CN105801640A - Preparation method of steviosin - Google Patents
Preparation method of steviosin Download PDFInfo
- Publication number
- CN105801640A CN105801640A CN201610219006.7A CN201610219006A CN105801640A CN 105801640 A CN105801640 A CN 105801640A CN 201610219006 A CN201610219006 A CN 201610219006A CN 105801640 A CN105801640 A CN 105801640A
- Authority
- CN
- China
- Prior art keywords
- steviosin
- ethanol
- described step
- extracting
- preparation
- 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.)
- Pending
Links
Classifications
-
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Seasonings (AREA)
Abstract
The invention discloses a preparation method of steviosin. The preparation method comprises the following steps: a), early treatment; b), extraction; c), membrane filtration; d), concentration; e), adsorption; f) elution; g) secondary concentration; h) drying separation; i), separation of residual ethanol; j) secondary drying separation. The preparation process combining membrane filtration, concentration, adsorption, elution, secondary concentration and drying separation is adopted, and accordingly, the extraction purity of steviosin is greatly improved; ultrasonic assisted extraction is adopted in the steviosin extraction process, and accordingly, the extraction efficiency of steviosin is improved; the step of separation of residual ethanol is added, and the quantity of residual organic solvents in steviosin is effectively reduced.
Description
[technical field]
Technical field prepared by steviosin of the present invention, the particularly technical field of the preparation method of a kind of steviosin.
[background technology]
Steviosin is the main sweet substance of Stevia leaves, extract is crystalloid, for sweetening agent also known as stevioside, the preparation of existing steviosin is usually and adopts organic solvent to carry out extracting, owing to existing steviosin is in preparation process, simply have employed the simple vacuum drying organic solvent to remove in steviosin, therefore obtained steviosin exists organic solvent, these organic solvents are not only harmful, and these organic solvents also affect the curative effect of steviosin.
[summary of the invention]
The purpose of the present invention solves the problems of the prior art exactly, the preparation method proposing a kind of steviosin, the one-tenth production. art that the present invention combines by adopting membrane filtration, concentration, absorption, eluting, secondary concentration, dry separation, thus considerably increasing the DNA purity of steviosin；The present invention by adopting ultrasonic assistant to extract in steviosin extraction process, thus adding the extraction efficiency of steviosin；The present invention is also by increasing the step that residual ethanol separates, thus the Determination of Residual Organic Solvents being effectively reduced in steviosin.
For achieving the above object, the preparation method that the present invention proposes a kind of steviosin, it is characterised in that comprise the steps:
A) early stage processes: by Stevia leaves respectively through clean, air-dry, pulverizing, sieving, thus obtaining Folium Stevlae Rebaudianae powder；
B) extract: by the Folium Stevlae Rebaudianae powder obtained of step a), join in extraction pot, be subsequently adding cellulase and alcoholic solution carries out circumfluence distillation, thus obtaining the mixed solution of ethanol and steviosin；
C) membrane filtration: by the mixed solution of the step b) ethanol obtained and steviosin, the NF membrane first passing through 6000Dal is filtered；
D) concentration: step c) is concentrated again through the NF membrane of 1200Dal by the filtrate of 6000Dal NF membrane；
E) absorption: the concentrated solution that step d) obtains successively adsorbs through cationic, anionic exchange resin with the flow velocity of 0.3BV/h；
F) eluting: respectively with 50% ethanol (v/v) solution and 80% ethanol (v/v) solution, the steviosin of eluting cationic, anionic exchange resin absorption, thus obtaining steviosin eluent；
G) secondary concentration: the steviosin eluent obtained by step f) crosses 600Dal NF membrane thus carrying out secondary concentration；
H) dry separation: to the steviosin eluent after step g) secondary concentration, carry out vacuum drying separation, thus obtaining rough steviosin；
I) residual ethanol separates: the rough steviosin obtained by step h) rejoins in pure water, then heat temperature raising, so that the ethanol of residual dissolves in pure water in rough steviosin；
J) redrying separates；The steviosin being settled out in step i) pure water is carried out secondary vacuum and dries concentration, thus obtaining steviosin finished product.
