered, with 50mL methanol point 3
Secondary lotion, obtain Tea Saponin-cholesterin complex；
3) Tea Saponin-cholesterin complex is dried to constant weight in 55 DEG C of baking oven, wrapped after cooling with filter paper, loaded
In soxhlet extraction pipe, 100mL petroleum ethers are added into Soxhlet flask, open cooling water system, turn on the power heating, control backflow
Speed is 1 time/8~10min, is heated to reflux 5~6h of extraction, after cooling, is obtained from soxhlet extraction pipe by purification process
Tea Saponin, purity 97%.The Tea Saponin color and luster of separation is pure white, and its aqueous solution is looked for bright.Contain cholesterol in extract, receive
1/3~2/3 petroleum ether extraction liquid is returned, cooling obtains cholesterol crystal, filters, and drying obtains cholesterol.
Embodiment 2
A kind of Simple Purification method of Tea Saponin, comprises the following steps：
1) 15g Tea Saponin crude products are dissolved in the alcoholic solution that 100mL volume fractions are 80%, centrifuged under 2500 revs/min
12min is handled, takes supernatant；
2) supernatant is placed in surname extraction flask, takes 10g cholesterol, wrapped with filter paper, be transferred in soxhlet extraction pipe,
Install soxhlet extraction device, open cooling water switch, open heater heated, control back-flow velocity be 1 time/7~
8min, after being heated to reflux 6~7h of extraction, switch is powered off, is cooled to room temperature, extract is filtered, with 50mL methanol point 2
Secondary lotion, obtain Tea Saponin-cholesterin complex；
3) Tea Saponin-cholesterin complex is dried to constant weight in 60 DEG C of baking oven, wrapped after cooling with filter paper, loaded
In soxhlet extraction pipe, 150mL ether is added into Soxhlet flask, opens cooling water system, turns on the power heating, control backflow speed
Spend for 1 time/8~10min, be heated to reflux 5~6h of extraction, after cooling, the tea by purification process is obtained from soxhlet extraction pipe
Saponin, purity 95%.The Tea Saponin color and luster of separation is pure white, and its aqueous solution is looked for bright.Contain cholesterol in extract, withdraw
1/3~2/3 ether extraction liquid, cooling obtain cholesterol crystal, filter, and drying obtains cholesterol.
Embodiment 3
A kind of Simple Purification method of Tea Saponin, comprises the following steps：
1) 13g Tea Saponin crude products are dissolved in the alcoholic solution that 100mL volume fractions are 80%, centrifuged under 3500 revs/min
8min is handled, takes supernatant；
2) supernatant is placed in surname extraction flask, takes 12g cholesterol, wrapped with filter paper, be transferred in soxhlet extraction pipe,
Install soxhlet extraction device, open cooling water switch, open heater heated, control back-flow velocity be 1 time/7~
8min, after being heated to reflux 6~7h of extraction, switch is powered off, is cooled to room temperature, extract is filtered, with 50mL methanol point 4
Secondary lotion, obtain Tea Saponin-cholesterin complex；
3) Tea Saponin-cholesterin complex is dried to constant weight in 60 DEG C of baking oven, wrapped after cooling with filter paper, loaded
In soxhlet extraction pipe, 130mL toluene is added into Soxhlet flask, opens cooling water system, turns on the power heating, control backflow speed
Spend for 1 time/8~10min, be heated to reflux 5~6h of extraction, after cooling, the tea by purification process is obtained from soxhlet extraction pipe
Saponin, purity 98%.The Tea Saponin color and luster of separation is pure white, and its aqueous solution is looked for bright.Contain cholesterol in extract, withdraw
1/3~2/3 toluene extract, cooling obtain cholesterol crystal, filter, and drying obtains cholesterol.
In summary, the inventive method is simple to operate, cost is low, and purification efficiency is high, purifying of the cholesterol in Tea Saponin
Do not lose, can recycle in journey, the purifying cost of Tea Saponin, the purifying cost main source of Tea Saponin will not be dramatically increased
In the energy resource consumption of extraction process.
Claims (6)
1. a kind of Simple Purification method of Tea Saponin, it is characterised in that comprise the following steps：
1) (10~15) g is pressed：100mL amount ratio, Tea Saponin crude product is dissolved in the alcoholic solution that volume fraction is 80%, centrifugation
Processing, takes supernatant；
2) supernatant is placed in surname extraction flask, by Tea Saponin crude product：Cholesterol=(10~15)：The quality of (7~12)
Than taking cholesterol, being wrapped with filter paper, is transferred in soxhlet extraction pipe, after being heated to reflux 6~7h of extraction, be cooled to room temperature, will extract
Liquid filters, and washing, obtains Tea Saponin-cholesterin complex；Wherein, speed control is heated to reflux at 7~8min/ times；
3) by Tea Saponin-cholesterin complex drying to constant weight, wrapped, be fitted into soxhlet extraction pipe with filter paper after cooling, to rope
Extractant is added in family name's flask, is heated to reflux 5~6h of extraction, after cooling, is obtained from soxhlet extraction pipe by purification process
Tea Saponin, purity are 95%~98%；Wherein, speed control is heated to reflux at 8~10min/ times.
2. the Simple Purification method of Tea Saponin according to claim 1, it is characterised in that in step 1), centrifugal treating is
Under 2500~3500r/min, 8~12min of centrifugal treating.
3. the Simple Purification method of Tea Saponin according to claim 1, it is characterised in that in step 2), washing is to use second
Alcohol cleans 2~4 times.
4. the Simple Purification method of Tea Saponin according to claim 1, it is characterised in that in step 3), be by Tea Saponin-
Cholesterin complex is dried at 55~60 DEG C.
5. the Simple Purification method of Tea Saponin according to claim 1, it is characterised in that extractant used in step 3) is second
Ether, toluene or petroleum ether.
6. the Simple Purification method of Tea Saponin according to claim 1, it is characterised in that also include after step 3) in recovery
Between product recycle the step of, be specially：
The extract for being heated to reflux extraction is collected, concentration volume to 1/3~2/3, is then cooled down, obtains cholesterol crystal, filter,
Drying, obtains cholesterol.
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| CN201610570369.5A CN106188213B (en) | 2016-07-19 | 2016-07-19 | A kind of Simple Purification method of Tea Saponin |
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| CN106188213B true CN106188213B (en) | 2018-04-06 |
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| CN108341716A (en) * | 2018-04-02 | 2018-07-31 | 青岛元汇丰企业管理咨询服务有限公司 | A kind of antibacterial growth-promoting elongated biological pesticide of plant source |
| CN108997467A (en) * | 2018-07-11 | 2018-12-14 | 永州职业技术学院 | A method of Tea Saponin is extracted using biotechnology |
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| CN102875631B (en) * | 2012-10-16 | 2013-12-04 | 老知青集团有限公司 | Method for extracting tea saponin from tea-seed pancake |
| CN104262426A (en) * | 2014-08-29 | 2015-01-07 | 王晓伟 | Method for extracting tea saponin |
| CN104945463A (en) * | 2015-07-29 | 2015-09-30 | 湖南湘浩油茶生物科技有限公司 | Extracting method for tea saponin |
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