CN108997467A - A method of Tea Saponin is extracted using biotechnology - Google Patents
A method of Tea Saponin is extracted using biotechnology Download PDFInfo
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- CN108997467A CN108997467A CN201810754104.XA CN201810754104A CN108997467A CN 108997467 A CN108997467 A CN 108997467A CN 201810754104 A CN201810754104 A CN 201810754104A CN 108997467 A CN108997467 A CN 108997467A
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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
- C07H1/08—Separation; Purification from natural products
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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 belongs to technical field of organic chemistry, a kind of method for extracting Tea Saponin using biotechnology is disclosed, the system for extracting Tea Saponin using biotechnology includes: to crush module, sterilization module, mixing module, complexing processing module, decomplexing separation module, purification blocks.The Tea Saponin purity that extracting method testing result provided by the invention shows is up to 98% or more, and recovery rate can reach 30%；It is not lost in the purification process of Tea Saponin by purification blocks with cholesterol simultaneously, it can recycle, the purifying cost of Tea Saponin will not be dramatically increased, the purifying cost of Tea Saponin is mainly derived from the energy consumption of extraction process, the problem of also can solve difficult solvent recovery in the prior art, easy to operate, at low cost, purification efficiency is high (purity is 95%~98%), is suitble to industrial amplification production.
Description
Technical field
The invention belongs to technical field of organic chemistry more particularly to a kind of methods for extracting Tea Saponin using biotechnology.
Background technique
Tea Saponin also known as tea saponin are a kind of glycoside compounds by extracting in tea tree seed (tea seed, tea seeds),
It is a kind of natural surfactant of good performance, it can be widely applied to light industry, chemical industry, pesticide, feed, cultivation, weaves, adopts
The fields such as oil, mining, building materials and expressway construction.Emulsifier, abluent, insecticides adjuvant, feed addictive, crab shrimp is manufactured to support
Grow protective agent, textile auxiliary, oilfield foaming agent, mining flotation agent and air entrained concrete foam stabilizer and concrete admixture ---
Antifreezing agent etc..However, existing Tea Saponin DNA purity is not high, extraction operation is complicated.
In conclusion problem of the existing technology is:
(1) existing Tea Saponin DNA purity is not high, and extraction operation is complicated.
(2) Tea Saponin slightly proposes processing there are recovery rates and is low, increases extraction cost.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of methods for extracting Tea Saponin using biotechnology.
The invention is realized in this way a method of Tea Saponin is extracted using biotechnology, it is described to utilize biotechnology
Extract Tea Saponin method the following steps are included:
Step 1 is crushed leached tea oil slag by crushing module；The leached tea oil slag of crushing is sterilized, is sterilized, is added
Aqueous solution is made in pure water；
The sterilization uses CO 2 bactericidal model: carrying out group using the Box-Behnken module of Response Surface Method
It closes, Three factors-levels, definition process time, temperature and pressure are independent variable, and true value is respectively with X1、X2And X3It indicates, compiles
Code value is respectively with x1、x2And x3It indicates, there are relationship xi=(Xi- X0)/△ X, X in formula0For the true value of independent variable, △ X is certainly
The change step of variable；Defining HPCD and killing the order of magnitude Y of lactic acid bacteria is response, Y=lgN0/Nt, N in formula0For the first of meat sample
Beginning bacterium number, Nt are the remaining bacterium number of meat sample after HPCD processing, and the regression equation for establishing model indicates:
Wherein, β0: intercept；βj: slope；εi: error；I=1,2 ... n；yiFor the predicted value for having removed error amount；
Step 2 is mixed leached tea oil slag aqueous solution with extracting solution by mixing module, and progress slightly proposes processing, obtains Tea Saponin
Extracting solution；The process conditions for slightly proposing processing are 53 DEG C of Extracting temperature, concentration of alcohol 45%, time 95min, liquid-solid ratio 10.5；
Step 3 is mixed tea saponin extract with sterols complexing agent by complexing processing module, using complexing model
Complexing processing is carried out, Tea Saponin complex compound is obtained；
Each point P and its 8- neighborhood point constitute a micro- curved surface on the complexing model particle surface, according to Differential Geometry
Surface theory it is theoretical, surface parameter equation is z=z (x, y), wherein x, y are coordinate of this in image array, then the point
The Gaussian curvature K and mean curvature H at place are as follows:
In formula, k1And k2For the principal curvatures at the point, maximum curvature and minimum curvature are respectively indicated；P, q indicates that single order is led
Number, r, s, t indicate second dervative；
Tea Saponin complex compound is mixed with solution sequester by decomplexing separation module, carries out decomplexing separation processing by step 4,
Obtain Tea Saponin；
Step 5, to Tea Saponin into purifying.
