CN110437299A - A kind of extracting method of Tea Saponin - Google Patents
A kind of extracting method of Tea Saponin Download PDFInfo
- Publication number
- CN110437299A CN110437299A CN201910615565.3A CN201910615565A CN110437299A CN 110437299 A CN110437299 A CN 110437299A CN 201910615565 A CN201910615565 A CN 201910615565A CN 110437299 A CN110437299 A CN 110437299A
- Authority
- CN
- China
- Prior art keywords
- seed cake
- tea
- tea seed
- tea saponin
- extracting method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Steroid Compounds (AREA)
Abstract
The invention discloses a kind of extracting methods of Tea Saponin, are related to Tea Saponin extractive technique field, comprising the following steps: crush tea seed cake, be sieved, petroleum ether is added thereto, stir, centrifuge separation obtains degreasing tea seed cake；It is passed through vapor into degreasing tea seed cake, seals, then takes out wet tea seed cake, freezing, defrosting processing obtain pretreatment tea seed cake；Pretreatment tea seed cake is placed in percolator, 70~80% ethanol solutions dipping is added, then carries out diacolation processing, collects percolate；Ethyl alcohol is recovered under reduced pressure in percolate, adds water, adjusts pH to 9.0~10.0, is stood, filtering obtains refining liquid；Into refining liquid be added dropwise hydrochloric acid solution to pH be 2~3, filter, washing, then with 95% ethanol solution dissolve, be added dropwise acetone, stand, filtering, drying to get.Operation of the present invention is simple, and obtained Tea Saponin is of light color, recovery rate is high and with high purity, to improve the practical application value of Tea Saponin.
Description
Technical field
The present invention relates to Tea Saponin extractive technique field more particularly to a kind of extracting methods of Tea Saponin.
Background technique
Tea Saponin also known as tea saponin are a kind of glycoside compounds by extracting in tea tree seed, are that a kind of performance is good
Good natural surfactant, it can be widely applied to light industry, chemical industry, pesticide, feed, cultivation, weaving, oil recovery, mining, building materials
It abluent, insecticides adjuvant, feed addictive, crab shrimp aquaculture protective agent, is spun with fields, manufacture emulsifiers such as expressway constructions
Knit auxiliary agent, oilfield foaming agent, mining flotation agent and air entrained concrete foam stabilizer and concrete admixture --- antifreezing agent etc..
The method for extracting Tea Saponin both at home and abroad at present mainly has water seaoning and organic solvent method and promotes on this basis
The new method to come.The shortcomings that water seaoning is that Tea Saponin yield and purity are low, limits Tea Saponin application range.Organic solvent method is normal
Use aqueous methanol or hydrous ethanol as digestion agent, since methanol is at high cost and toxic, ethyl alcohol multi-purpose greatly is extracted, but uses second
Alcohol is that the used time is short, but its purity is high not enough there are the advantages of this method, and it is still necessary to further increase for yield and purity.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of extracting method of Tea Saponin, extraction is obtained
Tea Saponin is of light color, recovery rate is high and with high purity, it is easy to operate.
A kind of extracting method of Tea Saponin proposed by the present invention, comprising the following steps:
S1, tea seed cake is crushed, is sieved, petroleum ether is added thereto, stirred, centrifuge separation obtains degreasing tea seed cake；
S2, it is passed through vapor into degreasing tea seed cake, sealed, then take out wet tea seed cake, freezing, defrosting processing obtain
Pre-process tea seed cake；
S3, pretreatment tea seed cake is placed in percolator, 70~80% ethanol solutions dipping is added, then carries out at diacolation
Reason collects percolate；
S4, ethyl alcohol is recovered under reduced pressure in percolate, adds water, adjust pH to 9.0~10.0, stood, filtering obtains refining liquid；
S5, into refining liquid be added dropwise hydrochloric acid solution to pH be 2~3, filter, washing, then with 95% ethanol solution dissolution,
Acetone is added dropwise, stands, filtering, it is dry to get.
