CN108101947A - A kind of extracting method of steviol glycoside - Google Patents
A kind of extracting method of steviol glycoside Download PDFInfo
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Abstract
The present invention relates to a kind of extracting methods of steviol glycoside.Stevia rebaudian leaf is put into extractant in extractor and is extracted, obtains steviol glycoside level-one extracting solution；Level-one extracting solution is subjected to flocculation sediment and is filtered, obtains steviol glycoside filtered fluid；By steviol glycoside filtered fluid elution action, steviol glycoside two level extracting solution is obtained；Purification operations are carried out to steviol glycoside two level extracting solution using finishing column, obtain steviol glycoside refined liquid；Steviol glycoside refined liquid is concentrated using dual-effect concentrator；Then degerming, spray drying are carried out, obtains steviol glycoside dry product；Wherein at least one of inorganic flocculating agent flocculation, attapulgite adsorption-flocculation and ethanol precipitation three kinds of flocculation modes of flocculation can be used in flocculation step.This method reduces the loss of steviol glycoside in flocculation process, greatly improves the extraction efficiency of steviol glycoside by the improvement to flocculant in stevia rebaudian leaf extraction process.
Description
Technical field
The present embodiments relate to a kind of extracting method more particularly to a kind of extracting methods of steviol glycoside.
Background technology
STEVIA REBAUDIANA alias stevia rebaudianum, sugar grass, it is the evergreen dwarf shrub for originating in South America Paraguay plateau to belong to composite family, by generation
Boundary introduces a fine variety various regions.STEVIA REBAUDIANA contains 14 kinds of trace elements, 32 kinds of nutritional ingredients, is not metabolized, does not accumulate in vivo, not carcinogenic, nothing
Toxicity, security has obtained the accreditation of the tissues such as international FAO and WHO and U.S. FAD, therefore it is both fabulous sugar
Source, and be good source of nutrition.
Steviol glycoside is the active ingredient in STEVIA REBAUDIANA, belongs to the high sweetener of natural diet.It is containing there are many not
Congruent tetracyclic diterpene monomer, these monomers have identical aglycon-steviol (Steviol), can be according to C13 and C19
Position links different aglycons and is divided into stevioside (Stevioside), stevioside A (RebaudiosideA), B
(RebaudiosideB), C (RebaudiosideC), D (Rebaudioside D), E (RebaudiosideE), Dole can glycosides
(DulcosideA), this is for the primary glycosides (Steviolbioside) of dimension and raspberry glycosides (Rubusoside).In these monomers,
Content it is highest for stevioside (Stevioside), stevioside A (RebaudiosideA) account for respectively leaf dry weight 5%~
9.5%th, 2%~4.5% sugariness is respectively the 300 of sucrose, 450 times.Research shows that steviol glycoside has high sugariness, low-heat
The characteristics of amount, no obvious toxic-side effects, it can inhibit hyperglycaemia, hypertension, and have anti-inflammatory, antitumor, antidiarrheal diuresis and association
Help immunoregulatory effect.
Stevioside, usually will be to carrying before resin is used to carry out active principle absorption and exquisiteness in industrial abstract
Liquid is taken to carry out flocculation operation, carrying out solution usually using inorganic salts carries out flocculation operation, for example, adding in ferrous sulfate solution and oxygen
Change calcium solution and carry out flocculation operation, the mass ratio of ferrous sulfate solid masses and extracting solution therein is 0.7:100, the oxygen of addition
The mass ratio for changing the calcium oxide solid masses in calcium solution and extracting solution is 0.2:100；At this point, the active ingredient meeting in extracting solution
It is lost with flocculation operation two, ordinary loss rate is more than 16%, and even above 20%, so there is larger impact to extraction efficiency, because
This needs a kind of good flocculant substance with when method in a hurry, to reduce the loss in flocculation operation to active principle.
The content of the invention
The present invention provides a kind of extracting methods of steviol glycoside, and stevia rebaudian leaf repeatedly can be extracted, reduce and flocculated
Loss late in journey greatly improves the extraction efficiency of steviol glycoside.
