CN102775453A - Method for crystallizing and separating stevioside A3 from stevia total glycoside mixture - Google Patents
Method for crystallizing and separating stevioside A3 from stevia total glycoside mixture Download PDFInfo
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- CN102775453A CN102775453A CN2012102083141A CN201210208314A CN102775453A CN 102775453 A CN102775453 A CN 102775453A CN 2012102083141 A CN2012102083141 A CN 2012102083141A CN 201210208314 A CN201210208314 A CN 201210208314A CN 102775453 A CN102775453 A CN 102775453A
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Abstract
The invention discloses a method for crystallizing and separating stevioside A3 from a stevia total glycoside mixture. The method comprises the following steps of: preparing a mixed solvent; adding a stevia total glycoside mixture raw material and the mixed solvent into a container for mixing according to a solid-liquid mass volume ratio of (1g:3ml)-(1g:5ml); stirring and dissolving at room temperature for 10-30 minutes; adding a stevioside A3 crystal seed; stirring at the temperature of 4-20DEG C for 2-6 hours and then centrifugally separating to obtain a crystal product; washing the crystal product with absolute ethyl alcohol and centrifugally separating and then washing with absolute methanol; and after centrifugally separating, carrying out vacuum drying to obtain a stevioside A3 product. The method disclosed by the invention has the advantages of simple and feasible process, low energy consumption and easy realization of industrial production.
Description
Technical field
The present invention relates to the method for purification of a kind of stevioside A3, specifically be to use the method for mixed solvent Crystallization Separation stevioside A3 from Flos Chrysanthemi total glycosides.
Background technology
Stevioside A3 claims content rebaudioside-A (rebaudioside A) again, and molecular formula is C
44H
71O
24, relative molecular mass 983 is sweeting agents of a kind of strong effect, and the sugariness of stevioside is about 200 times of sucrose, and its aftertaste has a little the sweetness and bitterness flavor.The sugariness of stevioside A3 is 350～400 times of sucrose, pure taste, not back bitter taste.The stevioside city general Flos Chrysanthemi total glycosides of price ratio that contains 80% stevioside A3 is high 4～5 times.Stevia rebaudianum glucoside sweeting agent has been widely used in foodstuffs industry and the medicine industry as sweeting agent, additive and correctives; In cake, biscuit, beverage, can, curing food, also can be used in mellitus, hypertension, obesity, coronary heart disease, eurodonticus's the protective foods and chinese-western medicine preparation.
The preparation method of stevioside A3 mainly adopts resin isolation method and low-temperature methanol crystallization process.The resin isolation method is to be raw material with the sweet Stevia liquid concentrator, through different resins repeatedly wash-out obtain stevioside A3.This method separation resin elution time is longer, and stevioside A3 concentration is on the low side in the elutriant, and concentrates difficulty, and power consumption is big.The methanol crystallization method is to use methyl alcohol to make solvent, and obtaining primary crystallization mainly is stevioside, and different with concentration, the consumption of methyl alcohol, its content has certain fluctuation; Most of stevioside A3 stays in the mother liquor, carry out the methyl alcohol secondary crystal after needing to concentrate, and Tc needs to carry out at sub-zero low temperature; This process also has the methyl alcohol of employing and the mixed solvent of Virahol to carry out crystallization, and its purity of stevioside A3 that this method obtains is on the low side, is about 90%; Time is long, is about 48h, and crystallization requires temperature low; The industriallization cost is high, and needs through crystallisation step repeatedly, and is not only consuming time but also the solvent loss amount is big.
Application number is that 200810196722.3 Chinese invention patent application discloses a kind of method of from the sweet Stevia liquid concentrator, separating purification stevioside A3 and stevioside.This method as fixing agent, is a raw material with the liquid concentrator through the simulation moving-bed acid calcium type resin that utilizes, and as eluent, stevioside A3, stevioside and other stevioside is separated with water.This method adopts simulated moving bed technology purify stevioside A3 and stevioside, needs synthetic resins, separate the back resin and have the recycling problem, and sepn process needs temperature higher, accomplishes for 35 ℃～95 ℃ in heating and separates, and needs to consume more heat energy.
