CN108003215A - The cleaning extracting method of Tea Saponin - Google Patents
The cleaning extracting method of Tea Saponin Download PDFInfo
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- CN108003215A CN108003215A CN201711423969.XA CN201711423969A CN108003215A CN 108003215 A CN108003215 A CN 108003215A CN 201711423969 A CN201711423969 A CN 201711423969A CN 108003215 A CN108003215 A CN 108003215A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/58—Multistep processes
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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 present invention provides the cleaning extracting method of Tea Saponin, step includes：1) cake of camellia oleifera seeds is crushed, sieved, fineness is 200~400 mesh；2) cake of camellia oleifera seeds powder is taken, by solid-liquid ratio 1：2~3 add n-hexane, are heated to 60~70 DEG C, carry out reflux 1~3h ungrease treatments, be then dried；3) extracting degreasing cake of camellia oleifera seeds powder, by solid-liquid ratio 1：15~25 add ethanol, are heated to 50~70 DEG C, carry out ultrasonic-microwave collaboration extraction；4) solution after extraction is filtered, centrifugation, tea saponin extract is made；5) extracting solution is dried, Tea Saponin crude product is made；6) ultrafiltration membrance filter and organic nanofiltration membrane filtering are carried out after Tea Saponin crude product is dissolved successively, is then dried, high-purity tea saponin is made.The present invention improves raw material availability, improves the recovery rate of Tea Saponin to a greater extent, shortens extraction time, compared with traditional separation process, have the advantages that energy consumption is low, single-stage separative efficiency is high, equipment simply, without phase-change, it is pollution-free.
Description
Technical field
The invention belongs to versatile chemical industry and medical material field, and in particular to a kind of cleaning extraction of Tea Saponin
Method.
Background technology
China is world's tea-oil tree yield highest, and cultivated area is maximum, the most abundant country of kind, be mainly distributed on Hunan,
Hubei, Guangdong, Guangxi, Fujian, Jiangxi etc. save.Existing oil tea area 40000km2 in China or so, according to incompletely statistics, the whole nation are every
Produce tea seed about 650kt per year, the tea seed cake after oil expression was used as fuel or fertilizer more, and also had and abandoned as discarded object in more than 400kt, past
Fall.The main component of tea seed cake is to remain tea oil 5% -8%, Tea Saponin about 10.6%, protein about 10.2%.Tea Saponin is again
Name tea saponin, is a kind of natural nonionic surface active agent, is made of seven kinds of aglucons, four kinds of sugared bodies and two kinds of organic carboxyl acids
A kind of pentacyclic triterpene saponins, can be widely used for light industry, chemical industry, pesticide, feed, cultivation, weaving, oil recovery, mining, building materials and height
The fields such as fast highway construction, manufacture emulsifying agent, abluent, insecticides adjuvant, feed addictive, crab shrimp aquaculture protective agent, weaving help
Agent, oilfield foaming agent, mining flotation agent and air entrained concrete foam stabilizer and concrete admixture, antifreezing agent etc..
Foreign scholar is more early to Tea Saponin research, and early in earlier 1900s, Weil and Hal-berkann have been begun to tea
The research of saponin each side.Newly secondary Lang Shouci has isolated Tea Saponin and has named tea seed in Japanese scholars green hill in 1931 from tea seed
Saponin " Teasaponin ", this is the Tea Saponin for separating acquisition first in the world, but obtained is not also the pure crystallization of Tea Saponin,
So far has more than 70 years history.Nineteen fifty-two Tokyo Univ Japan scholar stone shop keep three and upper Tianyang County just isolate the pure knot of Tea Saponin
It is brilliant.Foreign countries' saponin product mainly has the thea saponin of Japanese Ju Chu oilings Co., Ltd. production and refined thea saponin at present, also
There is white saponin (Saponin white) of German E.Merk companies production etc..
Although oil tea is the specialty in China, from the point of view of domestic research conditions, the research to Tea Saponin is started late, China
The water extraction that just begins one's study in the 1950s extracts Tea Saponin, and having arrived twentieth century just has larger progress the eighties, opens
Beginning realizes industrialized production.In recent years, production and application study of the various regions to Tea Saponin is increasingly paid attention to, it is proposed that different works
Industry production method, also conducts in-depth research in refined and application aspect.Industrialized production Tea Saponin in China's is mainly adopted at present
Extracted with organic solvent extraction or water, although water extraction cost is low, easy to operate, extraction time length, the Tea Saponin Yishui River
Solution, concentration are more difficult, obtained Tea Saponin product colour compared with it is deep, impurity is more, subsequent purification is more difficult；What alcohol extracting method obtained
Product quality is higher, color is shallower, yield is higher, but there are safety problem, extraction time are also long.Tea Saponin purifying side
Face, UF membrane, macroreticular resin are common Tea Saponin purification process, and although both approaches obtain product quality higher, still
Product yield is relatively low and equipment and raw material input are more, and film and resin utilization rate are low, easily cause blocking, and follow-up work is more multiple
It is miscellaneous；Extraction purifies long flow path, and consumption organic reagent is more, and yield is low；It is higher that silica gel column chromatography obtains Tea Saponin product purity,
But yield is very low, it is suitable only for laboratory and produces on a small quantity.Therefore, Tea Saponin extraction, purification process to having in the industry
Break through, it is necessary to the high method of the product quality for finding a kind of short, easy to operate, the efficient low energy of technological process and obtaining.
The content of the invention
The object of the present invention is to provide a kind of cleaning extracting method of saponin, realizes that technological process is short, easy to operate, efficient
Low energy and obtained product quality height.
To achieve these goals, the present invention provides the cleaning extracting method of Tea Saponin, step to include：
1) cake of camellia oleifera seeds is crushed, sieved, fineness is 200~400 mesh；
2) cake of camellia oleifera seeds powder is taken, by solid-liquid ratio 1：2~3 add n-hexanes, be heated to 60~70 DEG C, carry out reflux 1~
3h ungrease treatments, are then dried；
3) extracting degreasing cake of camellia oleifera seeds powder, by solid-liquid ratio 1：15~25 add ethanol, are heated to 50~70 DEG C, are surpassed
Sound-microwave cooperating extraction；
4) solution after extraction is filtered, centrifugation, tea saponin extract is made；
5) extracting solution is dried, Tea Saponin crude product is made；
6) ultrafiltration membrance filter and organic nanofiltration membrane filtering are carried out after Tea Saponin crude product is dissolved successively, is then done
It is dry, high-purity tea saponin is made.
Preferred solution is：In step 1 cake of camellia oleifera seeds is crushed with micronizer.
Preferred solution is：Step 1 with distilled water cleans cake of camellia oleifera seeds surface before crushing.
Preferred solution is：The ethanol solution that concentration is 75% is added in step 3.
Preferred solution is：In step 3,15~25KHz of supersonic frequency, ultrasonic power 300W~500W, microwave power 200~
500W, 10~30min of extraction time.
Preferred solution is：The extracting solution of Tea Saponin is concentrated by evaporation under 0.5~0.9MPa of vacuum, vacuum drying is made
Tea Saponin crude product.
Preferred solution is：Step 6 concretely comprises the following steps：
1) Tea Saponin crude product is dissolved with pure water, is configured to aqueous solution；
2) aqueous solution is subjected to hyperfiltration membrane assembly filtering, during filtering, adds water repeatedly, until solid-liquid ratio is 1：10
~15, operating pressure is 0.05~0.1MPa, and operation temperature is less than 45 DEG C；
3) filtrate after the filtering of above-mentioned hyperfiltration membrane assembly is subjected to organic nanofiltration membrane filtering, organic nanofiltration membrane retention point
Son amount is 1000Da, and operating pressure is 0.5~0.8MPa, and operation temperature is 25~40 DEG C；
4) will filtering after solution using spray dryer dry, inlet air temperature be 180~200 DEG C, leaving air temp be 100~
110 DEG C, sample introduction flow velocity is 20~40ml/min.
Preferred solution is：The hyperfiltration membrane assembly is followed successively by polyvinylidene fluoride microporous filtering film, hollow-fibre membrane and ceramic membrane, institute
Polyvinylidene fluoride microporous filtering film 0.3~0.5mm of wall thickness is stated, molecular cut off is 5~100,000 dalton, and aperture is 0.1~1.0um；
0.2~0.4mm of the hollow-fibre membrane wall thickness, aperture are 0.05~0.1um；The ceramics membrane aperture is 0.001~0.1um.
Preferred solution is：The organic nanofiltration membrane is sulfonated polysulfone membrane, sulfonated polyether sulfone film, PA membrane or polyvinyl alcohol
Film.
Preferred solution is：, the ultrasound-microwave cooperating extracting method is：
1) solution to be extracted configured is positioned in ultrasound-microwave reaction kettle；
2) ultrasonic gatherer is controlled to open, 15~20KHz of supersonic frequency, ultrasonic power 300W~400W, ultrasonic time
For 5~10min；
3) microwave introduction device is controlled to open, 200~300W of microwave power, the microwave time is 10~15min；
4) microwave and ultrasonic gatherer is controlled to open at the same time, 20~25KHz of supersonic frequency, ultrasonic power 400W~
500W, 300~500W of microwave power, operating time are 5~10min, and the importing direction of ultrasonic wave and the importing direction of microwave begin
Whole orthogonal vertical.
The invention discloses a kind of cleaning extractive technique of Tea Saponin, using cake of camellia oleifera seeds as raw material, ultramicro grinding, after sieving
N-hexane degreasing, ethanol extracts under ultrasound-microwave cooperating processing, and extracting solution is concentrated in vacuo, and is received using combining ultrafiltration organic film
The clean technologies such as filter isolate and purify Tea Saponin, and mist drying, obtains high-purity tea saponin, reduce organic in production process
The discharge of the waste liquids such as solvent, environmental benefit are notable.The present invention uses ultrasound-microwave cooperating extraction process, makes full use of ultrasound to shake
The effect of the high energy of dynamic cavitation and microwave, improves the recovery rate of Tea Saponin, shortens extraction time, reduces and be produced into
Originally the purity of product, is improved, purity is up to more than 98.0%.The present invention extracts saponin using tea seed cake, and abundant raw material is cheap,
Not only the recycling property of tea seed cake had been improved, but also can obtain being worth higher Tea Saponin, it is contemplated that better economic benefit.Specific beneficial effect
Fruit is as follows：
1) present invention is made raw material particle size be evenly distributed, is added micro mist using superfine communication technique processing cake of camellia oleifera seeds
Specific surface area, makes dissolubility also accordingly increase, improves raw material availability；
2) present invention uses ultrasound-microwave cooperating extraction process, makes full use of the cavitation and microwave of ultrasonic vibration
High energy acts on, and improves the recovery rate of Tea Saponin to a greater extent, shortens extraction time；
3) present invention carries out ultrafiltration membrance filter and organic nanofiltration membrane filtering successively after Tea Saponin crude product is dissolved, with biography
The separation process of system is compared, have the advantages that energy consumption is low, single-stage separative efficiency is high, equipment is simple, without phase-change, it is pollution-free.
Brief description of the drawings
Fig. 1 is the FB(flow block) of the embodiment of the present invention 1.
Embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings, to make those skilled in the art with reference to specification text
Word can be implemented according to this.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of a other elements or its combination.
Embodiment 1
The present embodiment is the cleaning extracting method for providing Tea Saponin, and step includes：
1) debris such as cake of camellia oleifera seeds surface flying dust are cleaned with distilled water, drying to constant weight at a temperature of 50 DEG C by it, so
Cake of camellia oleifera seeds is crushed with micronizer afterwards, sieving, fineness is 200 mesh；
2) cake of camellia oleifera seeds powder is taken, by solid-liquid ratio 1：2 add n-hexane, are heated to 60 DEG C, carry out reflux 1h ungrease treatments,
Then it is dried；
3) extracting degreasing cake of camellia oleifera seeds powder, by solid-liquid ratio 1：15 add the ethanol that concentration is 75%, are heated to 50 DEG C, carry out
Ultrasound-microwave cooperating extraction, supersonic frequency 15KHz, ultrasonic power 300W, microwave power 200W, extraction time 10min；
4) solution after extraction is filtered, centrifugation, tea saponin extract is made；
5) extracting solution of Tea Saponin is concentrated by evaporation under vacuum 0.5MPa, is dried in vacuo and Tea Saponin crude product is made；
6) ultrafiltration membrance filter and organic nanofiltration membrane filtering are carried out after Tea Saponin crude product is dissolved successively, is then done
It is dry, high-purity tea saponin is made, concretely comprises the following steps：A) Tea Saponin crude product is dissolved with pure water, is configured to aqueous solution；B) by aqueous solution
Hyperfiltration membrane assembly filtering is carried out, during filtering, adds water repeatedly, until solid-liquid ratio is 1：10, operating pressure is
0.05MPa, operation temperature are less than 45 DEG C；C) filtrate after the filtering of above-mentioned hyperfiltration membrane assembly is subjected to organic nanofiltration membrane mistake
Filter, organic nanofiltration membrane molecular cut off are 1000Da, and operating pressure 0.5MPa, operation temperature is 25 DEG C；D) it is molten after filtering
Liquid is dried using spray dryer, and inlet air temperature is 180 DEG C, and leaving air temp is 100 DEG C, and sample introduction flow velocity is 20ml/min, described
Hyperfiltration membrane assembly is followed successively by polyvinylidene fluoride microporous filtering film, hollow-fibre membrane and ceramic membrane, the polyvinylidene fluoride microporous filtering film wall thickness
0.3mm, molecular cut off are 50,000 dalton, aperture 0.1um；The hollow-fibre membrane wall thickness 0.2mm, aperture 0.05um；
The ceramics membrane aperture is 0.001um, and the organic nanofiltration membrane is sulfonated polysulfone membrane, sulfonated polyether sulfone film, PA membrane or poly-
Vinyl alcohol film.The recovery rate of the present embodiment Tea Saponin is 18.25%, and purity is up to 88.34%.
Embodiment 2
The present embodiment is the cleaning extracting method for providing Tea Saponin, and step includes：
1) debris such as cake of camellia oleifera seeds surface flying dust are cleaned with distilled water, drying to constant weight at a temperature of 60 DEG C by it, so
Cake of camellia oleifera seeds is crushed with micronizer afterwards, sieving, fineness is 400 mesh；
2) cake of camellia oleifera seeds powder is taken, by solid-liquid ratio 1：3 add n-hexane, are heated to 70 DEG C, carry out reflux 3h ungrease treatments,
Then it is dried；
3) extracting degreasing cake of camellia oleifera seeds powder, by solid-liquid ratio 1：25 add the ethanol that concentration is 75%, are heated to 70 DEG C, carry out
Ultrasound-microwave cooperating extraction, the ultrasound-microwave cooperating extracting method are：A) solution to be extracted configured is positioned over
In ultrasound-microwave reaction kettle；B) ultrasonic gatherer is controlled to open, supersonic frequency 20KHz, ultrasonic power 400W, ultrasonic time
For 10min；C) microwave introduction device is controlled to open, microwave power 300W, the microwave time is 15min；D) microwave and ultrasound are controlled
Gatherer is opened at the same time, supersonic frequency 25KHz, ultrasonic power 500W, microwave power 500W, operating time 10min, ultrasound
The importing direction of ripple and the importing direction of microwave orthogonal vertical all the time；
4) solution after extraction is filtered, centrifugation, tea saponin extract is made；
5) extracting solution of Tea Saponin is concentrated by evaporation under vacuum 0.9MPa, is dried in vacuo and Tea Saponin crude product is made；
6) ultrafiltration membrance filter and organic nanofiltration membrane filtering are carried out after Tea Saponin crude product is dissolved successively, is then done
It is dry, high-purity tea saponin is made, concretely comprises the following steps：A) Tea Saponin crude product is dissolved with pure water, is configured to aqueous solution；B) by aqueous solution
Hyperfiltration membrane assembly filtering is carried out, during filtering, adds water repeatedly, until solid-liquid ratio is 1：15, operating pressure 0.1MPa,
Operation temperature is less than 45 DEG C；C) filtrate after the filtering of above-mentioned hyperfiltration membrane assembly is subjected to organic nanofiltration membrane filtering, it is organic
Nanofiltration retaining molecular weight is 1000Da, and operating pressure 0.8MPa, operation temperature is 40 DEG C；D) solution is using spray after filtering
Mist drier is dried, and inlet air temperature is 200 DEG C, and leaving air temp is 110 DEG C, and sample introduction flow velocity is 40ml/min, the ultrafiltration membrane group
Part is followed successively by polyvinylidene fluoride microporous filtering film, hollow-fibre membrane and ceramic membrane, and the polyvinylidene fluoride microporous filtering film wall thickness 0.5mm, cuts
It is 100,000 dalton to stay molecular weight, aperture 1.0um；The hollow-fibre membrane wall thickness 0.4mm, aperture 0.1um；The ceramics
Membrane aperture is 0.1um, and the organic nanofiltration membrane is sulfonated polysulfone membrane, sulfonated polyether sulfone film, PA membrane or polyvinyl alcohol film.This
The recovery rate of embodiment Tea Saponin is 18.28%, and purity is up to 88.58%.
Embodiment 3
The present embodiment is the cleaning extracting method for providing Tea Saponin, and step includes：
1) debris such as cake of camellia oleifera seeds surface flying dust are cleaned with distilled water, drying to constant weight at a temperature of 55 DEG C by it, so
Cake of camellia oleifera seeds is crushed with micronizer afterwards, sieving, fineness is 300 mesh；
2) cake of camellia oleifera seeds powder is taken, by solid-liquid ratio 1：2.5 add n-hexane, are heated to 65 DEG C, carry out at reflux 2h degreasings
Reason, is then dried；
3) extracting degreasing cake of camellia oleifera seeds powder, by solid-liquid ratio 1：20 add the ethanol that concentration is 75%, are heated to 60 DEG C, carry out
Ultrasound-microwave cooperating extraction, the ultrasound-microwave cooperating extracting method are：A) solution to be extracted configured is positioned over
In ultrasound-microwave reaction kettle；B) ultrasonic gatherer is controlled to open, supersonic frequency 18KHz, ultrasonic power 350W, ultrasonic time
For 8min；C) microwave introduction device is controlled to open, microwave power 250W, the microwave time is 12min；D) microwave and ultrasound is controlled to lead
Enter device to open at the same time, supersonic frequency 22KHz, ultrasonic power 450W, microwave power 400W, operating time 6min, ultrasonic wave
Importing direction and microwave importing direction orthogonal vertical all the time；
4) solution after extraction is filtered, centrifugation, tea saponin extract is made；
5) extracting solution of Tea Saponin is concentrated by evaporation under vacuum 0.7MPa, is dried in vacuo and Tea Saponin crude product is made；
6) ultrafiltration membrance filter and organic nanofiltration membrane filtering are carried out after Tea Saponin crude product is dissolved successively, is then done
It is dry, high-purity tea saponin is made, concretely comprises the following steps：A) Tea Saponin crude product is dissolved with pure water, is configured to aqueous solution；B) by aqueous solution
Hyperfiltration membrane assembly filtering is carried out, during filtering, adds water repeatedly, until solid-liquid ratio is 1：12, operating pressure is
0.08MPa, operation temperature are less than 45 DEG C；C) filtrate after the filtering of above-mentioned hyperfiltration membrane assembly is subjected to organic nanofiltration membrane mistake
Filter, organic nanofiltration membrane molecular cut off are 1000Da, and operating pressure 0.7MPa, operation temperature is 30 DEG C；D) it is molten after filtering
Liquid is dried using spray dryer, and inlet air temperature is 190 DEG C, and leaving air temp is 105 DEG C, and sample introduction flow velocity is 30ml/min, described
Hyperfiltration membrane assembly is followed successively by polyvinylidene fluoride microporous filtering film, hollow-fibre membrane and ceramic membrane, the polyvinylidene fluoride microporous filtering film wall thickness
0.4mm, molecular cut off are 60,000 dalton, aperture 0.6um；The hollow-fibre membrane wall thickness 0.3mm, aperture 0.06um；
The ceramics membrane aperture is 0.008um, and the organic nanofiltration membrane is sulfonated polysulfone membrane, sulfonated polyether sulfone film, PA membrane or poly-
Vinyl alcohol film.The recovery rate of the present embodiment Tea Saponin is 18.35%, and purity is up to 88.42%.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Realize other modification, therefore under the universal limited without departing substantially from claim and equivalency range, it is of the invention and unlimited
In specific details and shown here as the legend with description.
Claims (10)
1. the cleaning extracting method of Tea Saponin, it is characterised in that step includes：
1) cake of camellia oleifera seeds is crushed, sieved, fineness is 200~400 mesh；
2) cake of camellia oleifera seeds powder is taken, by solid-liquid ratio 1：2~3 add n-hexane, are heated to 60~70 DEG C, carry out 1~3h of reflux and take off
Fat processing, is then dried；
3) extracting degreasing cake of camellia oleifera seeds powder, by solid-liquid ratio 1：15~25 add ethanol, are heated to 50~70 DEG C, carry out ultrasonic-micro-
Ripple collaboration extraction；
4) solution after extraction is filtered, centrifugation, tea saponin extract is made；
5) extracting solution is dried, Tea Saponin crude product is made；
6) ultrafiltration membrance filter and organic nanofiltration membrane filtering are carried out after Tea Saponin crude product is dissolved successively, is then dried,
High-purity tea saponin is made.