As preferably, described step b) is when entering shape and extracting, and employing is that the mode being heated to reflux carries out extracting, and described step b) additionally uses ultrasonic assistant and extracts when entering and extracting.
As preferably, the described step b) heating-up temperature when entering shape and extracting every time is 60 DEG C-80 DEG C, and described step b) enters the ultrasound wave that auxiliary ultrasonic is 35KHZ-40KHZ when extracting entering shape every time.
As preferably, the described step b) constant temperature time when entering shape and extracting every time is 1h-2h, described step b) is when entering shape and extracting every time, adding 6-7 times that weight is Folium Stevlae Rebaudianae powder weight of ethanol, the alcoholic solution that described step b) adds is 90% ethanol (v/v) solution.
As preferably, the described step i) heating-up temperature when carrying out residual ethanol and separating is 50 DEG C-60 DEG C, constant temperature persistent period 0.5h-1h, and described step i) also uses ultrasonic assistant when carrying out residual ethanol and separating and dissolves.
As preferably, the ultrasound wave that auxiliary ultrasonic is 35KHZ-40KHZ that described step i) adopts when carrying out residual ethanol and separating, described step i) to step j) can repetitive operation, until making the ethanol in steviosin be totally separated.
[detailed description of the invention]
The preparation method of a kind of steviosin of the present invention, it is characterised in that comprise the steps: that a) early stage processes: by Stevia leaves respectively through clean, air-dry, pulverizing, sieving, thus obtaining Folium Stevlae Rebaudianae powder；B) extract: by the Folium Stevlae Rebaudianae powder obtained of step a), join in extraction pot, be subsequently adding cellulase and alcoholic solution carries out circumfluence distillation, thus obtaining the mixed solution of ethanol and steviosin；C) membrane filtration: by the mixed solution of the step b) ethanol obtained and steviosin, the NF membrane first passing through 6000Dal is filtered；D) concentration: step c) is concentrated again through the NF membrane of 1200Dal by the filtrate of 6000Dal NF membrane；E) absorption: the concentrated solution that step d) obtains successively adsorbs through cationic, anionic exchange resin with the flow velocity of 0.3BV/h；F) eluting: respectively with 50% ethanol (v/v) solution and 80% ethanol (v/v) solution, the steviosin of eluting cationic, anionic exchange resin absorption, thus obtaining steviosin eluent；G) secondary concentration: the steviosin eluent obtained by step f) crosses 600Dal NF membrane thus carrying out secondary concentration；H) dry separation: to the steviosin eluent after step g) secondary concentration, carry out vacuum drying separation, thus obtaining rough steviosin；I) residual ethanol separates: the rough steviosin obtained by step h) rejoins in pure water, then heat temperature raising, so that the ethanol of residual dissolves in pure water in rough steviosin；J) redrying separates；nullThe steviosin being settled out in step i) pure water is carried out secondary vacuum and dries concentration，Thus obtaining steviosin finished product，Described step b) is when entering shape and extracting，What adopt is that the mode being heated to reflux carries out extracting，Described step b) additionally uses ultrasonic assistant and extracts when entering and extracting，The described step b) heating-up temperature when entering shape and extracting every time is 60 DEG C-80 DEG C，Described step b) enters the ultrasound wave that auxiliary ultrasonic is 35KHZ-40KHZ when extracting entering shape every time，The described step b) constant temperature time when entering shape and extracting every time is 1h-2h，Described step b) is when entering shape and extracting every time，Add 6-7 times that weight is Folium Stevlae Rebaudianae powder weight of ethanol，The alcoholic solution that described step b) adds is 90% ethanol (v/v) solution，The described step i) heating-up temperature when carrying out residual ethanol and separating is 50 DEG C-60 DEG C，Constant temperature persistent period 0.5h-1h，Described step i) also uses ultrasonic assistant when carrying out residual ethanol and separating and dissolves，The ultrasound wave that auxiliary ultrasonic is 35KHZ-40KHZ that described step i) adopts when carrying out residual ethanol and separating，Described step i) can repetitive operation to step j)，Until making the ethanol in steviosin be totally separated.
