CN106188213A - 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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- CN106188213A CN106188213A CN201610570369.5A CN201610570369A CN106188213A CN 106188213 A CN106188213 A CN 106188213A CN 201610570369 A CN201610570369 A CN 201610570369A CN 106188213 A CN106188213 A CN 106188213A
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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) is dissolved in by tea saponin crude product in the alcoholic solution that volume fraction is 80%, centrifugal treating, takes supernatant；2) supernatant is placed in surname extraction flask, takes cholesterol, wrap with filter paper, proceed in soxhlet extraction pipe, after being heated to reflux extracting 6～7h, be cooled to room temperature, extract is filtered, washing, obtain tea saponin cholesterin complex；3) tea saponin cholesterin complex is dried to constant weight, wraps with filter paper after cooling, load in soxhlet extraction pipe, in Soxhlet flask, add extractant, be heated to reflux extracting 5～6h, after cooling, obtaining the tea saponin through purification process from soxhlet extraction pipe, purity is 95%～98%.The present invention is simple to operate, low cost, and purification efficiency is high (purity is 95%～98%), is suitable for industrial amplification production.
Description
Technical field
The invention belongs to technical field of plant extraction, be specifically related 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 surfactant, is to extract by-product---the main active substances of leached tea oil slag after Oleum Camelliae.Due to tea saponin
Can be combined with the cholesterol in cell membrane, form complex, thus change membrane passage, destroy the knot of cell membrane
Structure, makes Cytoplasm exosmose, so that dead.Therefore, although containing a certain amount of reactive protein, polysaccharide etc. in tea seed cake, due to it
In containing a certain amount of tea saponin, cause leached tea oil slag only as Fertilizer application.
Along with the people's continuous understanding to Oleum Camelliae nutritive value, custom has the Oleum Camelliae of " title of east olive oil " to become
Flavored oils on people's dining table, but owing to camellia oleosa seed is difficult to gather, labor cost is higher, causes Oleum Camelliae processing cost to rise.
Therefore, other active component during active development utilizes camellia oleosa seed, it is achieved camellia oleosa seed recycling, produces into for reducing Oleum Camelliae
This, the first-class oil product really become on popular dining table has certain meaning.
A kind of natural nonionic surfactant of good performance of tea saponin, excellent foaming, foam stability can make it widely
Be applied to light industry, chemical industry, pesticide, feedstuff, cultivate, weave, recover the oil, dig up mine, the field such as building materials and expressway construction, be wash clean
Agent, insecticides adjuvant, feed additive, Eriocheir sinensis shrimp aquaculture protective agent, textile auxiliary, oilfield foaming agent, mining flotation agent and aerating
Concrete foam stabilizer and the important component part of concrete admixture antifreezing agent.Exploitation resources of tea saponin, obtains high-purity
Tea saponin there is certain realistic meaning.
Owing to tea saponin is insoluble in absolute methanol, ethanol, insoluble in organic solvents such as ether, acetone, benzene, petroleum ether, easily
It is dissolved in aqueous methanol, aquiferous ethanol and glacial acetic acid, acetic anhydride, pyridine etc..Therefore tea saponin is typically with aqueous methanol, ethanol for extraction
Taking agent to extract, the tea saponin purity that this method obtains is generally 60～80%, pale yellow powder.Someone is with water or low concentration
Ammonia is extractant, obtain purity be 40～50%, the tea saponin of brown-red powder.Someone uses with water as extractant, with second
Alcohol, methanol are flocculant, obtain the tea saponin that purity is of a relatively high.It is said that in general, the purity of tea saponin is the lowest, color and luster is the deepest,
Its application surface is the narrowest.Improve the purity of tea saponin, be the major measure widening tea saponin application.