2. the cleaning extracting method of Tea Saponin according to claim 1, it is characterised in that micronizer is used in step 1
Crush cake of camellia oleifera seeds.
3. the cleaning extracting method of Tea Saponin according to claim 1, it is characterised in that step 1 uses distilled water before crushing
Clean cake of camellia oleifera seeds surface.
4. the cleaning extracting method of Tea Saponin according to claim 1, it is characterised in that concentration is added in step 3 is
75% ethanol solution.
5. the cleaning extracting method of Tea Saponin according to claim 1, it is characterised in that in step 3, supersonic frequency 15~
25KHz, ultrasonic power 300W~500W, 200~500W of microwave power, 10~30min of extraction time.
6. the cleaning extracting method of Tea Saponin according to claim 1, it is characterised in that by the extracting solution of Tea Saponin true
It is concentrated by evaporation under 0.5~0.9MPa of reciprocal of duty cycle, is dried in vacuo and Tea Saponin crude product is made.
7. the cleaning extracting method of Tea Saponin according to claim 1, it is characterised in that step 6 concretely comprises the following steps：
1) Tea Saponin crude product is dissolved with pure water, is configured to aqueous solution；
2) aqueous solution is subjected to hyperfiltration membrane assembly filtering, during filtering, adds water repeatedly, until solid-liquid ratio is 1：10~
15, operating pressure is 0.05~0.1MPa, and operation temperature is less than 45 DEG C；
3) filtrate after the filtering of above-mentioned hyperfiltration membrane assembly is subjected to organic nanofiltration membrane filtering, organic nanofiltration membrane molecular cut off
For 1000Da, operating pressure is 0.5~0.8MPa, and operation temperature is 25~40 DEG C；
4) solution is dried using spray dryer after filtering, and inlet air temperature is 180~200 DEG C, and leaving air temp is 100~110
DEG C, sample introduction flow velocity is 20~40ml/min.
8. the cleaning extracting method of Tea Saponin according to claim 7, it is characterised in that the hyperfiltration membrane assembly is followed successively by
Polyvinylidene fluoride microporous filtering film, hollow-fibre membrane and ceramic membrane, 0.3~0.5mm of the polyvinylidene fluoride microporous filtering film wall thickness, retention point
Son amount is 5~100,000 dalton, and aperture is 0.1~1.0um；0.2~0.4mm of the hollow-fibre membrane wall thickness, aperture 0.05
~0.1um；The ceramics membrane aperture is 0.001~0.1um.
9. the cleaning extracting method of Tea Saponin according to claim 7, it is characterised in that the organic nanofiltration membrane is sulfonation
PS membrane, sulfonated polyether sulfone film, PA membrane or polyvinyl alcohol film.
10. the cleaning extracting method of Tea Saponin according to claim 1, it is characterised in that the ultrasound-microwave cooperating carries
The method is taken to be：
1) solution to be extracted configured is positioned in ultrasound-microwave reaction kettle；
2) control ultrasonic gatherer to open, 15~20KHz of supersonic frequency, ultrasonic power 300W~400W, ultrasonic time for 5~
10min；
3) microwave introduction device is controlled to open, 200~300W of microwave power, the microwave time is 10~15min；
4) microwave and ultrasonic gatherer is controlled to open at the same time, 20~25KHz of supersonic frequency, ultrasonic power 400W~500W are micro-
300~500W of wave power, operating time are 5~10min, and the importing direction of ultrasonic wave and the importing direction of microwave are orthogonal all the time vertical
Directly.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109627280A (en) * | 2019-01-18 | 2019-04-16 | 宜春学院 | A kind of extracting method of Tea Saponin |