The patent No. is that the Chinese invention patent of CN200710025792.8 discloses a kind of method of from stevioside, extracting high pure rebaudioside A; This method utilizes recrystallization and membrane separation technique to combine; Carry out recrystallization with methyl alcohol and isopropyl alcohol mixed solvent dissolving raw material stevioside; Tc needs-18 ℃, needs recrystallization behind the crystallization time 24-48h; Crystal with membrane sepn again after the pure water dissolving, is concentrated, vacuum-drying obtains high pure rebaudioside A content greater than 90% product.This method also need be carried out membrane separation technique after need carrying out recrystallization repeatedly, has not only increased life cycle of the product at recrystallization process, and has consumed a large amount of solvents, and membrane sepn increases cost especially, also has the recycling problem of film.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art; A kind of work simplification, a need primary crystallization are provided, and, need not to increase refrigeration equipment 4 ℃～20 ℃ following crystallizations; And shortened crystallization time greatly, energy-saving separation from Flos Chrysanthemi total glycosides obtains the method for highly purified stevioside A3.
The falling temperature method crystallization is adopted in invention, thereby forms the solute that principle that supersaturated solution separates out obtains higher degree according to solute through reducing temperature, and it is a lot of to influence the crystalline factor; Mainly contain selection, the Tc of single or double solvents, stirring velocity, alr mode; Selection of degree of supersaturation or the like, wherein choice of Solvent is that can the decision material successful crystalline key factor, according to the similar principle that mixes; Solute is soluble in the close solvent of structure; Polar material is soluble in polar solvent, and the solvent that polarity is stronger often has water, methyl alcohol, ethanol etc., and middle polarity reaches has Virahol, acetone, ETHYLE ACETATE, chloroform or the like than low polar solvent.But the selection of final suitable solvent can only decide with the method for test.Mainly stevioside A3 is carried out Crystallization Separation in the invention; Adopt water, methyl alcohol, alcohol mixed solvent as recrystallisation solvent, this mixed system is the stevioside A3 and other impurity in the dissolving raw material effectively, and makes stevioside A3 formation supersaturated solution at temperature-fall period; Can reach the purpose of Crystallization Separation at short notice; The introducing of water has increased solvent polarity, and it is interval better to have controlled supersaturation, makes primary crystallization can obtain high purity stevioside A3.And prior art uses recrystallisation solvent to be methyl alcohol or methyl alcohol and isopropyl alcohol mixed solvent; Because polarity is lower, stevioside A3 solubleness reduces, and need just can not make stevioside A3 be in hypersaturated state and slowly separate out at low temperature more; Other impurity are also slowly separated out in the lump in this process; Therefore primary crystallization stevioside A3 not only the time long, purity is not high, and needs recrystallization further to separate stevioside A3.
For adopting following technical scheme, the purpose the present invention who realizes foregoing invention is achieved:
A kind of from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, comprise the steps:
(1) mixed solvent preparation: be water by volume: ethanol: methyl alcohol=0.2～0.8: 1～3: 1 ratio is prepared mixed solvent with water, ethanol and methanol mixed;
(2) crystallization: be that the ratio of 1g: 3ml～1g: 5ml joins Flos Chrysanthemi total glycosides mixture material and mixed solvent in the container and mixes in the Flos Chrysanthemi total glycosides mixture material and the solid-liquid mass volume ratio of mixed solvent; Stirring and dissolving 10～30min under the room temperature; Add stevioside A3 crystal seed; Spinning after temperature is 4 ℃～20 ℃ stirring 2～6h obtains crystalline product; Stevioside A3 crystal seed is a purity greater than 99% stevioside A3, the consumption of stevioside A3 crystal seed be in the Flos Chrysanthemi total glycosides mixture material stevioside A3 weight 1～5%; Said Flos Chrysanthemi total glycosides mixture material is a stevioside A3 weight content greater than 40% Flos Chrysanthemi total glycosides mixture;
(3) separate: the gained crystalline product with absolute ethanol washing after spinning, wash with anhydrous methanol again; After the spinning, vacuum-drying gets stevioside A3 product.
For further realizing the object of the invention; By percentage to the quality; Stevioside A3 content is preferably 40～90% in the said Flos Chrysanthemi total glycosides mixture material, and stevioside content is preferably 7～50%, and stevia rebaudianum disaccharide salidroside content is preferably 1～5%; Stevioside B content is preferably 1～3%, and stevioside C content is preferably 1～2%.
Said ethanol is that volumetric concentration is preferably more than 95% aqueous ethanolic solution or absolute ethyl alcohol.
