CN110627851A - Preparation method of stevioside - Google Patents
Preparation method of stevioside Download PDFInfo
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- CN110627851A CN110627851A CN201910946339.3A CN201910946339A CN110627851A CN 110627851 A CN110627851 A CN 110627851A CN 201910946339 A CN201910946339 A CN 201910946339A CN 110627851 A CN110627851 A CN 110627851A
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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
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Abstract
The invention provides a preparation method of stevioside, which comprises the following steps: sequentially crushing, leaching, carrying out chromatography, eluting, nano-filtering, desalting and spray drying on high-quality dried stevia leaves with certain mass to prepare stevioside; the invention changes the traditional production process of stevioside, saves the production cost and the production period, improves the product quality and reduces the pollution of waste water to the environment.
Description
Technical Field
The invention relates to the technical field of stevioside extraction, and particularly relates to a preparation method of stevioside.
Background
Stevia rebaudiana, also known as stevia rebaudiana and Glycyrrhiza uralensis, belongs to the family Compositae and is a evergreen shrub native to the higher plant of Paraguay, south America. Stevia rebaudiana contains 14 trace elements and 32 nutrient components, is not metabolized, accumulated, carcinogenic and toxic in the body, has the safety approved by organizations such as international FAO and WHO and American FAD, and the like, and thus is an excellent sugar source and a good nutrient source. Stevioside is an effective component in stevia rebaudiana and belongs to a natural high-power sweetener with low calorie. Research shows that stevioside has the characteristics of high sweetness, low calorie and no obvious toxic or side effect, can inhibit hyperglycemia and hypertension, and has the functions of diminishing inflammation, resisting tumors, relieving diarrhea and promoting urination and assisting immune regulation.
The traditional extraction processes of stevioside in industrial production comprise a hot water extraction method, a dialysis method, an enzyme method, a supercritical carbon dioxide extraction method, an ultrahigh pressure method, a reflux extraction method, a counter-current method and the like, but the traditional extraction processes often have the defect of low extraction rate.
For example, one existing method for preparing steviol glycosides is: soaking stevia powder in 15 times of 5% methanol water, filtering, resin exchange adsorbing, ethanol resolving, concentrating to remove alcohol, diluting, decolorizing, concentrating, and spray drying to obtain stevioside; the method has complicated process steps and increases environmental pollution.
Disclosure of Invention
The invention provides a preparation method of stevioside, which changes the traditional production process of stevioside, saves the production cost and the production period, improves the product quality and reduces the pollution of waste water to the environment.
The technical scheme adopted by the invention for solving the problems is as follows: a method for preparing stevioside comprises the following steps:
1) crushing the leaves: pulverizing the screened high-quality dried stevia rebaudiana leaves, and sieving with a 40-80 mesh sieve to obtain stevia rebaudiana powder;
2) preparing a leaching solution: soaking the stevia rebaudiana powder prepared in the step 1) in pure water with the mass of 5-7 times of that of the stevia rebaudiana powder for 2-5 hours, and filtering to obtain a leaching solution; repeating the above method for 1-2 times, mixing the leaching solutions obtained after 2-3 times of filtration, ultrafiltering, and nanofiltering to obtain concentrated leaching solution;
3) chromatography: putting the concentrated leaching liquor obtained in the step 2) into a resin chromatographic column, controlling the volume ratio of the concentrated leaching liquor to the resin chromatographic column to be 3-4: 1, and controlling the concentrated leaching liquor to carry out chromatography at a flow rate of 1.5-2 times the volume of the chromatographic column to obtain a chromatographic solution;
4) and (3) elution: eluting the chromatographic solution in the step 3) by using 1BV pure water, and eluting by using ethanol at the flow rate of 1 hour and 1.5BV column volume for 1-2 hours;
5) preparing nano filtrate: collecting the eluent in the step 4), recovering ethanol by a concentrator, and performing ultrafiltration and nanofiltration to obtain nanofiltration solution;
6) desalting: adding pure water with the volume of 1.5-2 times that of the nano filtrate into the nano filtrate prepared in the step 5, and desalting with cation exchange resin to obtain a desalted nano filtrate;
7) spray drying: and (3) further dehydrating the desalted and nanofiltration liquid prepared in the step 6) through a nanofiltration membrane, and performing spray drying when the mass concentration of nanofiltration liquid reaches 1.1-1.4mol/L to prepare stevioside.