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| CN110483591A (en) * | 2019-08-28 | 2019-11-22 | 中国科学院青岛生物能源与过程研究所 | A method of combination embrane method refined theasapogenin |
| CN110483610A (en) * | 2019-08-28 | 2019-11-22 | 中国科学院青岛生物能源与过程研究所 | A kind of refining methd of high-purity tea saponin |
| CN110483590A (en) * | 2019-08-28 | 2019-11-22 | 中国科学院青岛生物能源与过程研究所 | A kind of method of Tea Saponin green purification |
| CN111018939A (en) * | 2019-12-16 | 2020-04-17 | 中国科学院青岛生物能源与过程研究所 | Rapid refining method of tea saponin |
| CN111592578A (en) * | 2020-05-29 | 2020-08-28 | 信阳师范学院 | Process for extracting tea saponin from camellia sinensis dregs and application of tea saponin in amino acid facial soap |
| CN112741117A (en) * | 2021-01-26 | 2021-05-04 | 广东派特埃尔生物科技有限公司 | Preparation method of herbal antibacterial disinfectant |
| CN113018896A (en) * | 2021-03-03 | 2021-06-25 | 北京林业大学 | Natural saponin decoloring method |
| CN113527403A (en) * | 2021-07-31 | 2021-10-22 | 海南黎草纪新生物科技有限公司 | Extraction method for camellia saponin |
| CN115322241A (en) * | 2022-08-11 | 2022-11-11 | 广西大学 | Method for extracting tea saponin from oil-tea camellia meal |
| CN115715891A (en) * | 2022-11-11 | 2023-02-28 | 湖南绿蔓生物科技股份有限公司 | Continuous method for separating multiple effective components from fructus Siraitiae Grosvenorii |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109627280B (en) * | 2019-01-18 | 2021-05-11 | 宜春学院 | Extraction method of tea saponin |
| CN109627280A (en) * | 2019-01-18 | 2019-04-16 | 宜春学院 | A kind of extracting method of Tea Saponin |
| CN110092810A (en) * | 2019-05-30 | 2019-08-06 | 中国科学院青岛生物能源与过程研究所 | A kind of Tea Saponin Hydrolysis kinetics method |
| CN110483591A (en) * | 2019-08-28 | 2019-11-22 | 中国科学院青岛生物能源与过程研究所 | A method of combination embrane method refined theasapogenin |
| CN110483610A (en) * | 2019-08-28 | 2019-11-22 | 中国科学院青岛生物能源与过程研究所 | A kind of refining methd of high-purity tea saponin |
| CN110483590A (en) * | 2019-08-28 | 2019-11-22 | 中国科学院青岛生物能源与过程研究所 | A kind of method of Tea Saponin green purification |
| CN110483591B (en) * | 2019-08-28 | 2022-02-15 | 中国科学院青岛生物能源与过程研究所 | Method for refining tea saponin by combined membrane method |
| CN110483590B (en) * | 2019-08-28 | 2021-10-01 | 中国科学院青岛生物能源与过程研究所 | Green refining method of tea saponin |
| CN111018939A (en) * | 2019-12-16 | 2020-04-17 | 中国科学院青岛生物能源与过程研究所 | Rapid refining method of tea saponin |
| CN111592578B (en) * | 2020-05-29 | 2021-11-19 | 信阳师范学院 | Process for extracting tea saponin from camellia sinensis dregs and application of tea saponin in amino acid facial soap |
| CN111592578A (en) * | 2020-05-29 | 2020-08-28 | 信阳师范学院 | Process for extracting tea saponin from camellia sinensis dregs and application of tea saponin in amino acid facial soap |
| CN112741117A (en) * | 2021-01-26 | 2021-05-04 | 广东派特埃尔生物科技有限公司 | Preparation method of herbal antibacterial disinfectant |
| CN112741117B (en) * | 2021-01-26 | 2022-01-25 | 广东派特埃尔生物科技有限公司 | Preparation method of herbal antibacterial disinfectant |
| CN113018896A (en) * | 2021-03-03 | 2021-06-25 | 北京林业大学 | Natural saponin decoloring method |
| CN113018896B (en) * | 2021-03-03 | 2022-08-26 | 北京林业大学 | Natural saponin decoloring method |
| CN113527403A (en) * | 2021-07-31 | 2021-10-22 | 海南黎草纪新生物科技有限公司 | Extraction method for camellia saponin |
| CN113527403B (en) * | 2021-07-31 | 2022-08-30 | 海南黎草纪新生物科技有限公司 | Extraction method for camellia saponin |
| CN115322241A (en) * | 2022-08-11 | 2022-11-11 | 广西大学 | Method for extracting tea saponin from oil-tea camellia meal |
| CN115322241B (en) * | 2022-08-11 | 2023-12-05 | 广西大学 | Method for extracting tea saponin from oil tea meal |
| CN115715891A (en) * | 2022-11-11 | 2023-02-28 | 湖南绿蔓生物科技股份有限公司 | Continuous method for separating multiple effective components from fructus Siraitiae Grosvenorii |
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