The condition optimization of said spinning is under 2000～3000rpm rotating speed, centrifugal 6～15min.
Said vacuum-drying for preferably be-0.04 in vacuum tightness～-carry out under the 0.02MPA.
In the said anhydrous methanol washing, crystal and anhydrous methanol feed liquid mass volume ratio are preferably 1g: 1ml～1g: 5ml.
The number of times of said anhydrous methanol washing is preferably 1-3 time.The number of times of said washing with alcohol is preferably 1-3 time.
With respect to prior art, the present invention has following advantage and positively effect:
1, the present invention chooses mixed solvent crystallization from Flos Chrysanthemi total glycosides, the separation stevioside A3 of ethanol, first alcohol and water composition; Primary crystallization can make 40% stevioside A3 purity bring up to 85-90% with washing; Can make the purity of stevioside A3 reach 95-99.9% with methanol wash again; Kept stevioside A3 to greatest extent, the purity of stevioside A3 is high, and this invention is than report technical matters process is more simple at present.
2, crystallization of the present invention can be carried out under 4 ℃～20 ℃ normal temperature, does not need low temperature crystallization, energy consumption low, and production cost is low.In crystallisation process, choice of Solvent is one of key factor that is related to the purifying stevioside A3 and the recovery, and water has play a part very crucial here in the mixed solvent of the present invention; Because the adding of water reaches the dissolving power that has improved stevioside A3, make temperature change among a small circle in the mixed solvent that water, ethanol, methyl alcohol are formed; Be that Tc will make stevioside A3 reach the supersaturation interval under 4 ℃～20 ℃; Solution reaches hypersaturated state, makes together to separate out crystallization at 4 ℃～20 ℃ following stevioside A3 with crystal seed, can obtain the higher stevioside A3 of purity through washing crystal; Therefore only need crystallization once; And need the sub-zero zero in open source literature not accomplish crystallisation process, energy consumption will be 20% of a prior art, and cost reduces over half.
3, take vacuum-drying stevioside A3, make stevioside A3 thoroughly dry, pulverize easily, solvent is safer and boiling point is low, is evaporated away easily, and organic solvent residual is low in the product.
4, through mixed solvent crystallization method of the present invention, not only can carry out Crystallization Separation stevioside A3, and can at room temperature carry out big content of starting materials, solvent is also recyclable after the crystallization utilizes again, greatly reduces cost, has realized being produced on a large scale.
Embodiment
Below in conjunction with embodiment the present invention is further described, need to prove, embodiment does not constitute the restriction that the present invention is required protection domain.
Embodiment 1
Raw material be stevioside A3 weight content greater than 40% Flos Chrysanthemi total glycosides mixture, wherein, stevioside A3 content 43%, stevioside content 50%, stevia rebaudianum disaccharide salidroside content 2%, stevioside B content 3%, stevioside C content 2%.The sugariness of stevioside A3 is 350～400 times of sucrose, pure taste, not back bitter taste.Stevioside A3 purity is high more, and price is high more.
A kind of from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, comprise the steps:
(1) mixed solvent configuration: be water by volume: ethanol: the ratio of methyl alcohol=0.5: 2: 1 disposes mixed solvent with water, ethanol and methanol mixed;
(2) crystallization: in the 250ml beaker, be raw material 10.0g, the mixed solvent 50ml that the ratio of 1g: 5ml takes by weighing in the solid-liquid mass volume ratio of Flos Chrysanthemi total glycosides mixture material and mixed solvent; Under the room temperature, rotating speed is stirring and dissolving 30min under the 60rpm magnetic agitation; In beaker, add stevioside A3 crystal seed (this stevioside A3 crystal seed purity is 99%, purchases to be formed on the precious bio tech ltd in west, Shanghai) in the ratio of stevioside A3 gross weight 5% in the raw material.Gained solution places 4 ℃ ± 1 ℃ stirred crystallization, and the crystal time of separating out is 2h, is spinning 10min under the 3000rpm condition at rotating speed, gets crystal; Can liquid be removed through centrifugal, obtain crystal;
(3) separate: the gained crystal is with 50ml ethanol (95%; Volume percent) washing is 2 times; After each washing all at 3000rpm spinning 10min; Obtaining stevioside A3 weight is 3.01g, and calculate recovery rate is 70%, and wherein the recovery is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity of measuring stevioside A3 through HPLC is 88%.Isolating mother liquor is collected the back otherwise processed and is reclaimed.Gained stevioside A3 with the washing of the anhydrous methanol of 40ml after, 3000rpm spinning 10min again, crystal is with anhydrous methanol 40ml washed twice, further to remove impurities.Carry out vacuum-drying 10h in vacuum tightness under-the 0.02MPA then.It is 2.236g that dry back obtains stevioside A3 weight, and the recovery that calculates stevioside A3 is 52%, and the recovery of stevioside A3 is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity that HPLC measures gained stevioside A3 is 96.7%, and the product sealing is for use.
Among this embodiment; Obtain purity and be to need not recrystallization in the crystallisation process of 96.7% stevioside A3, only adopt one time of crystallization, and crystallization time is merely 2h; Tc is accomplished down at 4 ℃ ± 1 ℃; This is that the Chinese invention patent of CN200710025792.8 discloses a kind of method of from stevioside, extracting high pure rebaudioside A and compares with the patent No., carries out recrystallization with methyl alcohol and isopropyl alcohol mixed solvent dissolving raw material stevioside ,-18 ℃ of Tc need; Crystallization time is 24h, and the crystallization crystal is also needed recrystallization process; And require crystal with after the pure water dissolving again membrane sepn could obtain stevioside A3 content 90%.Simplify technological operations such as recrystallization, membrane sepn from technology, saved 22h, improved Tc, need not to add expensive refrigeration equipment, reduced production cost from Tc from crystallization time.
Embodiment 2: raw material be stevioside A3 purity greater than 40% (weight) Flos Chrysanthemi total glycosides mixture, stevioside A3 content 40% wherein, stevioside content 50%, stevia rebaudianum disaccharide salidroside content 5%, stevioside B content 3%, stevioside C content 2%.The sugariness of stevioside A3 is 350～400 times of sucrose, pure taste, not back bitter taste.Stevioside A3 purity is high more, and price is high more.
A kind of from the stevioside mixture method of Crystallization Separation stevioside A3, comprise the steps:
(1) mixed solvent configuration: be water by volume: ethanol: the ratio of methyl alcohol=0.3: 1.6: 1 disposes mixed solvent with water, ethanol and methanol mixed;
(2) crystallization: in the 250ml beaker, be raw material 10.0g, the mixed solvent 50ml that the ratio of 1g: 5ml takes by weighing in the solid-liquid mass volume ratio of Flos Chrysanthemi total glycosides mixture material and mixed solvent; Under the room temperature, rotating speed is stirring and dissolving 30min under the 100rpm magnetic agitation; In beaker, add stevioside A3 crystal seed (this stevioside A3 crystal seed purity is 99%, purchases to be formed on the precious bio tech ltd in west, Shanghai) in the ratio of stevioside A3 gross weight 1% in the raw material.Gained solution places 15 ℃ ± 1 ℃ stirred crystallization, and the crystal time of separating out is 6h, is spinning 6min under the 3000rpm condition at rotating speed, gets crystal; Can liquid be removed through centrifugal, obtain crystal;
(3) separate: the gained crystal is with 50ml ethanol (95%; Volume percent) washing is 3 times; After each washing all at 3000rpm spinning 6min; Obtaining stevioside A3 weight is 2.72g, and calculate recovery rate is 68%, and wherein the recovery is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity of measuring stevioside A3 through HPLC is 82%.Isolating mother liquor is collected the back otherwise processed and is reclaimed.Gained stevioside A3 with the washing of the anhydrous methanol of 50ml after, 3000rpm spinning 6min again, crystal is with anhydrous methanol 50ml washed twice, further to remove impurities.Carry out vacuum-drying 10h in vacuum tightness under-the 0.04MPA then.It is 2.00g that dry back obtains stevioside A3 weight, and the recovery that calculates stevioside A3 is 50%, and the recovery of stevioside A3 is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity that HPLC measures gained stevioside A3 is 97.5%, and the product sealing is for use.
Embodiment 3
Raw material be stevioside A3 weight content greater than 40% Flos Chrysanthemi total glycosides mixture, wherein, stevioside A3 content 90%, stevioside content 7%, stevia rebaudianum disaccharide salidroside content 1%, stevioside B content 1%, stevioside C content 1%.The sugariness of stevioside A3 is 350～400 times of sucrose, pure taste, not back bitter taste.Stevioside A3 purity is high more, and price is high more.
A kind of from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, comprise the steps:
(1) mixed solvent configuration: be water by volume: ethanol: the ratio of methyl alcohol=0.8: 3: 1 disposes mixed solvent with water, ethanol and methanol mixed;
(2) crystallization: in the 250ml beaker, be raw material 10.0g, the mixed solvent 30ml that the ratio of 1g: 3ml takes by weighing in the solid-liquid mass volume ratio of Flos Chrysanthemi total glycosides mixture material and mixed solvent; Under the room temperature, rotating speed is stirring and dissolving 10min under the 60rpm magnetic agitation; In beaker, add stevioside A3 crystal seed (this stevioside A3 crystal seed purity is 99%, purchases to be formed on the precious bio tech ltd in west, Shanghai) in the ratio of stevioside A3 gross weight 3% in the raw material.Gained solution places 20 ℃ ± 1 ℃ stirred crystallization, and the crystal time of separating out is 4h, is spinning 8min under the 2500rpm condition at rotating speed, gets crystal; Can liquid be removed through centrifugal, obtain crystal;
(3) separate: the gained crystal is with twice of 50ml absolute ethanol washing; After each washing all at 2500rpm spinning 8min; Obtaining stevioside A3 weight is 6.12g, and calculate recovery rate is 65%, and wherein the recovery is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity of measuring stevioside A3 through HPLC is 86%.Isolating mother liquor is collected the back otherwise processed and is reclaimed.Gained stevioside A3 with the washing of the anhydrous methanol of 10ml after, 2500rpm spinning 8min again, crystal is with anhydrous methanol 10ml washed twice, further to remove impurities.Carry out vacuum-drying 10h in vacuum tightness under-the 0.02MPA then.It is 4.32g that dry back obtains stevioside A3 weight, and the recovery that calculates stevioside A3 is 48%, and the recovery of stevioside A3 is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity that HPLC measures gained stevioside A3 is 95.2%, and the product sealing is for use.
Embodiment 4
Raw material be stevioside A3 weight content greater than 40% Flos Chrysanthemi total glycosides mixture, wherein, stevioside A3 content 60%, stevioside content 30%, stevia rebaudianum disaccharide salidroside content 5%, stevioside B content 3%, stevioside C content 2%.The sugariness of stevioside A3 is 350～400 times of sucrose, pure taste, not back bitter taste.Stevioside A3 purity is high more, and price is high more.
A kind of from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, comprise the steps:
(1) mixed solvent configuration: be water by volume: ethanol: the ratio of methyl alcohol=0.6: 2: 1 disposes mixed solvent with water, ethanol and methanol mixed;
(2) crystallization: in the 250ml beaker, be raw material 10.0g, the mixed solvent 50ml that the ratio of 1g: 5ml takes by weighing in the solid-liquid mass volume ratio of Flos Chrysanthemi total glycosides mixture material and mixed solvent; Under the room temperature, rotating speed is stirring and dissolving 15min under the 60rpm magnetic agitation; In beaker, add stevioside A3 crystal seed (this stevioside A3 crystal seed purity is 99%, purchases to be formed on the precious bio tech ltd in west, Shanghai) in the ratio of stevioside A3 gross weight 2% in the raw material.Gained solution places 10 ℃ ± 1 ℃ stirred crystallization, and the crystal time of separating out is 5h, is spinning 15min under the 2000rpm condition at rotating speed, gets crystal; Can liquid be removed through centrifugal, obtain crystal;
(3) separate: the gained crystal is with 50ml ethanol (95%; Volume percent) washing is 1 time; After each washing all at 2000rpm spinning 15min; Obtaining stevioside A3 weight is 4.26g, and calculate recovery rate is 71%, and wherein the recovery is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity of measuring stevioside A3 through HPLC is 85%.Isolating mother liquor is collected the back otherwise processed and is reclaimed.Gained stevioside A3 with the washing of the anhydrous methanol of 30ml after, 2000rpm spinning 15min again, crystal washs 1 time with anhydrous methanol 30ml, further to remove impurities.Carry out vacuum-drying 10h in vacuum tightness under-the 0.03MPA then.It is 3.24g that dry back obtains stevioside A3 weight, and the recovery that calculates stevioside A3 is 54%, and the recovery of stevioside A3 is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity that HPLC measures gained stevioside A3 is 99.2%, and the product sealing is for use.
Embodiment 5
Raw material be stevioside A3 weight content greater than 40% Flos Chrysanthemi total glycosides mixture, wherein, stevioside A3 content 75%, stevioside content 20%, stevia rebaudianum disaccharide salidroside content 1%, stevioside B content 3%, stevioside C content 1%.The sugariness of stevioside A3 is 350～400 times of sucrose, pure taste, not back bitter taste.Stevioside A3 purity is high more, and price is high more.
A kind of from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, comprise the steps:
(1) mixed solvent configuration: be water by volume: ethanol: the ratio of methyl alcohol=0.2: 2: 1 disposes mixed solvent with water, ethanol and methanol mixed;
(2) crystallization: in the 250ml beaker, be raw material 10.0g, the mixed solvent 40ml that the ratio of 1g: 4ml takes by weighing in the solid-liquid mass volume ratio of Flos Chrysanthemi total glycosides mixture material and mixed solvent; Under the room temperature, rotating speed is stirring and dissolving 30min under the 60rpm magnetic agitation; In beaker, add stevioside A3 crystal seed (this stevioside A3 crystal seed purity is 99%, purchases to be formed on the precious bio tech ltd in west, Shanghai) in the ratio of stevioside A3 gross weight 5% in the raw material.Gained solution places 4 ℃ ± 1 ℃ stirred crystallization, and the crystal time of separating out is 2h, is spinning 10min under the 3000rpm condition at rotating speed, gets crystal; Can liquid be removed through centrifugal, obtain crystal;
(3) separate: the gained crystal is with 50ml absolute ethanol washing 3 times; After each washing all at 3000rpm spinning 10min; Obtaining stevioside A3 weight is 4.95g, and calculate recovery rate is 66%, and wherein the recovery is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity of measuring stevioside A3 through HPLC is 90%.Isolating mother liquor is collected the back otherwise processed and is reclaimed.Gained stevioside A3 with the anhydrous methanol of 50ml washing 1 time after, 3000rpm spinning 10min again.Carry out vacuum-drying 10h in vacuum tightness under-the 0.04MPA then.It is 4.65g that dry back obtains stevioside A3 weight, and the recovery that calculates stevioside A3 is 62%, and the recovery of stevioside A3 is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity that HPLC measures gained stevioside A3 is 99.9%, and the product sealing is for use.
Embodiment 6
Raw material be stevioside A3 weight content greater than 40% Flos Chrysanthemi total glycosides mixture, wherein, stevioside A3 content 50%, stevioside content 45%, stevia rebaudianum disaccharide salidroside content 1%, stevioside B content 2%, stevioside C content 2%.The sugariness of stevioside A3 is 350～400 times of sucrose, pure taste, not back bitter taste.Stevioside A3 purity is high more, and price is high more.
A kind of from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, comprise the steps:
(1) mixed solvent configuration: be water by volume: ethanol: the ratio of methyl alcohol=0.5: 1: 1 disposes mixed solvent with water, ethanol and methanol mixed;
(2) crystallization: in the 250ml beaker, be raw material 10.0g, the mixed solvent 50ml that the ratio of 1g: 5ml takes by weighing in the solid-liquid mass volume ratio of Flos Chrysanthemi total glycosides mixture material and mixed solvent; Under the room temperature, rotating speed is stirring and dissolving 30min under the 60rpm magnetic agitation; In beaker, add stevioside A3 crystal seed (this stevioside A3 crystal seed purity is 99%, purchases to be formed on the precious bio tech ltd in west, Shanghai) in the ratio of stevioside A3 gross weight 5% in the raw material.Gained solution places 20 ℃ ± 1 ℃ stirred crystallization, and the crystal time of separating out is 5h, is spinning 10min under the 2000rpm condition at rotating speed, gets crystal; Can liquid be removed through centrifugal, obtain crystal;
(3) separate: the gained crystal is with 50ml ethanol (95%; Volume percent) washing is 3 times; After each washing all at 2000rpm spinning 10min; Obtaining stevioside A3 weight is 3.25g, and calculate recovery rate is 65%, and wherein the recovery is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity of measuring stevioside A3 through HPLC is 90%.Isolating mother liquor is collected the back otherwise processed and is reclaimed.Gained stevioside A3 with the washing of the anhydrous methanol of 30ml after, 3000rpm spinning 6min again, crystal washs 2 times with anhydrous methanol 30ml, further to remove impurities.Carry out vacuum-drying 10h in vacuum tightness under-the 0.02MPA then.It is 2.90g that dry back obtains stevioside A3 weight, and the recovery that calculates stevioside A3 is 58%, and the recovery of stevioside A3 is calculated as the actual stevioside A3 weight that obtains divided by the stevioside A3 weight in the raw material; The purity that HPLC measures gained stevioside A3 is 98.9%, and the product sealing is for use.