The one-tenth production. art that the present invention combines by adopting membrane filtration, concentration, absorption, eluting, secondary concentration, dry separation, thus considerably increasing the DNA purity of steviosin；The present invention by adopting ultrasonic assistant to extract in steviosin extraction process, thus adding the extraction efficiency of steviosin；The present invention is also by increasing the step that residual ethanol separates, thus the Determination of Residual Organic Solvents being effectively reduced in steviosin.
Above-described embodiment is the description of the invention, is not limitation of the invention, any scheme after simple transformation of the present invention is belonged to protection scope of the present invention.
Claims (6)
1. the preparation method of a steviosin, it is characterised in that comprise the steps:
A) early stage processes: by Stevia leaves respectively through clean, air-dry, pulverizing, sieving, thus obtaining Folium Stevlae Rebaudianae powder；
B) extract: by the Folium Stevlae Rebaudianae powder obtained of step a), join in extraction pot, be subsequently adding cellulase and alcoholic solution carries out circumfluence distillation, thus obtaining the mixed solution of ethanol and steviosin；
C) membrane filtration: by the mixed solution of the step b) ethanol obtained and steviosin, the NF membrane first passing through 6000Dal is filtered；
D) concentration: step c) is concentrated again through the NF membrane of 1200Dal by the filtrate of 6000Dal NF membrane；
E) absorption: the concentrated solution that step d) obtains successively adsorbs through cationic, anionic exchange resin with the flow velocity of 0.3BV/h；
F) eluting: respectively with 50% ethanol (v/v) solution and 80% ethanol (v/v) solution, the steviosin of eluting cationic, anionic exchange resin absorption, thus obtaining steviosin eluent；
G) secondary concentration: the steviosin eluent obtained by step f) crosses 600Dal NF membrane thus carrying out secondary concentration；
H) dry separation: to the steviosin eluent after step g) secondary concentration, carry out vacuum drying separation, thus obtaining rough steviosin；
I) residual ethanol separates: the rough steviosin obtained by step h) rejoins in pure water, then heat temperature raising, so that the ethanol of residual dissolves in pure water in rough steviosin；
J) redrying separates；The steviosin being settled out in step i) pure water is carried out secondary vacuum and dries concentration, thus obtaining steviosin finished product.
2. the preparation method of a kind of steviosin as claimed in claim 1, it is characterised in that: described step b) is when entering shape and extracting, and employing is that the mode being heated to reflux carries out extracting, and described step b) additionally uses ultrasonic assistant and extracts when entering and extracting.
3. the preparation method of a kind of steviosin as claimed in claim 1, it is characterized in that: the described step b) heating-up temperature when entering shape and extracting every time is 60 DEG C-80 DEG C, described step b) enters the ultrasound wave that auxiliary ultrasonic is 35KHZ-40KHZ when extracting entering shape every time.
4. the preparation method of a kind of steviosin as claimed in claim 1, it is characterized in that: the described step b) constant temperature time when entering shape and extracting every time is 1h-2h, described step b) is when entering shape and extracting every time, adding 6-7 times that weight is Folium Stevlae Rebaudianae powder weight of ethanol, the alcoholic solution that described step b) adds is 90% ethanol (v/v) solution.
5. the preparation method of a kind of steviosin as claimed in claim 1, it is characterized in that: the described step i) heating-up temperature when carrying out residual ethanol and separating is 50 DEG C-60 DEG C, constant temperature persistent period 0.5h-1h, described step i) also use ultrasonic assistant when carrying out residual ethanol and separating and dissolve.