Preferably, in S1, petroleum ether is added, solid-liquid ratio is 1:3~5, stirs 20~30min.
Preferably, in S2, it is passed through vapor, makes its internal gas is wet to be maintained at 20~25%, sealing keeps 20~
40min。
Preferably, in S2, freezing is 22~26h of freezing at -12~-18 DEG C.
Preferably, which is characterized in that in S2, normal temperature unfreezing.
Preferably, in S2, repeated freezing-defrosting is operated 1~3 time.
Preferably, in S3,70~80% ethanol solutions is added and impregnate 30~40min, it is then molten using 70~80% ethyl alcohol
Liquid carries out diacolation processing, and the total amount of diacolation ethanol solution is 4~5 times of tea seed cake initial weight, at the beginning of diacolation speed is every 1000g
Beginning tea seed cake flows out 3~5mL percolate per minute.
Preferably, in S4,7~10 times of water is added, stands 5~8h.
Preferably, in S5, into refining liquid, the hydrochloric acid solution of dropwise addition 20~30% is 2~3 to pH, is filtered, with anhydrous second
Alcohol washing.
The utility model has the advantages that the invention proposes a kind of extracting methods of Tea Saponin, grease first remaining using petroleum ether removal,
Vapor is passed through into tea seed cake again, sealing is kept, and improves moisture content in tea seed cake, and the moisture in chilled rear cell is frozen into solid
Body, volume increase, and cell wall is made to swell, then the elasticity of cell wall reduces after thawing, the cell through the pretreated tea seed cake
Wall sporoderm-broken rate is high, to improve the recovery rate of Tea Saponin；The Tea Saponin in tea seed cake can be effectively extracted using percolation, and
Without heating and refluxing extraction, improve safety problem caused by ethyl alcohol heating volatilization；Again by add water water is heavy, hydrochloric acid purification is added dropwise,
Ethyl alcohol dissolution, be added dropwise acetone purification and etc., remove tea saponin extract in most of impurity.Operation of the present invention is simple, obtains
The Tea Saponin arrived is of light color, recovery rate is high and with high purity, to improve the practical application value of Tea Saponin.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of extracting method of Tea Saponin proposed by the present invention, comprising the following steps:
S1, tea seed cake is crushed, is sieved, petroleum ether is added thereto, solid-liquid ratio 1:3 stirs 20min, and centrifuge separation obtains
Degreasing tea seed cake；
S2, it is passed through vapor into degreasing tea seed cake, makes its internal gas is wet to be maintained at 20%, sealing keeps 20min, so
Wet tea seed cake is taken out afterwards, 22h is freezed at -12 DEG C, is then thawed at normal temperature, repeated freezing-defrosting operates 1 time, obtains
Pre-process tea seed cake；
S3, pretreatment tea seed cake is placed in percolator, 70% ethanol solution is added and impregnates 30min, then uses 70% second
Alcoholic solution carries out diacolation processing, and the total amount of diacolation ethanol solution is 4 times of tea seed cake initial weight, and diacolation speed is every 1000g
Initial tea seed cake flows out 3mL percolate per minute, collects percolate；
S4, ethyl alcohol is recovered under reduced pressure in percolate, adds 7 times of water, adjust pH to 9.0, stirring stands 5h, and filtering obtains smart mention
Liquid；
S5, into refining liquid be added dropwise hydrochloric acid solution to pH be 2, stir, stand, filter, washing, it is then molten with 95% ethyl alcohol
Liquid dissolution, is added dropwise acetone, stands, filtering, it is dry to get.