Claims (8)
1. the method for a Crystallization Separation stevioside A3 from the Flos Chrysanthemi total glycosides mixture is characterized in that comprising the steps:
(1) mixed solvent preparation: be water by volume: ethanol: methyl alcohol=0.2～0.8: 1～3: 1 ratio is prepared mixed solvent with water, ethanol and methanol mixed;
(2) crystallization: be that the ratio of 1g: 3ml～1g: 5ml joins Flos Chrysanthemi total glycosides mixture material and mixed solvent in the container and mixes in the Flos Chrysanthemi total glycosides mixture material and the solid-liquid mass volume ratio of mixed solvent; Stirring and dissolving 10～30min under the room temperature; Add stevioside A3 crystal seed; Spinning after temperature is 4 ℃～20 ℃ stirring 2～6h obtains crystalline product; Stevioside A3 crystal seed is a purity greater than 99% stevioside A3, the consumption of stevioside A3 crystal seed be in the Flos Chrysanthemi total glycosides mixture material stevioside A3 weight 1～5%; Said Flos Chrysanthemi total glycosides mixture material is a stevioside A3 weight content greater than 40% Flos Chrysanthemi total glycosides mixture;
(3) separate: the gained crystalline product with absolute ethanol washing after spinning, wash with anhydrous methanol again; After the spinning, vacuum-drying gets stevioside A3 product.
2. according to claim 1 from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3; It is characterized in that: by percentage to the quality; Stevioside A3 content 40～90% in the said Flos Chrysanthemi total glycosides mixture material, stevioside content 7～50%, stevia rebaudianum disaccharide salidroside content 1～5%; Stevioside B content 1～3%, stevioside C content 1～2%.
3. according to claim 1 from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, it is characterized in that: said ethanol is volumetric concentration greater than 95% aqueous ethanolic solution or absolute ethyl alcohol.
4. according to claim 1 from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, it is characterized in that: said spinning condition is under 2000～3000rpm rotating speed, centrifugal 6～15min.
5. according to claim 1 from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, it is characterized in that: said vacuum-drying in vacuum tightness be-0.04～-carry out under the 0.02MPA.
6. according to claim 1 from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, it is characterized in that: in the said anhydrous methanol washing, crystal and anhydrous methanol feed liquid mass volume ratio are 1g: 1ml～1g: 5ml.
7. according to claim 1 from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, it is characterized in that: the number of times of said anhydrous methanol washing is 1-3 time.
8. according to claim 1 from the Flos Chrysanthemi total glycosides mixture method of Crystallization Separation stevioside A3, it is characterized in that: the number of times of said washing with alcohol is 1-3 time.
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| CN104231017A (en) * | 2014-09-28 | 2014-12-24 | 晨光生物科技集团股份有限公司 | Method for improving quality of mother liquid glucose of stevioside |
| CN104548648A (en) * | 2014-10-08 | 2015-04-29 | 浙江大学 | Crystallizing device for preparing high-purity rebaudioside A by employing continuous purification, and control method of crystallizing device |
| CN117658833A (en) * | 2023-11-13 | 2024-03-08 | 河北广祥制药有限公司 | Mixed solvent for purifying L-epinephrine and salt thereof, and method for purifying L-epinephrine and salt thereof |
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| CN104548648A (en) * | 2014-10-08 | 2015-04-29 | 浙江大学 | Crystallizing device for preparing high-purity rebaudioside A by employing continuous purification, and control method of crystallizing device |
| CN117658833A (en) * | 2023-11-13 | 2024-03-08 | 河北广祥制药有限公司 | Mixed solvent for purifying L-epinephrine and salt thereof, and method for purifying L-epinephrine and salt thereof |
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