Further, extracting solution is one of methanol, ethyl alcohol, water, normal propyl alcohol, isopropanol and butanol or a variety of.
Further, the amount ratio of leached tea oil slag and extracting solution is 1g:1mL~12mL.
Further, slightly proposing processing includes: successively to be heated, filtered after mixing leached tea oil slag with extracting solution, obtains tea soap
Plain extracting solution；The temperature of heating is 50 DEG C~110 DEG C, and the time is 1h~3h.
Further, purification process includes:
1) amount ratio for pressing 11~15g:100mL, Tea Saponin crude product is dissolved in the alcoholic solution that volume fraction is 80%, from
Heart processing, takes supernatant；
2) supernatant is placed in Soxhlet extraction flask, by Tea Saponin crude product: cholesterol=11~15:7~12 quality
Than taking cholesterol, being wrapped with filter paper, is transferred in soxhlet extraction pipe, after being heated to reflux 6~7h of extraction, is cooled to room temperature, will be extracted
Liquid filtering, washing obtain Tea Saponin-cholesterin complex；
3) it by Tea Saponin-cholesterin complex drying to constant weight, is wrapped, is fitted into soxhlet extraction pipe with filter paper after cooling,
Extractant is added into Soxhlet flask, is heated to reflux 5~6h of extraction and is obtained from soxhlet extraction pipe by purifying place after cooling
The Tea Saponin of reason, purity are 95%~98%.
Another object of the present invention is to provide a kind of benefits for realizing the method that Tea Saponin is extracted using biotechnology
The system for extracting Tea Saponin with biotechnology, the system for extracting Tea Saponin using biotechnology include:
Crush module, sterilization module, mixing module, complexing processing module, decomplexing separation module, purification blocks；
Module is crushed, is connect with sterilization module, for crushing leached tea oil slag；
Sterilization module is connect with crushing module, mixing module, for being sterilized, being sterilized by the leached tea oil slag of crushing, is added
Aqueous solution is made in pure water；
Mixing module is connect with sterilization module, complexing processing module, for leached tea oil slag aqueous solution to be mixed with extracting solution,
Progress slightly proposes processing, obtains tea saponin extract；
Processing module is complexed, is connect with mixing module, decomplexing separation module, is used for the tea saponin extract and sterol
The mixing of class complexing agent, carries out complexing processing, obtains Tea Saponin complex compound；
Decomplexing separation module connect with complexing processing module, purification blocks, is used for the Tea Saponin complex compound and decomplexing
Solvent mixing, carries out decomplexing separation processing, obtains Tea Saponin；
Purification blocks are connect with decomplexing separation module, for Tea Saponin into purifying.
Advantages of the present invention and good effect are as follows: extracting method provided by the invention by trace effect, make Tea Saponin with
Sterols complexing agent is complexed to obtain solid, and other impurities are not complexed, to realize the separation of chemical reaction level, then lead to
It crosses decomplexing and obtains the Tea Saponin of high-purity.Testing result shows the Tea Saponin purity is high that extracting method provided by the invention obtains
Up to 98% or more, recovery rate can reach 30%；Do not have in the purification process of Tea Saponin by purification blocks cholesterol simultaneously
There is loss, can recycle, the purifying cost of Tea Saponin will not be dramatically increased, the purifying cost of Tea Saponin is mainly derived from extraction
The energy consumption of process, moreover it is possible to solve the problems, such as difficult solvent recovery in the prior art, easy to operate, at low cost, purification efficiency
High (purity is 95%~98%), is suitble to industrial amplification production.Sterilization of the invention is significant using CO 2 bactericidal model
Property is good, accuracy is high, and independence is good between each significant factor, can express killing for the lactic acid bacteria of HPCD at different conditions well
Bacterium effect；Meanwhile on significant factor influence bactericidal effect analysis the result shows that, temperature and pressure can enhance bactericidal effect,
It influences extremely significant.It is 81.92% ± 0.59% that the present invention, which slightly mentions the recovery rate that the process conditions of processing are,.Particle of the invention
The non-uniform Distribution of surface charge, closer to natural characterization of adsorption.