The extracting method of steviol glycoside of the present invention is specific as follows：
A kind of extracting method of steviol glycoside, which is characterized in that including：Step S10, stevia rebaudian leaf and extractant are put into extractor
In extract, obtain steviol glycoside level-one extracting solution；Step S20, level-one extracting solution is subjected to flocculation sediment and filtered, obtained
Steviol glycoside filtered fluid；Step S30, by steviol glycoside filtered fluid elution action, steviol glycoside two level extracting solution is obtained；Step
S40, purification operations are carried out to steviol glycoside two level extracting solution using finishing column, obtains steviol glycoside refined liquid；Step S50, make
Steviol glycoside refined liquid is concentrated with dual-effect concentrator；Then degerming, spray drying are carried out, obtains steviol glycoside dry product；
Wherein, inorganic flocculating agent flocculation, attapulgite adsorption-flocculation and ethanol precipitation flocculation three can be used in the flocculation step in step 20
At least one of kind flocculation mode.
Wherein repeatedly extraction is specially：Using tap water to stevia rebaudianum leaf raw material extraction 2.5 it is small when, collect first production liquid；Make
When continuing small to stevia rebaudianum leaf raw material extraction 1 with tap water, the second production liquid is collected；First production liquid and the second production liquid are mixed to get mixed
Liquid is closed, as steviol glycoside level-one extracting solution；Continue to carry out stevia rebaudianum leaf raw material respectively third time extraction and using tap water
Four times extraction, every time 1 it is small when, by tertiary industry liquid and the 4th production liquid mix, new stevia rebaudianum leaf raw material is carried for the first time as next time
The extracting solution taken；Wherein Extracting temperature is 50-60 degrees Celsius.
It is specially using the flocculated flocculation filtration step of inorganic flocculating agent：Ferric chloride solution is added in into level-one extracting solution,
It stirs half an hour, the calcium oxide added, stirs half an hour, carry out flocculation sediment and filter, carbon acid solution is added in into filtrate,
Half an hour is stirred, is precipitated and filtered, obtain steviol glycoside filtered fluid.
The mass ratio of iron chloride solid masses and extracting solution in the ferric chloride solution of addition is 0.5:100, the oxygen of addition
The mass ratio for changing the calcium oxide solid masses in calcium solution and extracting solution is 0.1:100, it is Celsius for 60-70 to add in whipping temp
Degree, flocculation sediment temperature are 5-20 degrees Celsius；
The volume ratio for adding in carbonic acid and extracting solution is 0.5:100, carbonate concentration 1%, it is 10-20 degrees Celsius to add in whipping temp.
Included using inorganic flocculating agent flocculation：25%-35% chitosans, 20%-30% ferric sulfate, 15%-25% magnesium sulfate, 10%-
20% ferrosilite, 5%-10% Ireland seaweed, 5%-10% zeolite powders.Said ratio inorganic flocculating agent is added in into level-one extracting solution,
Temperature is adjusted to 65-85 degrees Celsius and stirs 40 minutes, then adjusts temperature and obtains flocculation sediment to 5-10 degrees Celsius and filter, obtains
To steviol glycoside filtered fluid；Wherein level-one extracting solution and inorganic flocculating agent mass ratio are 300:1.
It is concretely comprised the following steps using the filtering of attapulgite adsorption-flocculation：Level-one extracting solution is added in after attapulgite is crushed, is added
The mass ratio for entering attapulgite and extracting solution is 1:100, it stirs one hour, whipping temp is 65-70 degrees Celsius, and temperature is reduced
To 15-20 degrees Celsius, stand one hour and obtain flocculation sediment and filter, obtain steviol glycoside filtered fluid.The crushing of attapulgite
Process is specially：Attapulgite is acidified using sulfuric acid, when 500 degrees Celsius of calcinings 3 are small, is crushed as attapulgite powder.
It is concretely comprised the following steps using ethanol precipitation flocculation filtration：It is small that the ethyl alcohol of 95% concentration is added in into the stirring one of level-one extracting solution
When；Vacuum distillation operation removal ethyl alcohol is carried out after standing one hour, flocculation sediment is obtained after standing half an hour and filters, obtain sweet tea
Synanthrin glycosides filtered fluid；Wherein add in the volume ratio 1 of ethyl alcohol and extracting solution:10, essence puts temperature as 5-20 degrees Celsius after removing ethyl alcohol.
It is filtered using plate filter, plate filter is filtered using non-woven fabrics, and pore size is 280-320 mesh.
After the steviol glycoside saturation in resin adsorption steviol glycoside two level extracting solution in finishing column, inhaled using ethanol elution
The steviol glycoside being attached on finishing column resin makes steviol glycoside depart from finishing column, obtains steviol glycoside refined liquid.
It can be seen that from above-mentioned introduction using the method for the invention, to stevia rebaudian leaf using repeatedly extraction and a variety of flocculation modes
Combination, greatly reduces loss late of the steviol glycoside in flocculation process, while improves the extraction efficiency of steviol glycoside and pure
Degree.
【Description of the drawings】
Fig. 1 is the flow chart of present invention extraction steviol glycoside.
【Specific embodiment】
For problems of the prior art, the extracting method of steviol glycoside of the invention can repeatedly extract stevia rebaudian leaf,
The loss late in flocculation process is reduced, greatly improves the extraction efficiency of steviol glycoside.
In order to make the object, technical solutions and advantages of the present invention clearer, in the following with reference to the drawings and specific embodiments to this hair
It is bright to be described in detail.
Embodiment 1
Fig. 1 is the flow chart of present invention extraction steviol glycoside first embodiment, as shown in Figure 1, including realization side in detail below
Formula.
Step S10, stevia rebaudian leaf is put into extractant in extractor and extracted, obtain steviol glycoside level-one extracting solution.
In the step, 1 ton of first use stevia rebaudianum leaf raw material adds in 20 tons of tap water at normal temperature, as extractant, is averagely put into
The extractor that 8 volumes are 4m3.
Extraction preferably 45 degree, starts to extract for the first time specifically, by the water temperature heating in extractor to 35-50 degrees Celsius,
Continue 2.5 it is small when, then collect extracting solution；
Tap water is added in into 8 extractors again, is heated to 35-50 degrees Celsius, preferably 45 degree, carries out second of extraction behaviour
Make, continue 1 it is small when, then collect extracting solution；
The extracting solution extracted twice is mixed, as steviol glycoside level-one extracting solution, volume is 20m3 or so.
Continue to carry out stevia rebaudianum leaf raw material respectively third time extraction and the 4th extraction using tap water, every time 1 it is small when, will
Tertiary industry liquid and the 4th production liquid mixing, the extracting solution extracted for the first time to new stevia rebaudianum leaf raw material as next time.Wherein third time
When being 1 small with the time of the 4th extraction, third time extracts Extracting temperature as 40-60 degrees Celsius, preferably 50 degrees Celsius, the 4th
Secondary extraction Extracting temperature is 50-60 degrees Celsius, preferably 55 degrees Celsius.
After obtaining level-one extracting solution, the waste residue of stevia rebaudian leaf can carry out secondary production, most as the raw material of production organic fertilizer
The efficiency of the performance raw material of limits.
Step S20, level-one extracting solution is subjected to flocculation sediment and filtered, obtain steviol glycoside filtered fluid；Use two appearances
Product flocculates to level-one extracting solution for 10 m3 flocculation tanks, and inorganic flocculating agent flocculation, attapulgite adsorption-flocculation may be employed
And at least one of ethanol precipitation three kinds of flocculation modes of flocculation.
Concretely comprising the following steps during using inorganic flocculating agent：
Ferric chloride solution is added in into level-one extracting solution, is stirred half an hour, the calcium oxide added, half an hour is stirred, wads a quilt with cotton
Retrogradation is formed sediment and is filtered, and carbon acid solution is added in into filtrate, stirs half an hour, is precipitated and filtered, and obtains steviol glycoside filtering
Liquid.
The mass ratio of iron chloride solid masses and extracting solution in the ferric chloride solution of addition is 0.5:100, the oxygen of addition
The mass ratio for changing the calcium oxide solid masses in calcium solution and extracting solution is 0.1:100, it is Celsius for 60-70 to add in whipping temp
Degree, preferably 65 degrees Celsius, flocculation sediment temperature is 5-20 degrees Celsius, preferably 10 degrees Celsius；Add in the volume of carbonic acid and extracting solution
Than for 0.5:100, carbonate concentration 1%, it is 10-20 degrees Celsius to add in whipping temp.
When after measured, using above-mentioned inorganic flocculating agent, the loss late of steviol glycoside is 13%, simultaneously because last carbonic acid
Processing so that the inorganic ions to dissociate in extracting solution is effectively precipitated, and greatly improves the purity of steviol glycoside.
Another inorganic flocculating agent matches and step is as follows：
The heavy inorganic flocculating agent flocculation includes：25%-35% chitosans, 20%-30% ferric sulfate, 15%-25% magnesium sulfate, 10%-20%
Ferrosilite, 5%-10% Ireland seaweed, 5%-10% zeolite powders.
Optimum ratio is：Chitosan, ferric sulfate, magnesium sulfate, ferrosilite, Irish seaweed, the ratio of zeolite powder is 30%,
25%, 20%, 15%, 5%, 5%；Or
Chitosan, ferric sulfate, magnesium sulfate, ferrosilite, Irish seaweed, the ratio of zeolite powder is 35%, 20%, 25%, 10%, 5%,
5%；
Wherein chitosan is physical modification chitosan.
Said ratio inorganic flocculating agent is added in into level-one extracting solution, temperature is adjusted to 65-85 degrees Celsius（It is preferred that 80 is Celsius
Degree）Then stirring 40 minutes adjusts temperature and obtains flocculation sediment to 5-10 degrees Celsius and filter, obtains steviol glycoside filtered fluid；
Wherein level-one extracting solution and inorganic flocculating agent mass ratio are 300:1.
When after measured, using above-mentioned inorganic flocculating agent, the loss late of steviol glycoside is 6.2%, simultaneously because the work of zeolite powder
With flocculation rate being accelerated, simultaneously because adding in Irish seaweed so that the organic matters such as extracting solution protein more effectively precipitate,
Greatly improve the purity of steviol glycoside.
It is concretely comprised the following steps using the filtering of attapulgite adsorption-flocculation：
Attapulgite is acidified using sulfuric acid, when 500 degrees Celsius of calcinings 3 are small, is crushed as attapulgite powder, by concave convex rod
Mountain flour adds in level-one extracting solution, and the mass ratio for adding in attapulgite and extracting solution is 1:100, it stirs one hour, whipping temp is
65-70 degrees Celsius, temperature is reduced to 15-20 degrees Celsius, preferably 15 degrees Celsius, one hour is stood and obtains flocculation sediment and mistake
Filter, obtains steviol glycoside filtered fluid.The crushing process of attapulgite is specially：
When after measured, using above-mentioned attapulgite flocculant, the loss late of steviol glycoside is 6%.
It is concretely comprised the following steps using ethanol precipitation flocculation filtration：
The ethyl alcohol of 95% concentration is added in level-one extracting solution to stir one hour；Vacuum distillation operation removal is carried out after standing one hour
Ethyl alcohol obtains flocculation sediment after standing half an hour and filters, obtains steviol glycoside filtered fluid；Wherein add in ethyl alcohol and extracting solution
Volume ratio 1:10, essence puts temperature as 5-20 degrees Celsius after removing ethyl alcohol.
When after measured, using above-mentioned ethyl alcohol flocculant, the loss late of steviol glycoside is 8%.
For above-mentioned three kinds of flocculation modes, can be selected wherein according to product condition and production cost in practical applications
One or more carry out, to reach good flocculating effect；
After the completion of flocculation, flocculation liquid using three plate filters is filtered by the level-one extracting solution for completion of flocculating, obtains stevia rebaudianum
Glucosides filtered fluid, wherein each sheet frame area is 100 square metres, filter is the production of Shanghai great Zhang filter plants Co., Ltd
The van-type plate and frame filter press of XMY100/1000-30U, filtration fraction use the non-woven fabrics of aperture 280-320 mesh, preferably 300 mesh.
The filtered fluid for being collected into 18m3 or so is sent into the filtrate tank of two 9m3.
Step S30, by steviol glycoside filtered fluid elution action, steviol glycoside two level extracting solution is obtained；；
Specifically, steviol glycoside filtered fluid is transferred to LX-T28 resin absorbing columns；Using NaOH wash after the completion of absorption miscellaneous；Make
Soda is carried out to pH8 with pure water；It is washed using HCl miscellaneous then sour to pH6 with pure washing；The ethyl alcohol that concentration is 60% is to inhaling
Attached column is parsed.
What is generated in the step crosses column waste liquid, washing waste liquid and acid-base waste fluid, and wastewater treatment dress is discharged by waste pipe
It puts, after processing reaches discharging standards, is discharged.
Then the steviol glycoside liquid after parsing is subjected to desalination, decoloration, dealcoholation treatment, obtains the extraction of steviol glycoside two level
Liquid；
Wherein, the steviol glycoside liquid after parsing is once passed through into desalting column（001X16）, decolorizing column（LX-T5, three, single 1.8
m³）And dealcoholization device（Nanofiltration membrane and single-action concentration）, obtain steviol glycoside two level extracting solution, volume about 3m3.
Step S40, purification operations are carried out to steviol glycoside two level extracting solution using finishing column, obtains steviol glycoside and refine
Liquid；
In the step, two level extracting solution is refined using the LX-69B finishing columns that a volume is 1.1 m3, is refined
Liquid about 3m3.Specifically, after steviol glycoside saturation in resin adsorption steviol glycoside two level extracting solution in finishing column, 60% is used
Ethanol elution adsorb steviol glycoside on finishing column resin, steviol glycoside is made to depart from finishing column, steviol glycoside is obtained and refines
Liquid.
Step S50, steviol glycoside refined liquid is concentrated using dual-effect concentrator；Then degerming, spray drying are carried out,
Obtain steviol glycoside dry product；
Specifically, obtain steviol glycoside concentrate about 300L after concentration.
Degerming and filtering, steviol glycoside end liquid about 300L are carried out to concentrate using 0.22 μm of filter.
Steviol glycoside end liquid is spray-dried in temperature for 50-70 degrees Celsius, preferably 65 degree.The step obtains stevia rebaudianum
Glucosides dry product 60kg.
Total glycosides content of the steviol glycoside dry product prepared by the present embodiment method is close to 90%, wherein RA（Stevioside A）Content
More than 65%.It can be seen that the extracting method step in embodiment is simple, the loss late in flocculation process, while extraction efficiency are reduced
It is higher, obtain total glycosides content and the higher steviol glycoside dry product of purity.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God and any modification, equivalent substitution, improvement and etc. within principle, done, should be included within the scope of protection of the invention.
Claims (10)
1. a kind of extracting method of steviol glycoside, which is characterized in that including：
Step S10, stevia rebaudian leaf is put into extractant in extractor and extracted, obtain steviol glycoside level-one extracting solution；
Step S20, level-one extracting solution is subjected to flocculation sediment and filtered, obtain steviol glycoside filtered fluid；
Step S30, by steviol glycoside filtered fluid elution action, steviol glycoside two level extracting solution is obtained；
Step S40, purification operations are carried out to steviol glycoside two level extracting solution using finishing column, obtains steviol glycoside refined liquid；
Step S50, steviol glycoside refined liquid is concentrated using dual-effect concentrator；Then degerming, spray drying are carried out, is obtained
Steviol glycoside dry product；
Wherein, inorganic flocculating agent flocculation, attapulgite adsorption-flocculation and ethanol precipitation wadding can be used in the flocculation step in step S20
Coagulate at least one of three kinds of flocculation modes.
2. extracting method according to claim 1, which is characterized in that it is described it is multiple extraction be specially：
Using tap water to stevia rebaudianum leaf raw material extraction 2.5 it is small when, collect first production liquid；
When continuing small to stevia rebaudianum leaf raw material extraction 1 using tap water, the second production liquid is collected；
First production liquid and the second production liquid are mixed to get mixed liquor, as steviol glycoside level-one extracting solution；
Continue to carry out stevia rebaudianum leaf raw material respectively third time extraction and the 4th extraction using tap water, every time 1 it is small when, by the 3rd
Produce liquid and the 4th production liquid mixing, the extracting solution extracted for the first time to new stevia rebaudianum leaf raw material as next time；
Wherein Extracting temperature is 50-60 degrees Celsius.
3. extracting method according to claim 1, which is characterized in that using the flocculated flocculation filtration step of inorganic flocculating agent
Specially：Ferric chloride solution is added in into level-one extracting solution, is stirred half an hour, the calcium oxide added, stirs half an hour, is carried out
Flocculation sediment simultaneously filters, and carbon acid solution is added in into filtrate, stirs half an hour, is precipitated and filtered, obtain steviol glycoside mistake
Filtrate.
4. extracting method according to claim 3, which is characterized in that the iron chloride solid matter in the ferric chloride solution of addition
The mass ratio of amount and extracting solution is 0.5:100, the quality of calcium oxide solid masses and extracting solution in the calcium oxide solution of addition
Than for 0.1:100, it is 60-70 degrees Celsius to add in whipping temp, and flocculation sediment temperature is 5-20 degrees Celsius；
The volume ratio for adding in carbonic acid and extracting solution is 0.5:100, carbonate concentration 1%, it is 10-20 degrees Celsius to add in whipping temp.
5. extracting method according to claim 1, which is characterized in that included using inorganic flocculating agent flocculation：25%-35% shells
Glycan, 20%-30% ferric sulfate, 15%-25% magnesium sulfate, 10%-20% ferrosilites, 5%-10% Ireland seaweed, 5%-10% zeolite powders；
Into level-one extracting solution add in said ratio inorganic flocculating agent, temperature be adjusted to 65-85 degrees Celsius stir 40 minutes, then
It adjusts temperature to obtain flocculation sediment to 5-10 degrees Celsius and filter, obtains steviol glycoside filtered fluid；
Wherein level-one extracting solution and inorganic flocculating agent mass ratio are 300:1.
6. extracting method according to claim 1, which is characterized in that specific steps are filtered using attapulgite adsorption-flocculation
For：Level-one extracting solution is added in after attapulgite is crushed, the mass ratio for adding in attapulgite and extracting solution is 1:100, stirring one
Hour, whipping temp is 65-70 degrees Celsius, and temperature is reduced to 15-20 degrees Celsius, one hour is stood and obtains flocculation sediment and mistake
Filter, obtains steviol glycoside filtered fluid.
7. extracting method according to claim 6, which is characterized in that the crushing process of attapulgite is specially：Use sulphur
Acid is acidified attapulgite, when 500 degrees Celsius of calcinings 3 are small, crushes as attapulgite powder.
8. extracting method according to claim 1, which is characterized in that concretely comprised the following steps using ethanol precipitation flocculation filtration：
The ethyl alcohol of 95% concentration is added in level-one extracting solution to stir one hour；Vacuum distillation operation removal ethyl alcohol is carried out after standing one hour,
Flocculation sediment is obtained after standing half an hour and is filtered, and obtains steviol glycoside filtered fluid；
Wherein add in the volume ratio 1 of ethyl alcohol and extracting solution:10, essence puts temperature as 5-20 degrees Celsius after removing ethyl alcohol.
9. according to any extracting methods of claim 3-8, which is characterized in that be filtered using plate filter, plate
Frame filter is filtered using non-woven fabrics, and pore size is 280-320 mesh.
10. extracting method according to claim 1, which is characterized in that step S40 is specially：
After the steviol glycoside saturation in resin adsorption steviol glycoside two level extracting solution in finishing column, existed using ethanol elution absorption
Steviol glycoside on finishing column resin makes steviol glycoside depart from finishing column, obtains steviol glycoside refined liquid.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110372762A (en) * | 2019-07-31 | 2019-10-25 | 诸城市浩天药业有限公司 | A kind of STEVIA REBAUDIANA crude protein and stevioside integrated extraction technique |
| CN111111256A (en) * | 2020-01-06 | 2020-05-08 | 江苏泽博环保科技有限公司 | Method and device for purifying plant water extracting solution |
| CN112940057A (en) * | 2021-02-04 | 2021-06-11 | 北京澳特舒尔保健品开发有限公司 | Preparation and purification method of stevioside and application of stevioside in anti-fatigue product |
| CN114456216A (en) * | 2020-11-09 | 2022-05-10 | 江苏施宇甜生物科技有限公司 | Method for extracting high-purity stevioside |
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| CN112940057A (en) * | 2021-02-04 | 2021-06-11 | 北京澳特舒尔保健品开发有限公司 | Preparation and purification method of stevioside and application of stevioside in anti-fatigue product |
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