Preferably, the temperature of the pure water in the step 2) is 40-50 ℃.
Preferably, the filtrate obtained in the step 2) is subjected to ultrafiltration by an ultrafiltration membrane with molecular weight of 15000-.
Preferably, the eluent in the step 5) is respectively subjected to ultrafiltration by an ultrafiltration membrane with a molecular weight of 8000-.
Preferably, the cation exchange resin in the step 6) is 732 or 717 ion exchange resin.
Preferably, the spray drying method in step 7) adopts centrifugal spray drying.
The invention has the beneficial effects that: the traditional production process of stevioside is changed, and the production cost and the production period are saved; the ethanol is used for resolution, so that the production cost is reduced, the pollution caused by introducing other organic solvents is avoided, the safety of stevioside production and the product quality are improved, and the pollution of waste water to the environment is reduced.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1
Pulverizing the screened high-quality dried stevia rebaudiana leaves, sieving with a 40-mesh sieve, soaking the prepared stevia rebaudiana powder in pure water at 40 ℃ for 2 hours, and filtering to obtain a leaching solution; repeating the above method for 2 times, mixing 3 times, filtering to obtain concentrated extractive solution, ultrafiltering the filtrate with ultrafiltration membrane having molecular weight of 20000, and nanofiltering with nanofiltration membrane having molecular weight of 500 to obtain concentrated extractive solution; putting the concentrated leaching liquor into a resin chromatographic column, controlling the volume ratio of the concentrated leaching liquor to the chromatographic column to be 3: 1, carrying out chromatography on the concentrated leaching liquor at the flow rate of 2BV for 1 hour, eluting with pure water after chromatography, wherein the volume ratio of the used pure water to the chromatographic column is 1: 1, and after washing, eluting with 75% ethanol at the flow rate of 1BV for 1 hour; recovering ethanol from the eluate by a concentrator, ultrafiltering with an ultrafiltration membrane having a molecular weight of 8000, and nanofiltering with a nanofiltration membrane having a molecular weight of 500 to obtain nanofiltration solution; adding pure water with the volume 2 times that of the nano filtrate into the nano filtrate, and then carrying out desalination treatment on 732 ion exchange resin; and (3) further dehydrating the desalted and nanofiltration solution through a nanofiltration membrane, and performing centrifugal spray drying when the mass concentration of the nanofiltration solution reaches 1.5 to prepare stevioside.
Example 2
Pulverizing the screened high-quality dried stevia rebaudiana leaves, sieving with a 60-mesh sieve, soaking the prepared stevia rebaudiana powder in pure water at 50 ℃ for 4 hours, and filtering to obtain a leaching solution; repeating the above method for 2 times, mixing 3 times, and filtering to obtain concentrated extractive solution; ultrafiltering the filtrate with an ultrafiltration membrane with a molecular weight of 18000, and nanofiltering with a nanofiltration membrane with a molecular weight of 400 to obtain concentrated extract; putting the concentrated leaching liquor into a resin chromatographic column, controlling the volume ratio of the concentrated leaching liquor to the chromatographic column to be 4: 1, carrying out chromatography on the concentrated leaching liquor at the flow rate of 2BV for 1 hour, eluting with pure water after the sugar liquor is finished, wherein the volume ratio of the used pure water to the chromatographic column is 1: 1, and eluting with 80% ethanol at the flow rate of 1BV for 1 hour after the washing is finished; recovering ethanol from the eluate by a concentrator, ultrafiltering with an ultrafiltration membrane having a molecular weight of 10000, and nanofiltering with a nanofiltration membrane having a molecular weight of 400 to obtain nanofiltration solution; adding pure water with the volume 2 times that of the nano filtrate into the nano filtrate, and then carrying out desalination treatment on 717 ion exchange resin; and (3) further dehydrating the desalted nanofiltration liquid through a nanofiltration membrane, and performing centrifugal spray drying when the quantity concentration of nanofiltration liquid substances reaches 1.5 to prepare stevioside.
The invention is specifically illustrated by 2 embodiments, which do not limit the scope of the invention; the technical features disclosed in the technical solutions of the present invention are within the scope of the present invention.