Embodiment 2
A kind of extracting method of Tea Saponin proposed by the present invention, comprising the following steps:
S1, tea seed cake is crushed, is sieved, petroleum ether is added thereto, solid-liquid ratio 1:5 stirs 30min, and centrifuge separation obtains
Degreasing tea seed cake；
S2, it is passed through vapor into degreasing tea seed cake, makes its internal gas is wet to be maintained at 25%, sealing keeps 40min, so
Wet tea seed cake is taken out afterwards, 26h is freezed at -18 DEG C, is then thawed at normal temperature, repeated freezing-defrosting operates 3 times, obtains
Pre-process tea seed cake；
S3, pretreatment tea seed cake is placed in percolator, 80% ethanol solution is added and impregnates 40min, then uses 80% second
Alcoholic solution carries out diacolation processing, and the total amount of diacolation ethanol solution is 5 times of tea seed cake initial weight, and diacolation speed is every 1000g
Initial tea seed cake flows out 5mL percolate per minute, collects percolate；
S4, ethyl alcohol being recovered under reduced pressure in percolate, adds 10 times of water, adjust pH to 10.0, stirring stands 5~8h, it filters,
Obtain refining liquid；
S5, into refining liquid be added dropwise hydrochloric acid solution to pH be 3, stir, stand, filter, washing, it is then molten with 95% ethyl alcohol
Liquid dissolution, is added dropwise acetone, stands, filtering, it is dry to get.
Embodiment 3
A kind of extracting method of Tea Saponin proposed by the present invention, comprising the following steps:
S1, tea seed cake being crushed, is sieved, petroleum ether is added thereto, solid-liquid ratio 1:3.5 stirs 20min, it is centrifugated,
Obtain degreasing tea seed cake；
S2, it is passed through vapor into degreasing tea seed cake, makes its internal gas is wet to be maintained at 22%, sealing keeps 25min, so
Wet tea seed cake is taken out afterwards, 23h is freezed at -14 DEG C, is then thawed at normal temperature, repeated freezing-defrosting operates 1 time, obtains
Pre-process tea seed cake；
S3, pretreatment tea seed cake is placed in percolator, 75% ethanol solution is added and impregnates 35min, then uses 75% second
Alcoholic solution carries out diacolation processing, and the total amount of diacolation ethanol solution is 4 times of tea seed cake initial weight, and diacolation speed is every 1000g
Initial tea seed cake flows out 3.5mL percolate per minute, collects percolate；
S4, ethyl alcohol is recovered under reduced pressure in percolate, adds 8 times of water, adjust pH to 9.5, stirring stands 6h, and filtering obtains smart mention
Liquid；
S5, into refining liquid be added dropwise hydrochloric acid solution to pH be 2, stir, stand, filter, washing, it is then molten with 95% ethyl alcohol
Liquid dissolution, is added dropwise acetone, stands, filtering, it is dry to get.
Embodiment 4
A kind of extracting method of Tea Saponin proposed by the present invention, comprising the following steps:
S1, tea seed cake is crushed, is sieved, petroleum ether is added thereto, solid-liquid ratio 1:4 stirs 25min, and centrifuge separation obtains
Degreasing tea seed cake；
S2, it is passed through vapor into degreasing tea seed cake, makes its internal gas is wet to be maintained at 24%, sealing keeps 30min, so
Wet tea seed cake is taken out afterwards, freezes at -16 DEG C for 24 hours, then thaws at normal temperature, repeated freezing-defrosting operates 2 times, obtains
Pre-process tea seed cake；
S3, pretreatment tea seed cake is placed in percolator, 75% ethanol solution is added and impregnates 30min, then uses 75% second
Alcoholic solution carries out diacolation processing, and the total amount of diacolation ethanol solution is 4.5 times of tea seed cake initial weight, and diacolation speed is every
The initial tea seed cake of 1000g flows out 4mL percolate per minute, collects percolate；
S4, ethyl alcohol is recovered under reduced pressure in percolate, adds 9 times of water, adjust pH to 10.0, stirring stands 5~8h, and filtering obtains
Refining liquid；
S5, into refining liquid be added dropwise hydrochloric acid solution to pH be 2.5, stir, stand, filter, washing, then with 95% ethyl alcohol
Solution dissolution, is added dropwise acetone, stands, filtering, it is dry to get.
Comparative example
Compared with Example 4, difference is only that not include step S2.