Summary of the invention
It is an object of the invention to a kind of Simple Purification method of tea saponin, the method is simple to operate, practical, purifies
Efficiency is high, and the tea saponin purity prepared 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) by the amount ratio of (10～15) g:10mL, 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, by tea saponin crude product: cholesterol=(10～15): (7～12)
Mass ratio, takes cholesterol, wraps with filter paper, proceeds in soxhlet extraction pipe, after being heated to reflux extracting 6～7h, is cooled to room temperature, will
Extract filters, washing, obtains tea saponin-cholesterin complex；
3) tea saponin-cholesterin complex is dried to constant weight, wraps with filter paper after cooling, load in soxhlet extraction pipe,
In Soxhlet flask, add extractant, be heated to reflux extracting 5～6h, after cooling, obtain from soxhlet extraction pipe at through purification
The tea saponin of reason, purity is 95%～98%.
Step 1) in, centrifugal treating is under 2500～3500r/min, centrifugal treating 8～12min.
Step 2) in, it is heated to reflux speed controlling 7～8min/ time.
Step 2) in, washing is with ethanol purge 2～4 times.
Step 3) in, it is that tea saponin-cholesterin complex is dried at 55～60 DEG C.
Step 3) used by extractant be ether, toluene or petroleum ether.
Step 3) in, it is heated to reflux speed controlling 8～10min/ time.
Step 3) after also include reclaim intermediate product recycling step, particularly as follows:
Collecting the extract being heated to reflux extraction, concentration volume, to 1/3～2/3, then cools down, obtains cholesterol crystal,
Filter, dry, obtain cholesterol.
Compared with prior art, the present invention has a following useful technique effect:
The Simple Purification method of tea saponin disclosed by the invention, owing to tea saponin is soluble in aqueous methanol/ethanol, therefore with
80v/v ethanol dissolves, and loads in Soxhlet flask.Though cholesterol is dissolved in ethanol, but when 20～50 DEG C, solubility with temperature becomes
Changing little, but during more than 50 DEG C, dissolubility raises suddenly, Soxhlet method of purification utilizes this principle to carry out just.Tea saponin exists
Easily be combined formation tea saponin-cholesterin complex in liquid phase with cholesterol, tea saponin-cholesterin complex is insoluble in aqueous second
Alcohol/methanol, it is easy to separate with extractant (aqueous ethanol/methanol).Again owing to tea saponin is insoluble 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 extractant according to this, can be by tea soap
Element, cholesterol separate.Cholesterol used by the inventive method is not loss in the purge process of tea saponin, can be repeatedly sharp
With, the purification cost of tea saponin will not be dramatically increased, the purification cost of tea saponin is mainly derived from the energy resource consumption of extraction process,
Can also solve the problem of difficult solvent recovery in prior art, simple to operate, low cost, purification efficiency high (purity be 95%～
98%), it is suitable for industrial amplification production.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, described in be explanation of the invention and
It not to limit.
The reaction principle of the present invention is: tea saponin is easily combined formation tea saponin-cholesterol in the liquid phase and is combined with cholesterol
Thing, tea saponin-cholesterin complex is insoluble in aqueous ethanol/methanol, it is easy to extractant (aqueous ethanol/methanol) point
From.Again owing to tea saponin is insoluble in organic solvents such as ether/toluene/petroleum ether, and cholesterol is soluble in ether/toluene/oil
The organic solvents such as ether, are followed successively by extractant, can tea saponin, cholesterol be separated.
With the methanol/ethanol of 80v/v as solvent, take the inferior tea Saponin of 10～15g being dissolved in 100mL volume fraction is 80v/v
Methanol/ethanol in, 3000 revs/min of lower centrifugal treating 10min, supernatant is loaded in the surname extraction flask of 150mL, claim
Take the cholesterol of 7.0-12g, wrap with filter paper, proceed in soxhlet extraction pipe, soxhlet extraction device is installed, open cooling water and open
Closing, open heater and heat, controlling back-flow velocity is 1 time/7～8min, and continuous extraction 6～7h powers off switch,
After being cooled to room temperature, Soxhlet extraction device of dismantling.By extract centrifugal filtration, obtain tea saponin-cholesterin complex, use 50mL
Methanol divide 3 lotions, obtain the tea saponin complex that color and luster is pure white.
Tea saponin complex is dried to constant weight in the baking oven of 55～60 DEG C, wraps with filter paper after cooling, load Soxhlet extraction
Take in pipe, extractant ether/toluene/petroleum ether 100～150mL is moved in Soxhlet flask, open cooling water system, open electricity
Source is heated, and controlling back-flow velocity is 1 time/8～10min, continuous extraction 5～6h, after cooling, removes soxhlet extraction device, from rope
Remove in family name's pipe is the tea saponin through purification process, and its purity is 95～98%, and color and luster is pure white, and its aqueous solution is looked for
Bright.Containing cholesterol in extract, regaining the ether/toluene/petroleum ether extraction liquid of 1/3～2/3, cooling obtains cholesterol knot
Crystalline substance, filters, and dries and obtains cholesterol.
Cholesterol dissolubility 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, dissolubility drastically increases
Add, more than 2 times of the most dissolved solution degree.The present invention just make use of this character of cholesterol, is placed in by cholesterol
In soxhlet extraction pipe, because being cooled down by the thermal evaporation condensed device of methanol/ethanol in soxhlet extraction device, its temperature many 55 DEG C with
On, now the dissolubility of cholesterol raises quickly, the cholesterol being dissolved in methanol/ethanol tea in backflow with Soxhlet flask
Saponin combines and forms cholesterol-tea saponin complex.This process simplify tea saponin purifying technique, it is to avoid 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 product is dissolved in the alcoholic solution that 100mL volume fraction is 80%, centrifugal under 3000 revs/min
Process 10min, take supernatant；
2) supernatant is placed in surname extraction flask, takes 7g cholesterol, wrap with filter paper, proceed in soxhlet extraction pipe,
Soxhlet extraction device is installed, opens cooling water switch, open heater and heat, control back-flow velocity be 1 time/7～
8min, after being heated to reflux extracting 6～7h, powers off switch, is cooled to room temperature, is filtered by extract, divides 3 with the methanol of 50mL
Secondary lotion, obtains tea saponin-cholesterin complex；
3) tea saponin-cholesterin complex is dried to constant weight in the baking oven of 55 DEG C, wraps with filter paper after cooling, load
In soxhlet extraction pipe, in Soxhlet flask, add 100mL petroleum ether, open cooling water system, turn on the power heating, control backflow
Speed is 1 time/8～10min, is heated to reflux extracting 5～6h, after cooling, obtains through purification process from soxhlet extraction pipe
Tea saponin, purity is 97%.The tea saponin color and luster separated is pure white, and its aqueous solution is looked for bright.Containing cholesterol in extract, receive
Returning the petroleum ether extraction liquid of 1/3～2/3, cooling obtains cholesterol crystal, filters, and dries and obtains cholesterol.
Embodiment 2
A kind of Simple Purification method of tea saponin, comprises the following steps:
1) 15g tea saponin crude product is dissolved in the alcoholic solution that 100mL volume fraction is 80%, centrifugal under 2500 revs/min
Process 12min, take supernatant；
2) supernatant is placed in surname extraction flask, takes 10g cholesterol, wrap with filter paper, proceed in soxhlet extraction pipe,
Soxhlet extraction device is installed, opens cooling water switch, open heater and heat, control back-flow velocity be 1 time/7～
8min, after being heated to reflux extracting 6～7h, powers off switch, is cooled to room temperature, is filtered by extract, divides 2 with the methanol of 50mL
Secondary lotion, obtains tea saponin-cholesterin complex；
3) tea saponin-cholesterin complex is dried to constant weight in the baking oven of 60 DEG C, wraps with filter paper after cooling, load
In soxhlet extraction pipe, in Soxhlet flask, add 150mL ether, open cooling water system, turn on the power heating, control backflow speed
Degree is 1 time/8～10min, is heated to reflux extracting 5～6h, after cooling, obtains the tea through purification process from soxhlet extraction pipe
Saponin, purity is 95%.The tea saponin color and luster separated is pure white, and its aqueous solution is looked for bright.Containing cholesterol in extract, regain
The ether extraction liquid of 1/3～2/3, cooling obtains cholesterol crystal, filters, and dries and obtains cholesterol.
Embodiment 3
A kind of Simple Purification method of tea saponin, comprises the following steps:
1) 13g tea saponin crude product is dissolved in the alcoholic solution that 100mL volume fraction is 80%, centrifugal under 3500 revs/min
Process 8min, take supernatant；
2) supernatant is placed in surname extraction flask, takes 12g cholesterol, wrap with filter paper, proceed in soxhlet extraction pipe,
Soxhlet extraction device is installed, opens cooling water switch, open heater and heat, control back-flow velocity be 1 time/7～
8min, after being heated to reflux extracting 6～7h, powers off switch, is cooled to room temperature, is filtered by extract, divides 4 with the methanol of 50mL
Secondary lotion, obtains tea saponin-cholesterin complex；
3) tea saponin-cholesterin complex is dried to constant weight in the baking oven of 60 DEG C, wraps with filter paper after cooling, load
In soxhlet extraction pipe, in Soxhlet flask, add 130mL toluene, open cooling water system, turn on the power heating, control backflow speed
Degree is 1 time/8～10min, is heated to reflux extracting 5～6h, after cooling, obtains the tea through purification process from soxhlet extraction pipe
Saponin, purity is 98%.The tea saponin color and luster separated is pure white, and its aqueous solution is looked for bright.Containing cholesterol in extract, regain
The toluene extract of 1/3～2/3, cooling obtains cholesterol crystal, filters, and dries and obtains cholesterol.
In sum, the inventive method is simple to operate, low cost, and purification efficiency is high, and cholesterol is in the purification mistake of tea saponin
In journey, not loss, can recycle, will not dramatically increase the purification cost of tea saponin, the purification cost main source of tea saponin
Energy resource consumption in extraction process.
Claims (8)
1. the Simple Purification method of a tea saponin, it is characterised in that comprise the following steps:
1) by the amount ratio of (10～15) g:100mL, tea saponin crude product is dissolved in the alcoholic solution that volume fraction is 80%, centrifugal
Process, take supernatant；
2) supernatant is placed in surname extraction flask, by tea saponin crude product: cholesterol=(10～15): the quality of (7～12)
Ratio, takes cholesterol, wraps with filter paper, proceeds in soxhlet extraction pipe, after being heated to reflux extracting 6～7h, is cooled to room temperature, will extraction
Liquid filters, washing, obtains tea saponin-cholesterin complex；
3) tea saponin-cholesterin complex is dried to constant weight, wraps with filter paper after cooling, load in soxhlet extraction pipe, to rope
Family name's flask adds extractant, is heated to reflux extracting 5～6h, after cooling, obtains through purification process from soxhlet extraction pipe
Tea saponin, purity is 95%～98%.
The Simple Purification method of tea saponin the most according to claim 1, it is characterised in that step 1) in, centrifugal treating is
Under 2500～3500r/min, centrifugal treating 8～12min.
The Simple Purification method of tea saponin the most according to claim 1, it is characterised in that step 2) in, it is heated to reflux speed
Degree controls 7～8min/ time.
The Simple Purification method of tea saponin the most according to claim 1, it is characterised in that step 2) in, washing is to use second
Alcohol cleans 2～4 times.
The Simple Purification method of tea saponin the most according to claim 1, it is characterised in that step 3) in, be by tea saponin-
Cholesterin complex is dried at 55～60 DEG C.
The Simple Purification method of tea saponin the most according to claim 1, it is characterised in that step 3) used by extractant be second
Ether, toluene or petroleum ether.
The Simple Purification method of tea saponin the most according to claim 1, it is characterised in that step 3) in, it is heated to reflux speed
Degree controls 8～10min/ time.
The Simple Purification method of tea saponin the most according to claim 1, it is characterised in that step 3) after also include reclaim in
Between product recycling step, particularly as follows:
Collecting the extract being heated to reflux extraction, concentration volume to 1/3～2/3, then cools down, obtains cholesterol crystal, filter,
Dry, obtain cholesterol.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| CN102875631A (en) * | 2012-10-16 | 2013-01-16 | 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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| CN102875631A (en) * | 2012-10-16 | 2013-01-16 | 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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| CN106188213B (en) | 2018-04-06 |
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