Claims (7)
1. A method for preparing stevioside is characterized by comprising the following steps:
1) crushing the leaves: pulverizing the screened high-quality dried stevia rebaudiana leaves, and sieving with a 40-80 mesh sieve to obtain stevia rebaudiana powder;
2) preparing a leaching solution: soaking the stevia rebaudiana powder prepared in the step 1) in pure water with the mass of 5-7 times of that of the stevia rebaudiana powder for 2-5 hours, and filtering to obtain a leaching solution; repeating the above method for 1-2 times, mixing the leaching solutions obtained after 2-3 times of filtration, ultrafiltering, and nanofiltering to obtain concentrated leaching solution;
3) chromatography: putting the concentrated leaching liquor obtained in the step 2) into a resin chromatographic column, controlling the volume ratio of the concentrated leaching liquor to the resin chromatographic column to be 3-4: 1, and controlling the concentrated leaching liquor to carry out chromatography at a flow rate of 1.5-2 times the volume of the chromatographic column to obtain a chromatographic solution;
4) and (3) elution: eluting the chromatographic solution in the step 3) by using 1BV pure water, and eluting by using ethanol at the flow rate of 1 hour and 1.5BV column volume for 1-2 hours;
5) preparing nano filtrate: collecting the eluent in the step 4), recovering ethanol by a concentrator, and performing ultrafiltration and nanofiltration to obtain nanofiltration solution;
6) desalting: adding pure water with the volume of 1.5-2 times that of the nano filtrate into the nano filtrate prepared in the step 5, and desalting with cation exchange resin to obtain a desalted nano filtrate;
7) spray drying: and (3) further dehydrating the desalted and nanofiltration liquid prepared in the step 6) through a nanofiltration membrane, and performing spray drying when the mass concentration of nanofiltration liquid reaches 1.1-1.4mol/L to prepare stevioside.
2. The method of claim 1, wherein the method comprises the following steps: the temperature of the pure water in the step 2) is 40-50 ℃.
3. The method of claim 1 or 2, wherein the method comprises the following steps: and (3) ultrafiltering the filtrate in the step 2) by using an 15000-.
4. The method of claim 1, wherein the method comprises the following steps: and 5) respectively performing ultrafiltration on the washing liquid by an ultrafiltration membrane with the molecular weight of 8000-.
5. The method of claim 3, wherein the method comprises the following steps: and 5) respectively carrying out ultrafiltration on the eluent in the step 5) by an ultrafiltration membrane with 8000-.
6. The method of claim 1, wherein the method comprises the following steps: the cation exchange resin in the step 6) is 732 ion exchange resin or 717 ion exchange resin.
7. The method of claim 1, wherein the method comprises the following steps: the spray drying method in the step 7) adopts centrifugal spray drying.
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| CN201910946339.3A CN110627851A (en) | 2019-10-04 | 2019-10-04 | Preparation method of stevioside |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876982A (en) * | 2015-01-23 | 2015-09-02 | 南通海天生物科技有限公司 | Technology for separating stervioside from stevia rebaudian leaf |
| CN108864223A (en) * | 2018-09-05 | 2018-11-23 | 安徽龙津生物科技有限公司 | A kind of technique separating steviol glycoside parallel connection yield of chlorogenic acid from stevia rebaudian leaf |
| CN109354596A (en) * | 2018-10-09 | 2019-02-19 | 山东奥晶生物科技有限公司 | A kind of preparation method of efficient steviol glycoside |
| CN110229201A (en) * | 2019-06-25 | 2019-09-13 | 浙江天草生物科技股份有限公司 | A kind of process preparing high-purity steviosides RM |
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2019
- 2019-10-04 CN CN201910946339.3A patent/CN110627851A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876982A (en) * | 2015-01-23 | 2015-09-02 | 南通海天生物科技有限公司 | Technology for separating stervioside from stevia rebaudian leaf |
| CN108864223A (en) * | 2018-09-05 | 2018-11-23 | 安徽龙津生物科技有限公司 | A kind of technique separating steviol glycoside parallel connection yield of chlorogenic acid from stevia rebaudian leaf |
| CN109354596A (en) * | 2018-10-09 | 2019-02-19 | 山东奥晶生物科技有限公司 | A kind of preparation method of efficient steviol glycoside |
| CN110229201A (en) * | 2019-06-25 | 2019-09-13 | 浙江天草生物科技股份有限公司 | A kind of process preparing high-purity steviosides RM |
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