6. the preparation method of a kind of steviosin as claimed in claim 1, it is characterized in that: the ultrasound wave that auxiliary ultrasonic is 35KHZ-40KHZ that described step i) adopts when carrying out residual ethanol and separating, described step i) to step j) can repetitive operation, until making the ethanol in steviosin be totally separated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610219006.7A CN105801640A (en) | 2016-04-08 | 2016-04-08 | Preparation method of steviosin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610219006.7A CN105801640A (en) | 2016-04-08 | 2016-04-08 | Preparation method of steviosin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105801640A true CN105801640A (en) | 2016-07-27 |
Family
ID=56460237
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610219006.7A Pending CN105801640A (en) | 2016-04-08 | 2016-04-08 | Preparation method of steviosin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105801640A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108047286A (en) * | 2017-12-12 | 2018-05-18 | 蚌埠市华东生物科技有限公司 | A kind of method that steviol glycoside is extracted from STEVIA REBAUDIANA |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286040A (en) * | 2011-08-09 | 2011-12-21 | 山东千千药业有限公司 | Refining method of high-purity steviosin |
| CN103408614A (en) * | 2013-07-31 | 2013-11-27 | 李玉山 | Novel preparation technique of steviosin and Rebaudioside-A |
-
2016
- 2016-04-08 CN CN201610219006.7A patent/CN105801640A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286040A (en) * | 2011-08-09 | 2011-12-21 | 山东千千药业有限公司 | Refining method of high-purity steviosin |
| CN103408614A (en) * | 2013-07-31 | 2013-11-27 | 李玉山 | Novel preparation technique of steviosin and Rebaudioside-A |
Non-Patent Citations (3)
| Title |
|---|
| 付娟娟等: "超声波辅助纤维素酶提取甜菊糖苷", 《中国食品添加剂》 * |
| 凌立新等: "甜叶菊中甜菊素提取工艺研究", 《食品工业科技》 * |
| 姚国新等: "膜技术在提取甜菊糖中的应用", 《食品研究与开发》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108047286A (en) * | 2017-12-12 | 2018-05-18 | 蚌埠市华东生物科技有限公司 | A kind of method that steviol glycoside is extracted from STEVIA REBAUDIANA |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104558088A (en) | Method for extracting mogroside V from momordica grosvenori | |
| CN102351956B (en) | Extraction method of morindea officinalis polysaccharide | |
| CN101829210B (en) | Method for preparing apple polyphenol | |
| CN103588742A (en) | Method for extracting rose flavone from rose residue solution | |
| CN106046194A (en) | Extraction method of dendrobium huoshanense polysaccharide | |
| CN104069151B (en) | A kind of high method for preparing extractive of content of mogroside IV | |
| CN106045959B (en) | A kind of method that glucosidase procyanidins are prepared using grape seed extract | |
| CN105859675A (en) | Preparation method of high-purity anthocyanins by extracting from roselle | |
| EP3505525B1 (en) | Method for preparing rubusoside | |
| CN110818585A (en) | Separation method for simultaneously preparing five dopamine compounds from aspongopus | |
| CN105801640A (en) | Preparation method of steviosin | |
| CN105062129A (en) | Method for extracting anthocyanins from mulberries | |
| CN105061281B (en) | A kind of method that ultrasonic wave added counter-current extraction extracts carrotene | |
| CN102060706A (en) | Method for extracting and purifying cichoric acid from Echinacea purpurea | |
| CN104825510B (en) | A kind of method of embrane method extraction radix rauvolfia total alkaloids | |
| CN108299542B (en) | Method for comprehensively extracting saponin and polyphenol from camellia oleifera abel cake | |
| CN112353832B (en) | A method for separating active components from radix Adenophorae | |
| CN103271973A (en) | Method for extracting total triterpenoid substances from cornel | |
| WO2017185281A1 (en) | Fritillary flower extractive preparation method | |
| CN106946833A (en) | A kind of method that high-purity sinensetin is extracted from Mao Xu Cao | |
| CN103044253A (en) | Extraction separation method of rosmarinic acid in salvia castabea diels f. tomentosa stib | |
| CN103288898B (en) | Neomangiferin reference substance extracts method for purifying and separating | |
| CN107353296B (en) | A method of extracting activated protein and eurycomanone from Tongkat Ali | |
| CN104876986A (en) | Method for extracting anthocyanin in purple sweet potato | |
| CN106565813B (en) | The processing method that a kind of Tea Saponin continuously purifies |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160727 |
|
| RJ01 | Rejection of invention patent application after publication |