The recovery rate (%) and purity (%) of Tea Saponin in 1-4 of the embodiment of the present invention and comparative example are detected, tied
Fruit is as shown in the table:
| Group | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example |
| Recovery rate/% | 88.2 | 88.8 | 90.8 | 91.2 | 75.4 |
| Purity/% | 86.7 | 86.9 | 87.2 | 87.2 | 85.3 |
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of extracting method of Tea Saponin, which comprises the following steps:
S1, tea seed cake is crushed, is sieved, petroleum ether is added thereto, stirred, centrifuge separation obtains degreasing tea seed cake；
S2, it is passed through vapor into degreasing tea seed cake, sealed, then take out wet tea seed cake, freezing, defrosting processing obtain pre- place
Manage tea seed cake；
S3, pretreatment tea seed cake is placed in percolator, 70~80% ethanol solutions dipping is added, then carries out diacolation processing, receives
Collect percolate；
S4, ethyl alcohol is recovered under reduced pressure in percolate, adds water, adjust pH to 9.0~10.0, stood, filtering obtains refining liquid；
S5, into refining liquid be added dropwise hydrochloric acid solution to pH be 2~3, filter, washing, then with 95% ethanol solution dissolve, dropwise addition
Acetone is stood, filtering, it is dry to get.
2. the extracting method of Tea Saponin according to claim 1, which is characterized in that in S1, petroleum ether is added, solid-liquid ratio is
20~30min is stirred in 1:3~5.
3. the extracting method of Tea Saponin according to claim 1 or 2, which is characterized in that in S2, be passed through vapor, make it
Internal gas is wet to be maintained at 20~25%, and sealing keeps 20~40min.
4. the extracting method of Tea Saponin according to claim 1-3, which is characterized in that in S2, freezing is -12
22~26h is freezed at~-18 DEG C.
5. the extracting method of Tea Saponin according to claim 1-4, which is characterized in that it is characterized in that, in S2,
Normal temperature unfreezing.
6. the extracting method of Tea Saponin according to claim 1-5, which is characterized in that in S2, repeated freezing-solution
Freeze operation 1~3 time.
7. the extracting method of Tea Saponin according to claim 1-6, which is characterized in that in S3, addition 70~
80% ethanol solution impregnates 30~40min, then carries out diacolation processing, diacolation ethanol solution using 70~80% ethanol solutions
Total amount be 4~5 times of tea seed cake initial weight, diacolation speed is that the initial tea seed cake of every 1000g flows out 3~5mL percolate per minute.
8. the extracting method of Tea Saponin according to claim 1-7, which is characterized in that in S4, be added 7~10 times
Water, stand 5~8h.
9. the extracting method of Tea Saponin according to claim 1-8, which is characterized in that in S5, into refining liquid
The hydrochloric acid solution of dropwise addition 20~30% is 2~3 to pH, and filtering is washed with dehydrated alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910615565.3A CN110437299B (en) | 2019-07-09 | 2019-07-09 | Extraction method of tea saponin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910615565.3A CN110437299B (en) | 2019-07-09 | 2019-07-09 | Extraction method of tea saponin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110437299A true CN110437299A (en) | 2019-11-12 |
| CN110437299B CN110437299B (en) | 2020-09-18 |
Family
ID=68429983
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910615565.3A Active CN110437299B (en) | 2019-07-09 | 2019-07-09 | Extraction method of tea saponin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110437299B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111449090A (en) * | 2020-04-13 | 2020-07-28 | 湖南润农生态茶油有限公司 | Preparation method of tea seed cake extract |
| CN113018896A (en) * | 2021-03-03 | 2021-06-25 | 北京林业大学 | Natural saponin decoloring method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061155A (en) * | 2021-03-18 | 2021-07-02 | 广州妙思生物科技有限公司 | Method for extracting tea saponin from camellia seeds |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009057365A (en) * | 2007-08-07 | 2009-03-19 | Nippon Yakuyo Shokuhin Kenkyusho:Kk | Bowel motion-enhancing action and pancreatic lipase-inhibiting action ingredient of tea flower and its application |