Detailed description of the invention
Fig. 1 is the method flow diagram that Tea Saponin is extracted using biotechnology that the present invention implements to provide.
Fig. 2 is the system structure diagram that Tea Saponin is extracted using biotechnology that the present invention implements to provide.
In Fig. 2: 1, crushing module；2, sterilization module；3, mixing module；4, processing module is complexed；5, decomplexing separation module；
6, purification blocks.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
With reference to the accompanying drawing and specific embodiment is further described application principle of the invention.
As shown in Figure 1, it is provided by the invention it is a kind of using biotechnology extract Tea Saponin method the following steps are included:
Step S101 is crushed leached tea oil slag by crushing module；The leached tea oil slag of crushing is carried out by sterilization module
Sterilization, disinfection are added pure water and aqueous solution are made；
Step S102 is mixed leached tea oil slag aqueous solution with extracting solution by mixing module, and progress slightly proposes processing, obtains tea soap
Plain extracting solution；
The tea saponin extract is mixed with sterols complexing agent by complexing processing module, carries out network by step S103
Conjunction processing, obtains Tea Saponin complex compound；
The Tea Saponin complex compound is mixed with solution sequester by decomplexing separation module, carries out decomplexing point by step S104
From processing, Tea Saponin is obtained；
Step S105, by purification blocks to Tea Saponin into purifying.
As shown in Fig. 2, the system provided by the invention for extracting Tea Saponin using biotechnology includes: to crush module 1, sterilization
Module 2, mixing module 3, complexing processing module 4, decomplexing separation module 5, purification blocks 6.
Module 1 is crushed, is connect with sterilization module 2, for crushing leached tea oil slag；
Sterilization module 2 is connect with crushing module 1, mixing module 3, for the leached tea oil slag of crushing to be sterilized, is sterilized,
Pure water is added, aqueous solution is made；
Mixing module 3 is connect, for mixing leached tea oil slag aqueous solution with extracting solution with sterilization module 2, complexing processing module 4
It closes, progress slightly proposes processing, obtains tea saponin extract；
Processing module 4 is complexed, connect with mixing module 3, decomplexing separation module 5, for by the tea saponin extract and
The mixing of sterols complexing agent, carries out complexing processing, obtains Tea Saponin complex compound；
Decomplexing separation module 5 connect with complexing processing module 4, purification blocks 6, for by the Tea Saponin complex compound and
Sequester mixing is solved, decomplexing separation processing is carried out, obtains Tea Saponin；
Purification blocks 6 are connect with decomplexing separation module 5, for Tea Saponin into purifying.
Extracting solution described in mixing module 3 provided by the invention is in methanol, ethyl alcohol, water, normal propyl alcohol, isopropanol and butanol
It is one or more.
The amount ratio of leached tea oil slag described in mixing module 3 provided by the invention and extracting solution is 1g:(1mL~12mL).
The process of processing is slightly proposed described in mixing module 3 provided by the invention specifically includes the following steps:
It successively heated, filtered after leached tea oil slag is mixed with extracting solution, obtain tea saponin extract；
The temperature of the heating is 50 DEG C~110 DEG C, and the time is 1h~3h.
6 purification process of purification blocks provided by the invention is as follows:
1) amount ratio for pressing (11~15) g:100mL, Tea Saponin crude product is dissolved in the alcoholic solution that volume fraction is 80%,
Centrifugal treating takes supernatant；
2) supernatant is placed in Soxhlet extraction flask, by Tea Saponin crude product: cholesterol=(11~15): (7~12)
Mass ratio takes cholesterol, is wrapped with filter paper, is transferred in soxhlet extraction pipe, after being heated to reflux 6~7h of extraction, is cooled to room temperature, will
Extract liquor filtering, washing obtain Tea Saponin-cholesterin complex；
3) it by Tea Saponin-cholesterin complex drying to constant weight, is wrapped, is fitted into soxhlet extraction pipe with filter paper after cooling,
Extractant is added into Soxhlet flask, is heated to reflux 5~6h of extraction and is obtained from soxhlet extraction pipe by purifying place after cooling
The Tea Saponin of reason, purity are 95%~98%.
Application principle of the invention is further described combined with specific embodiments below.
It is provided in an embodiment of the present invention using biotechnology extract Tea Saponin method the following steps are included:
Step 1 is crushed leached tea oil slag by crushing module；The leached tea oil slag of crushing is sterilized, is sterilized, is added
Aqueous solution is made in pure water；
The sterilization uses CO 2 bactericidal model: carrying out group using the Box-Behnken module of Response Surface Method
It closes, Three factors-levels, definition process time, temperature and pressure are independent variable, and true value is respectively with X1、X2And X3It indicates, compiles
Code value is respectively with x1、x2And x3It indicates, there are relationship xi=(Xi- X0)/△ X, X in formula0For the true value of independent variable, △ X is certainly
The change step of variable；Defining HPCD and killing the order of magnitude Y of lactic acid bacteria is response, Y=lgN0/Nt, N in formula0For the first of meat sample
Beginning bacterium number, Nt are the remaining bacterium number of meat sample after HPCD processing, and the regression equation for establishing model indicates:
Wherein, β0: intercept；βj: slope；εi: error；I=1,2 ... n；yiFor the predicted value for having removed error amount；
Step 2 is mixed leached tea oil slag aqueous solution with extracting solution by mixing module, and progress slightly proposes processing, obtains Tea Saponin
Extracting solution；The process conditions for slightly proposing processing are 53 DEG C of Extracting temperature, concentration of alcohol 45%, time 95min, liquid-solid ratio 10.5；
Step 3 is mixed tea saponin extract with sterols complexing agent by complexing processing module, using complexing model
Complexing processing is carried out, Tea Saponin complex compound is obtained；
Each point P and its 8- neighborhood point constitute a micro- curved surface on the complexing model particle surface, according to Differential Geometry
Surface theory it is theoretical, surface parameter equation is z=z (x, y), wherein x, y are coordinate of this in image array, then the point
The Gaussian curvature K and mean curvature H at place are as follows:
In formula, k1And k2For the principal curvatures at the point, maximum curvature and minimum curvature are respectively indicated；P, q indicates that single order is led
Number, r, s, t indicate second dervative；
Tea Saponin complex compound is mixed with solution sequester by decomplexing separation module, carries out decomplexing separation processing by step 4,
Obtain Tea Saponin；
Step 5, to Tea Saponin into purifying.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. a kind of method for extracting Tea Saponin using biotechnology, which is characterized in that described to extract Tea Saponin using biotechnology
Method the following steps are included:
Step 1 is crushed leached tea oil slag by crushing module；The leached tea oil slag of crushing is sterilized, is sterilized, is added pure
Aqueous solution is made in water；
The sterilization uses CO 2 bactericidal model: being combined using the Box-Behnken module of Response Surface Method, three
Factor three is horizontal, and definition process time, temperature and pressure are independent variable, and true value is respectively with X1、X2And X3It indicates, encoded radio
Respectively with x1、x2And x3It indicates, there are relationship xi=(Xi- X0)/△ X, X in formula0For the true value of independent variable, △ X is independent variable
Change step；Defining HPCD and killing the order of magnitude Y of lactic acid bacteria is response, Y=lgN0/Nt, N in formula0For the initial bacterium of meat sample
Number, Nt are the remaining bacterium number of meat sample after HPCD processing, and the regression equation for establishing model indicates:
Wherein, β0: intercept；βj: slope；εi: error；I=1,2 ... n；yiFor the predicted value for having removed error amount；
Step 2 is mixed leached tea oil slag aqueous solution with extracting solution by mixing module, and progress slightly proposes processing, obtains Tea Saponin extraction
Liquid；The process conditions for slightly proposing processing are 53 DEG C of Extracting temperature, concentration of alcohol 45%, time 95min, liquid-solid ratio 10.5；
Tea saponin extract is mixed with sterols complexing agent by complexing processing module, is carried out using complexing model by step 3
Complexing processing, obtains Tea Saponin complex compound；
Each point P and its 8- neighborhood point constitute a micro- curved surface on the complexing model particle surface, according to the song of Differential Geometry
Normally face is discussed, surface parameter equation is z=z (x, y), wherein x, y are coordinate of this in image array, then at the point
Gaussian curvature K and mean curvature H are as follows:
In formula, k1And k2For the principal curvatures at the point, maximum curvature and minimum curvature are respectively indicated；P, q expression first derivative, r,
S, t indicates second dervative；
Tea Saponin complex compound is mixed with solution sequester by decomplexing separation module, carries out decomplexing separation processing, obtain by step 4
Tea Saponin；
Step 5, to Tea Saponin into purifying.
2. as described in claim 1 using biotechnology extract Tea Saponin method, which is characterized in that extracting solution be methanol,
One of ethyl alcohol, water, normal propyl alcohol, isopropanol and butanol are a variety of.
3. the method for extracting Tea Saponin using biotechnology as described in claim 1, which is characterized in that leached tea oil slag and extracting solution
Amount ratio be 1g:1mL~12mL.
4. the method for extracting Tea Saponin using biotechnology as described in claim 1, which is characterized in that slightly proposing processing includes:
It successively heated, filtered after leached tea oil slag is mixed with extracting solution, obtain tea saponin extract；The temperature of heating be 50 DEG C~
110 DEG C, the time is 1h~3h.
5. the method for extracting Tea Saponin using biotechnology as described in claim 1, which is characterized in that purification process includes:
1) amount ratio for pressing 11~15g:100mL, Tea Saponin crude product is dissolved in the alcoholic solution that volume fraction is 80%, at centrifugation
Reason, takes supernatant；
2) supernatant is placed in Soxhlet extraction flask, by Tea Saponin crude product: cholesterol=11~15:7~12 mass ratio takes
Cholesterol is wrapped with filter paper, is transferred in soxhlet extraction pipe, after being heated to reflux 6~7h of extraction, is cooled to room temperature, by extract liquor mistake
Filter, washing, obtains Tea Saponin-cholesterin complex；
3) Tea Saponin-cholesterin complex is dry to constant weight, it is wrapped, is fitted into soxhlet extraction pipe, to rope with filter paper after cooling
Extractant is added in family name's flask, is heated to reflux 5~6h of extraction and is obtained from soxhlet extraction pipe by purification process after cooling
Tea Saponin, purity are 95%~98%.
6. a kind of realize extracts tea soap using the utilization biotechnology that biotechnology extracts the method for Tea Saponin described in claim 1
Element system, which is characterized in that it is described using biotechnology extract Tea Saponin system include:
Crush module, sterilization module, mixing module, complexing processing module, decomplexing separation module, purification blocks；
Module is crushed, is connect with sterilization module, for crushing leached tea oil slag；
Sterilization module is connect with crushing module, mixing module, for being sterilized, being sterilized by the leached tea oil slag of crushing, is added pure
Aqueous solution is made in water；
Mixing module connect with sterilization module, complexing processing module, for mixing leached tea oil slag aqueous solution with extracting solution, carries out
Processing slightly is proposed, obtains tea saponin extract；
Processing module is complexed, is connect with mixing module, decomplexing separation module, is used for the tea saponin extract and sterols network
Mixture mixing, carries out complexing processing, obtains Tea Saponin complex compound；
Decomplexing separation module is connect with complexing processing module, purification blocks, is used for the Tea Saponin complex compound and solution sequester
Mixing carries out decomplexing separation processing, obtains Tea Saponin；
Purification blocks are connect with decomplexing separation module, for Tea Saponin into purifying.
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| CN112194700A (en) * | 2020-10-09 | 2021-01-08 | 张利民 | Preparation method of natural high-purity tea saponin with high decontamination efficiency |
| CN114371748A (en) * | 2021-12-15 | 2022-04-19 | 同济大学 | Greenhouse crop illumination carbon dioxide regulation and control method based on Gaussian curvature |
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| CN112194700A (en) * | 2020-10-09 | 2021-01-08 | 张利民 | Preparation method of natural high-purity tea saponin with high decontamination efficiency |
| CN114371748A (en) * | 2021-12-15 | 2022-04-19 | 同济大学 | Greenhouse crop illumination carbon dioxide regulation and control method based on Gaussian curvature |
| CN114371748B (en) * | 2021-12-15 | 2022-09-20 | 同济大学 | Greenhouse crop illumination carbon dioxide regulation and control method based on Gaussian curvature |
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Application publication date: 20181214 |