| CN101817853A (en) * | 2009-03-14 | 2010-09-01 | 兰州理工大学 | Method for extracting tea saponin by adopting tea seed cake |
| CN102977162A (en) * | 2012-12-17 | 2013-03-20 | 贵州泰谷农业科技有限公司 | Method for producing high-purity tea saponin |
| CN104530173A (en) * | 2014-12-11 | 2015-04-22 | 福建华仁油脂有限公司 | Process for extracting tea saponin from oil tea cake |
| CN106309228A (en) * | 2016-09-07 | 2017-01-11 | 文山金七药业有限公司 | Toothpaste for night use and preparation method thereof |
-
2019
- 2019-07-09 CN CN201910615565.3A patent/CN110437299B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009057365A (en) * | 2007-08-07 | 2009-03-19 | Nippon Yakuyo Shokuhin Kenkyusho:Kk | Bowel motion-enhancing action and pancreatic lipase-inhibiting action ingredient of tea flower and its application |
| CN101817853A (en) * | 2009-03-14 | 2010-09-01 | 兰州理工大学 | Method for extracting tea saponin by adopting tea seed cake |
| CN102977162A (en) * | 2012-12-17 | 2013-03-20 | 贵州泰谷农业科技有限公司 | Method for producing high-purity tea saponin |
| CN104530173A (en) * | 2014-12-11 | 2015-04-22 | 福建华仁油脂有限公司 | Process for extracting tea saponin from oil tea cake |
| CN106309228A (en) * | 2016-09-07 | 2017-01-11 | 文山金七药业有限公司 | Toothpaste for night use and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111449090A (en) * | 2020-04-13 | 2020-07-28 | 湖南润农生态茶油有限公司 | Preparation method of tea seed cake extract |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110437299B (en) | 2020-09-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110437299A (en) | A kind of extracting method of Tea Saponin | |
| CN103333268A (en) | Method for preparing lycium ruthenicum polysaccharide | |
| CN108997471A (en) | A kind of environment-friendly preparation method thereof of high-purity tea saponin | |
| CN102250159A (en) | Method for extracting and preparing high-purity tannic acid from plant raw material containing tannin | |
| CN102382199B (en) | High yield energy saving preparation method of Hericium erinaceus polysaccharide | |
| CN101289364A (en) | Method for preparing and abstracting lycopene | |
| CN103466984A (en) | Sasanqua saponin concrete air entraining agent and preparation method thereof | |
| CN105753999A (en) | Method for extracting tremella polysaccharide at ultralow temperature | |
| CN108640966B (en) | Eutectic solvent for extracting tea saponin from tea seed meal and extraction process | |
| CN105903227B (en) | lavender absolute oil and preparation method thereof | |
| CN105985315A (en) | Method for extracting nicotine from tobacco waste | |
| CN104844721A (en) | Extraction and separation method of Agrocybe aegirit polysaccharides | |
| CN103788219A (en) | Method for extracting and preparing low molecular fucoidan from Ascophyllum mackaii | |
| CN106188213B (en) | A kind of Simple Purification method of Tea Saponin | |
| CN104974207B (en) | A kind of method that GP4G is extracted in the artemia cysts from salt water | |
| CN109293728A (en) | A kind of green low cost preparation method of high-purity tea saponin | |
| CN102796034B (en) | Method for preparing lutein crystal from marigold flowers | |
| CN110092810A (en) | A kind of Tea Saponin Hydrolysis kinetics method | |
| CN103451005A (en) | Method for extracting squid oil from leftovers of fresh squids | |
| CN104557953A (en) | One-step method for separating pectin, chlorophyll and tigogenin in sisal hemp pressed liquor | |
| CN208465238U (en) | A kind of resveratrol extracting system | |
| CN1348947A (en) | Prepn process of vitamin A intermediate | |
| CN107556359B (en) | Method for improving dissolution rate of water-extracted tea saponin | |
| CN103193750B (en) | Method for preparing shikimic acid and anise flavonoid by joint separation of macroporous resin XAD7HP | |
| CN104557651A (en) | Method for extracting astaxanthin from haematococcus pluvialis by double-aqueous-phase coupled wall breaking technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |