CN106046075A - Method for extracting stevioside from stevia rebaudiana leaves - Google Patents
Method for extracting stevioside from stevia rebaudiana leaves Download PDFInfo
- Publication number
- CN106046075A CN106046075A CN201610446983.0A CN201610446983A CN106046075A CN 106046075 A CN106046075 A CN 106046075A CN 201610446983 A CN201610446983 A CN 201610446983A CN 106046075 A CN106046075 A CN 106046075A
- Authority
- CN
- China
- Prior art keywords
- stevioside
- leaf
- stevlae rebaudianae
- folium stevlae
- mass fraction
- 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.)
- Withdrawn
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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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 method for extracting stevioside from stevia rebaudiana leaves. The method comprises the following steps of washing, soaking, drying stevia rebaudiana leaves and sieving to obtain stevia rebaudiana leaf powder; mixing the stevia rebaudiana leaf powder with water, adding complex enzyme, adjusting the pH value and heating by microwave, extracting and filtering by ultrasound to obtain an extracting solution and a filter residue; mixing the filter residue with diethyl ether, performing centrifugal separation to obtain a total extract; mixing the total extract with a ferric trichloride solution and a calcium hydroxide solution; after performing heating, heat preservation and cooling, mixing with a sodium hydroxide solution; after adjusting the pH value, mixing with an aluminum sulfate solution, after stirring, performing supercritical extraction to obtain an extract liquor; using AB-8 type macroporous resin to adsorb the extract liquor; performing elution, distillation, concentration and drying, so as to obtain a stevioside crude product; putting the stevioside crude product into water; ultrasonically dissolving and adding active aluminium oxide for adsorbing; and then filtering, washing, subsiding, combining filter liquor and washing liquor, and concentrating and drying.
Description
Technical field
The present invention relates to stevioside extractive technique field, particularly relate to the extraction side of stevioside in a kind of leaf of Folium Stevlae Rebaudianae
Method.
Background technology
Folium Stevlae Rebaudianae is to originate in the evergreen dwarf shrub between South America Paraguay plateau south latitude 25-26 degree, each by the world
Introduce a fine variety, containing a class stevioside material in its blade, be a class tetracylic diterpene derivatives, mainly by stevioside, sweet
8 kinds of glucosides compositions such as echinacoside A, stevioside B and stevioside C, its sugariness is about 300 times of sucrose.Research shows, stevioside
Glycosides has high sugariness, low in calories, and without the feature of obvious toxic-side effects, it can suppress hyperglycemia, hypertension, and has antiinflammatory, anti-swollen
Tumor, antidiarrheal diuresis and assist immunoregulatory effect.At present, South America, Japan and China using stevioside as one
Natural sweetener is widely used in Food & Drink.Stevioside traditional extraction technique in the industrial production has multiple,
Including hot water extraction method, dialysis, enzyme process, supercritical CO2Extraction method, superelevation platen press, backflow set lifting manipulation, counter-current etc., but
Often there is the defect that extraction ratio is low in these methods.
Summary of the invention
The technical problem existed based on background technology, the present invention proposes the extraction side of stevioside in a kind of leaf of Folium Stevlae Rebaudianae
Method, its process is simple, mild condition, and extraction ratio is high.
The extracting method of stevioside in a kind of leaf of Folium Stevlae Rebaudianae that the present invention proposes, comprises the following steps:
S1, leaf of Folium Stevlae Rebaudianae clear water is rinsed well, be subsequently placed in dehydrated alcohol immersion 0.5-1.5h, be dried after taking-up
Being 5-6wt% to moisture content, grinding and sieving obtains leaf of Folium Stevlae Rebaudianae powder；
S2, by leaf of Folium Stevlae Rebaudianae powder and water, ratio for 1:5-10 in mass ratio is mixed homogeneously, and is subsequently adding compound enzyme, its
In, the quality of compound enzyme is the 0.2-0.25% of leaf of Folium Stevlae Rebaudianae opaque amount, and regulation pH value is to 3-4, and then microwave heating is to 35-45
DEG C insulated and stirred 5-10min, the most ultrasonic 20-50min, obtain extracting solution and filtering residue after filtration；
S3, by filtering residue and ether be in mass ratio 1:3-5 ratio addition centrifuge in, be centrifuged after stirring point
From, wherein, centrifugal speed is 2500-3500r/min, and the centrifugal time is 50-100min, collects after standing 15-30min
Layer clear liquid, merges with the extracting solution in S2 and obtains total extracting solution；
S4, by mass fraction be the liquor ferri trichloridi of 20-30%, mass fraction be the aqua calcis of 20-30%
Volume ratio mix homogeneously with total extracting solution presses 5-10:1-3:50-80, is heated to 45-50 DEG C, is incubated 25-30min, the coldest
But to room temperature, material A is obtained；Material A is mixed by the volume ratio of 1:3-5 with the sodium hydroxide solution that mass fraction is 3-8%
Uniformly, regulation pH value obtains material B after being 7-7.5；It is that the aluminum sulfate solution of 1-2% is by 5-15:1 by material B and mass fraction
Volume ratio mix homogeneously, carry out supercritical extraction and be extracted liquid, wherein, in supercritical extraction process after stirring 30-50min
In, the pressure of extraction is 0.65-0.8MPa, and the temperature of extraction is 90-110 DEG C, and the time of extraction is 15-25min；
S5, extract is adsorbed by AB-8 type macroporous resin, then wash with the ethanol that mass fraction is 65-75%
Take off to effluent without sweet taste, distill through decompression, concentrate, be dried to obtain stevioside crude product；
S6, being added to the water by stevioside crude product, wherein, the weight of water is 15-30 times of stevioside crude product weight, super
Sound adds activated alumina after dissolving, and wherein, the weight of activated alumina is 4-8 times of stevioside crude product weight, at 38-45
15-35min is adsorbed, through filtering, concentrate, be dried to obtain described stevioside at DEG C.
Preferably, in S1, leaf of Folium Stevlae Rebaudianae clear water is rinsed well, be subsequently placed in dehydrated alcohol immersion 0.8-
1.2h, being dried at 60-70 DEG C after taking-up to moisture content is 5-6wt%, crosses 50-60 mesh sieve and obtain leaf of Folium Stevlae Rebaudianae powder after pulverizing.
Preferably, in S2, described compound enzyme is that cellulase, pectase are by weight the mixture for 1-5:2-6.
Preferably, in S2, in microwave heating process, the power of microwave is 520-580W.
Preferably, in S2, in ultrasonic procedure, ultrasonic power is 120-200W.
Preferably, the extracting method of stevioside in described leaf of Folium Stevlae Rebaudianae, comprise the following steps:
S1, leaf of Folium Stevlae Rebaudianae clear water is rinsed well, be subsequently placed in dehydrated alcohol immersion 1h, dry at 65 DEG C after taking-up
Dry is 5.5wt% to moisture content, crosses 55 mesh sieves and obtain leaf of Folium Stevlae Rebaudianae powder after pulverizing；
S2, by leaf of Folium Stevlae Rebaudianae powder and water, ratio for 1:7 in mass ratio is mixed homogeneously, and is subsequently adding compound enzyme, wherein, and institute
State compound enzyme be cellulase, pectase by weight for the mixture of 3:5, the quality of compound enzyme is leaf of Folium Stevlae Rebaudianae opaque amount
0.22%, regulation pH value is to 3.5, and then microwave heating is to 40 DEG C of insulated and stirred 8min, and wherein, the power of microwave is 550W, so
Rear ultrasonic 30min, ultrasonic power is 150W, obtains extracting solution and filtering residue after filtration；
S3, by filtering residue and ether be in mass ratio 1:4 ratio addition centrifuge in, be centrifuged after stirring point
From, wherein, centrifugal speed is 3000r/min, and the centrifugal time is 70min, collects the supernatant, with S2 after standing 25min
In extracting solution merge obtain total extracting solution；
S4, liquor ferri trichloridi, mass fraction that mass fraction is 25% are the aqua calcis of 28% and always carry
Take liquid by the volume ratio mix homogeneously of 7:2:60, be heated to 48 DEG C, be incubated 29min, after naturally cooling to room temperature, obtain material A；
Material A being mixed homogeneously by the volume ratio of 1:4 with the sodium hydroxide solution that mass fraction is 6%, regulation pH value is to obtain after 7.2
Material B；Material B is mixed homogeneously by the volume ratio of 8.5:1 with the aluminum sulfate solution that mass fraction is 1.5%, after stirring 40min
Carrying out supercritical extraction and be extracted liquid, wherein, during supercritical extraction, the pressure of extraction is 0.75MPa, the temperature of extraction
Degree is 100 DEG C, and the time of extraction is 20min；
S5, extract is adsorbed by AB-8 type macroporous resin, be then the ethanol elution of 70% with mass fraction
To effluent without sweet taste, distill through decompression, concentrate, be dried to obtain stevioside crude product；
S6, being added to the water by stevioside crude product, wherein, the weight of water is 25 times of stevioside crude product weight, ultrasonic
Adding activated alumina after dissolving, wherein, the weight of activated alumina is 6 times of stevioside crude product weight, inhales at 42 DEG C
Attached 25min, through filtering, concentrate, be dried to obtain described stevioside.
In the present invention, first carry out leaf of Folium Stevlae Rebaudianae rinsing being placed in dehydrated alcohol immersion, eliminated leaf of Folium Stevlae Rebaudianae
The impurity on surface, adds compound enzyme after pulverizing, the constituent (cellulose, hemicellulose and pectic substance) to cell wall is carried out
Hydrolysis or degraded, coordinate microwave and ultrasonic cooperation to extract, farthest improve stripping quantity and the yield of steviol glycosides,
Reduce glucoside residual quantity in leaf slag, shorten extraction time simultaneously, reduce Extracting temperature, it is to avoid sweetleaf during subsequent extracted
More dissolution such as chrysanthemum Ye Zhongyi a little low temperature indissoluble material such as pigment, pectin, cellulose etc., is conducive to improving the pure of stevioside
Degree, by controlling the consumption of compound enzyme and microwave and ultrasonic technological parameter, farthest remains having of leaf of Folium Stevlae Rebaudianae
Effect composition, and improve the repeatability of extraction；Add liquor ferri trichloridi and aqua calcis afterwards as flocculant, and
Adding aluminum sulfate, by controlling technological parameter, the flocculating effect making flocculant is optimal, and the clear liquid light transmittance after flocculation is maximum,
The loss rate of glucosides is minimum；Carry out adsorbing and adsorbing with activated alumina with AB-8 type macroporous resin afterwards, improve sweet
The purity of inulin glycosides and whiteness, make the purity of stevioside reach more than 93.6%.
Detailed description of the invention
Below, by specific embodiment, technical scheme is described in detail.
Embodiment 1
The extracting method of stevioside in a kind of leaf of Folium Stevlae Rebaudianae that the present invention proposes, comprises the following steps:
S1, leaf of Folium Stevlae Rebaudianae clear water is rinsed well, be subsequently placed in dehydrated alcohol immersion 0.5h, be dried after taking-up to containing
Water rate is 6wt%, and grinding and sieving obtains leaf of Folium Stevlae Rebaudianae powder；
S2, by leaf of Folium Stevlae Rebaudianae powder and water, ratio for 1:5 in mass ratio is mixed homogeneously, and is subsequently adding compound enzyme, wherein, multiple
The quality of synthase is the 0.25% of leaf of Folium Stevlae Rebaudianae opaque amount, and regulation pH value is to 3, and then microwave heating is to 45 DEG C of insulated and stirred
5min, the most ultrasonic 50min, obtain extracting solution and filtering residue after filtration；
S3, by filtering residue and ether be in mass ratio 1:3 ratio addition centrifuge in, be centrifuged after stirring point
From, wherein, centrifugal speed is 3500r/min, and the centrifugal time is 50min, collects the supernatant, with S2 after standing 30min
In extracting solution merge obtain total extracting solution；
S4, liquor ferri trichloridi, mass fraction that mass fraction is 20% are the aqua calcis of 30% and always carry
Take liquid by the volume ratio mix homogeneously of 5:3:50, be heated to 50 DEG C, be incubated 25min, after naturally cooling to room temperature, obtain material A；
Material A being mixed homogeneously by the volume ratio of 1:3 with the sodium hydroxide solution that mass fraction is 8%, regulation pH value is to obtain after 7.5
Material B；Being mixed homogeneously by the volume ratio of 15:1 with the aluminum sulfate solution that mass fraction is 1% by material B, 30min is laggard in stirring
Row supercritical extraction is extracted liquid, and wherein, during supercritical extraction, the pressure of extraction is 0.8MPa, the temperature of extraction
Being 90 DEG C, the time of extraction is 25min；
S5, extract is adsorbed by AB-8 type macroporous resin, be then the ethanol elution of 65% with mass fraction
To effluent without sweet taste, distill through decompression, concentrate, be dried to obtain stevioside crude product；
S6, being added to the water by stevioside crude product, wherein, the weight of water is 30 times of stevioside crude product weight, ultrasonic
Adding activated alumina after dissolving, wherein, the weight of activated alumina is 4 times of stevioside crude product weight, inhales at 45 DEG C
Attached 15min, through filtering, concentrate, be dried to obtain described stevioside.
Embodiment 2
The extracting method of stevioside in a kind of leaf of Folium Stevlae Rebaudianae that the present invention proposes, comprises the following steps:
S1, leaf of Folium Stevlae Rebaudianae clear water is rinsed well, be subsequently placed in dehydrated alcohol immersion 1.5h, be dried after taking-up to containing
Water rate is 5wt%, and grinding and sieving obtains leaf of Folium Stevlae Rebaudianae powder；
S2, by leaf of Folium Stevlae Rebaudianae powder and water, ratio for 1:10 in mass ratio is mixed homogeneously, and is subsequently adding compound enzyme, wherein,
The quality of compound enzyme is the 0.2% of leaf of Folium Stevlae Rebaudianae opaque amount, and regulation pH value is to 4, and then microwave heating is to 35 DEG C of insulated and stirred
10min, the most ultrasonic 20min, obtain extracting solution and filtering residue after filtration；
S3, by filtering residue and ether be in mass ratio 1:5 ratio addition centrifuge in, be centrifuged after stirring point
From, wherein, centrifugal speed is 2500r/min, and the centrifugal time is 100min, collects the supernatant, with S2 after standing 15min
In extracting solution merge obtain total extracting solution；
S4, liquor ferri trichloridi, mass fraction that mass fraction is 30% are the aqua calcis of 20% and always carry
Take liquid by the volume ratio mix homogeneously of 10:1:80, be heated to 45 DEG C, be incubated 30min, after naturally cooling to room temperature, obtain material A；
Material A being mixed homogeneously by the volume ratio of 1:5 with the sodium hydroxide solution that mass fraction is 3%, regulation pH value is to obtain thing after 7
Material B；Material B is mixed homogeneously by the volume ratio of 5:1 with the aluminum sulfate solution that mass fraction is 2%, surpasses after stirring 50min
Critical extract being obtained by extraction, wherein, during supercritical extraction, the pressure of extraction is 0.65MPa, and the temperature of extraction is
110 DEG C, the time of extraction is 15min；
S5, extract is adsorbed by AB-8 type macroporous resin, be then the ethanol elution of 75% with mass fraction
To effluent without sweet taste, distill through decompression, concentrate, be dried to obtain stevioside crude product；
S6, being added to the water by stevioside crude product, wherein, the weight of water is 15 times of stevioside crude product weight, ultrasonic
Adding activated alumina after dissolving, wherein, the weight of activated alumina is 8 times of stevioside crude product weight, inhales at 38 DEG C
Attached 35min, through filtering, concentrate, be dried to obtain described stevioside.
Embodiment 3
The extracting method of stevioside in a kind of leaf of Folium Stevlae Rebaudianae that the present invention proposes, comprises the following steps:
S1, leaf of Folium Stevlae Rebaudianae clear water is rinsed well, be subsequently placed in dehydrated alcohol immersion 0.8h, after taking-up at 60 DEG C
Being dried to moisture content is 6wt%, crosses 50 mesh sieves and obtain leaf of Folium Stevlae Rebaudianae powder after pulverizing；
S2, by leaf of Folium Stevlae Rebaudianae powder and water, ratio for 1:6 in mass ratio is mixed homogeneously, and is subsequently adding compound enzyme, wherein, and institute
State compound enzyme be cellulase, pectase by weight for the mixture of 5:6, the quality of compound enzyme is leaf of Folium Stevlae Rebaudianae opaque amount
0.24%, regulation pH value is to 3.2, and then microwave heating is to 43 DEG C of insulated and stirred 6.5min, wherein, in microwave heating process,
The power of microwave is 580W, the most ultrasonic 40min, and wherein, ultrasonic power is 120W, obtains extracting solution and filtering residue after filtration；
S3, by filtering residue and ether be in mass ratio 1:3.2 ratio addition centrifuge in, be centrifuged after stirring point
From, wherein, centrifugal speed is 3300r/min, and the centrifugal time is 65min, collects the supernatant, with S2 after standing 28min
In extracting solution merge obtain total extracting solution；
S4, liquor ferri trichloridi, mass fraction that mass fraction is 22% are the aqua calcis of 29% and always carry
Take liquid by the volume ratio mix homogeneously of 6:1.8:55, be heated to 48 DEG C, be incubated 26min, after naturally cooling to room temperature, obtain material
A；Material A is mixed homogeneously by the volume ratio of 1:3.5 with the sodium hydroxide solution that mass fraction is 7%, after regulation pH value is 7.4
Obtain material B；Material B is mixed homogeneously by the volume ratio of 12:1 with the aluminum sulfate solution that mass fraction is 1.2%, stirring
Carrying out supercritical extraction after 35min and be extracted liquid, wherein, during supercritical extraction, the pressure of extraction is 0.75MPa,
The temperature of extraction is 95 DEG C, and the time of extraction is 24min；
S5, extract is adsorbed by AB-8 type macroporous resin, be then the ethanol elution of 67% with mass fraction
To effluent without sweet taste, distill through decompression, concentrate, be dried to obtain stevioside crude product；
S6, being added to the water by stevioside crude product, wherein, the weight of water is 25 times of stevioside crude product weight, ultrasonic
Adding activated alumina after dissolving, wherein, the weight of activated alumina is 5 times of stevioside crude product weight, inhales at 42 DEG C
Attached 30min, through filtering, concentrate, be dried to obtain described stevioside.
Embodiment 4
The extracting method of stevioside in a kind of leaf of Folium Stevlae Rebaudianae that the present invention proposes, comprises the following steps:
S1, leaf of Folium Stevlae Rebaudianae clear water is rinsed well, be subsequently placed in dehydrated alcohol immersion 1.2h, after taking-up at 70 DEG C
Being dried to moisture content is 5wt%, crosses 60 mesh sieves and obtain leaf of Folium Stevlae Rebaudianae powder after pulverizing；
S2, by leaf of Folium Stevlae Rebaudianae powder and water, ratio for 1:9 in mass ratio is mixed homogeneously, and is subsequently adding compound enzyme, wherein, and institute
State compound enzyme be cellulase, pectase by weight for the mixture of 1:2, the quality of compound enzyme is leaf of Folium Stevlae Rebaudianae opaque amount
0.22%, regulation pH value is to 3.8, and then microwave heating is to 36 DEG C of insulated and stirred 8min, wherein, in microwave heating process, micro-
The power of ripple is 520W, the most ultrasonic 25min, and wherein, ultrasonic power is 200W, obtains extracting solution and filtering residue after filtration；
S3, by filtering residue and ether be in mass ratio 1:4.8 ratio addition centrifuge in, be centrifuged after stirring point
From, wherein, centrifugal speed is 2650r/min, and the centrifugal time is 80min, collects the supernatant, with S2 after standing 20min
In extracting solution merge obtain total extracting solution；
S4, liquor ferri trichloridi, mass fraction that mass fraction is 28% are the aqua calcis of 25% and always carry
Take liquid by the volume ratio mix homogeneously of 9:1.2:78, be heated to 46 DEG C, be incubated 28min, after naturally cooling to room temperature, obtain material
A；Material A is mixed homogeneously by the volume ratio of 1:4.8 with the sodium hydroxide solution that mass fraction is 4%, after regulation pH value is 7.2
Obtain material B；Material B is mixed homogeneously by the volume ratio of 7:1 with the aluminum sulfate solution that mass fraction is 1.8%, stirs 48min
After carry out supercritical extraction and be extracted liquid, wherein, during supercritical extraction, the pressure of extraction is 0.7MPa, extraction
Temperature is 100 DEG C, and the time of extraction is 19min；
S5, extract is adsorbed by AB-8 type macroporous resin, be then the ethanol elution of 74% with mass fraction
To effluent without sweet taste, distill through decompression, concentrate, be dried to obtain stevioside crude product；
S6, being added to the water by stevioside crude product, wherein, the weight of water is 18 times of stevioside crude product weight, ultrasonic
Adding activated alumina after dissolving, wherein, the weight of activated alumina is 7 times of stevioside crude product weight, inhales at 40 DEG C
Attached 20min, through filtering, concentrate, be dried to obtain described stevioside.
Embodiment 5
The extracting method of stevioside in a kind of leaf of Folium Stevlae Rebaudianae that the present invention proposes, comprises the following steps:
S1, leaf of Folium Stevlae Rebaudianae clear water is rinsed well, be subsequently placed in dehydrated alcohol immersion 1h, dry at 65 DEG C after taking-up
Dry is 5.5wt% to moisture content, crosses 55 mesh sieves and obtain leaf of Folium Stevlae Rebaudianae powder after pulverizing；
S2, by leaf of Folium Stevlae Rebaudianae powder and water, ratio for 1:7 in mass ratio is mixed homogeneously, and is subsequently adding compound enzyme, wherein, and institute
State compound enzyme be cellulase, pectase by weight for the mixture of 3:5, the quality of compound enzyme is leaf of Folium Stevlae Rebaudianae opaque amount
0.22%, regulation pH value is to 3.5, and then microwave heating is to 40 DEG C of insulated and stirred 8min, and wherein, the power of microwave is 550W, so
Rear ultrasonic 30min, ultrasonic power is 150W, obtains extracting solution and filtering residue after filtration；
S3, by filtering residue and ether be in mass ratio 1:4 ratio addition centrifuge in, be centrifuged after stirring point
From, wherein, centrifugal speed is 3000r/min, and the centrifugal time is 70min, collects the supernatant, with S2 after standing 25min
In extracting solution merge obtain total extracting solution；
S4, liquor ferri trichloridi, mass fraction that mass fraction is 25% are the aqua calcis of 28% and always carry
Take liquid by the volume ratio mix homogeneously of 7:2:60, be heated to 48 DEG C, be incubated 29min, after naturally cooling to room temperature, obtain material A；
Material A being mixed homogeneously by the volume ratio of 1:4 with the sodium hydroxide solution that mass fraction is 6%, regulation pH value is to obtain after 7.2
Material B；Material B is mixed homogeneously by the volume ratio of 8.5:1 with the aluminum sulfate solution that mass fraction is 1.5%, after stirring 40min
Carrying out supercritical extraction and be extracted liquid, wherein, during supercritical extraction, the pressure of extraction is 0.75MPa, the temperature of extraction
Degree is 100 DEG C, and the time of extraction is 20min；
S5, extract is adsorbed by AB-8 type macroporous resin, be then the ethanol elution of 70% with mass fraction
To effluent without sweet taste, distill through decompression, concentrate, be dried to obtain stevioside crude product；
S6, being added to the water by stevioside crude product, wherein, the weight of water is 25 times of stevioside crude product weight, ultrasonic
Adding activated alumina after dissolving, wherein, the weight of activated alumina is 6 times of stevioside crude product weight, inhales at 42 DEG C
Attached 25min, through filtering, concentrate, be dried to obtain described stevioside.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, according to technical scheme and
Inventive concept equivalent or change in addition, all should contain within protection scope of the present invention.
Claims (6)
1. the extracting method of stevioside in a leaf of Folium Stevlae Rebaudianae, it is characterised in that comprise the following steps:
S1, leaf of Folium Stevlae Rebaudianae clear water is rinsed well, be subsequently placed in dehydrated alcohol immersion 0.5-1.5h, be dried after taking-up to containing
Water rate is 5-6wt%, and grinding and sieving obtains leaf of Folium Stevlae Rebaudianae powder；
S2, by leaf of Folium Stevlae Rebaudianae powder and water, ratio for 1:5-10 in mass ratio is mixed homogeneously, and is subsequently adding compound enzyme, wherein, multiple
The quality of synthase is the 0.2-0.25% of leaf of Folium Stevlae Rebaudianae opaque amount, and regulation pH value is to 3-4, and then microwave heating is to 35-45 DEG C of guarantor
Temperature stirring 5-10min, the most ultrasonic 20-50min, obtain extracting solution and filtering residue after filtration；
S3, by filtering residue and ether be in mass ratio 1:3-5 ratio addition centrifuge in, carry out centrifugation after stirring,
Wherein, centrifugal speed is 2500-3500r/min, and the centrifugal time is 50-100min, collects upper strata after standing 15-30min
Clear liquid, merges with the extracting solution in S2 and obtains total extracting solution；
S4, by mass fraction be the liquor ferri trichloridi of 20-30%, mass fraction be the aqua calcis of 20-30% and total
Extracting solution presses the volume ratio mix homogeneously of 5-10:1-3:50-80, is heated to 45-50 DEG C, is incubated 25-30min, naturally cools to
Material A is obtained after room temperature；Material A is mixed all by the volume ratio of 1:3-5 with the sodium hydroxide solution that mass fraction is 3-8%
Even, regulation pH value is to obtain material B after 7-7.5；It is that the aluminum sulfate solution of 1-2% is by 5-15:1's by material B and mass fraction
Volume ratio mix homogeneously, carries out supercritical extraction after stirring 30-50min and is extracted liquid, wherein, in supercritical extraction process
In, the pressure of extraction is 0.65-0.8MPa, and the temperature of extraction is 90-110 DEG C, and the time of extraction is 15-25min；
S5, extract is adsorbed by AB-8 type macroporous resin, then with the ethanol elution that mass fraction is 65-75% extremely
Effluent, without sweet taste, distills through decompression, concentrate, is dried to obtain stevioside crude product；
S6, being added to the water by stevioside crude product, wherein, the weight of water is 15-30 times of stevioside crude product weight, ultrasonic molten
Adding activated alumina after solution, wherein, the weight of activated alumina is 4-8 times of stevioside crude product weight, at 38-45 DEG C
Absorption 15-35min, through filtering, concentrate, be dried to obtain described stevioside.
The extracting method of stevioside in leaf of Folium Stevlae Rebaudianae the most according to claim 1, it is characterised in that in S1, by sweetleaf
Chrysanthemum leaf clear water is rinsed well, is subsequently placed in dehydrated alcohol immersion 0.8-1.2h, is dried to aqueous after taking-up at 60-70 DEG C
Rate is 5-6wt%, crosses 50-60 mesh sieve and obtain leaf of Folium Stevlae Rebaudianae powder after pulverizing.
The extracting method of stevioside in leaf of Folium Stevlae Rebaudianae the most according to claim 1 or claim 2, it is characterised in that in S2, described
Compound enzyme is that cellulase, pectase are by weight the mixture for 1-5:2-6.
4. according to the extracting method of stevioside in leaf of Folium Stevlae Rebaudianae according to any one of claim 1-3, it is characterised in that at S2
In, in microwave heating process, the power of microwave is 520-580W.
5. according to the extracting method of stevioside in leaf of Folium Stevlae Rebaudianae according to any one of claim 1-4, it is characterised in that at S2
In, in ultrasonic procedure, ultrasonic power is 120-200W.
6. according to the extracting method of stevioside in leaf of Folium Stevlae Rebaudianae according to any one of claim 1-5, it is characterised in that include
Following steps:
S1, leaf of Folium Stevlae Rebaudianae clear water is rinsed well, is subsequently placed in dehydrated alcohol immersion 1h, be dried at 65 DEG C after taking-up to
Moisture content is 5.5wt%, crosses 55 mesh sieves and obtain leaf of Folium Stevlae Rebaudianae powder after pulverizing；
S2, by leaf of Folium Stevlae Rebaudianae powder and water, ratio for 1:7 in mass ratio is mixed homogeneously, and is subsequently adding compound enzyme, wherein, described multiple
Synthase be cellulase, pectase by weight for the mixture of 3:5, the quality of compound enzyme is leaf of Folium Stevlae Rebaudianae opaque amount
0.22%, regulation pH value is to 3.5, and then microwave heating is to 40 DEG C of insulated and stirred 8min, and wherein, the power of microwave is 550W, so
Rear ultrasonic 30min, ultrasonic power is 150W, obtains extracting solution and filtering residue after filtration；
S3, by filtering residue and ether be in mass ratio 1:4 ratio addition centrifuge in, carry out centrifugation after stirring, its
In, centrifugal speed is 3000r/min, and the centrifugal time is 70min, collects carrying in the supernatant, with S2 after standing 25min
Take liquid merging and obtain total extracting solution；
S4, it is the aqua calcis of 28% and total extracting solution by liquor ferri trichloridi that mass fraction is 25%, mass fraction
By the volume ratio mix homogeneously of 7:2:60, it is heated to 48 DEG C, is incubated 29min, after naturally cooling to room temperature, obtains material A；By thing
Material A is mixed homogeneously by the volume ratio of 1:4 with the sodium hydroxide solution that mass fraction is 6%, and regulating pH value is to obtain material after 7.2
B；Material B is mixed homogeneously by the volume ratio of 8.5:1 with the aluminum sulfate solution that mass fraction is 1.5%, carries out after stirring 40min
Supercritical extraction is extracted liquid, and wherein, during supercritical extraction, the pressure of extraction is 0.75MPa, and the temperature of extraction is
100 DEG C, the time of extraction is 20min；
S5, extract is adsorbed by AB-8 type macroporous resin, then with the ethanol elution that mass fraction is 70% to stream
Go out liquid without sweet taste, distill through decompression, concentrate, be dried to obtain stevioside crude product；
S6, being added to the water by stevioside crude product, wherein, the weight of water is 25 times of stevioside crude product weight, ultrasonic dissolution
Rear addition activated alumina, wherein, the weight of activated alumina is 6 times of stevioside crude product weight, adsorbs at 42 DEG C
25min, through filtering, concentrate, be dried to obtain described stevioside.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610446983.0A CN106046075A (en) | 2016-06-17 | 2016-06-17 | Method for extracting stevioside from stevia rebaudiana leaves |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610446983.0A CN106046075A (en) | 2016-06-17 | 2016-06-17 | Method for extracting stevioside from stevia rebaudiana leaves |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106046075A true CN106046075A (en) | 2016-10-26 |
Family
ID=57167785
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610446983.0A Withdrawn CN106046075A (en) | 2016-06-17 | 2016-06-17 | Method for extracting stevioside from stevia rebaudiana leaves |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106046075A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106632539A (en) * | 2016-11-03 | 2017-05-10 | 明光市大全甜叶菊专业合作社 | A stevia rebaudiana glucoside extracting method |
| CN106674307A (en) * | 2016-11-03 | 2017-05-17 | 明光市大全甜叶菊专业合作社 | Method for extracting stevioside from stevia rebaudiana |
| CN107371672A (en) * | 2017-06-14 | 2017-11-24 | 湖南祥民制药有限公司 | A kind of method for improving STEVIA REBAUDIANA REB D yield |
| CN108033986A (en) * | 2018-02-07 | 2018-05-15 | 内蒙古昶辉生物科技股份有限公司 | The preparation method of Steviosin |
| CN108676042A (en) * | 2018-07-09 | 2018-10-19 | 山东端信堂大禹药业有限公司 | A kind of device and its extracting method extracting stevioside from STEVIA REBAUDIANA |
| CN109293712A (en) * | 2018-09-30 | 2019-02-01 | 晨光生物科技集团股份有限公司 | The industrialized utilization method and its steviol glycoside and chlorogenic acid of a kind of STEVIA REBAUDIANA |
| CN109432153A (en) * | 2018-10-25 | 2019-03-08 | 东台市浩瑞生物科技有限公司 | A method of stevia rebaudianum polyphenol is prepared with recombination chitosan flocculence |
| 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 |
| CN110959863A (en) * | 2019-12-13 | 2020-04-07 | 徐明德 | Stevia rebaudiana leaf mixed nutrient syrup and preparation method and application thereof |
| CN111349127A (en) * | 2020-03-28 | 2020-06-30 | 蚌埠市华东生物科技有限公司 | Method for producing stevioside |
| CN113440548A (en) * | 2021-08-16 | 2021-09-28 | 桂林莱茵生物科技股份有限公司 | Method for obtaining total chlorogenic acid and stevioside from stevia rebaudiana |
| CN114403319A (en) * | 2022-02-18 | 2022-04-29 | 北京鲜汽十族食品科技有限公司 | Preparation method of sugar-free bubble water |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105418703A (en) * | 2015-12-12 | 2016-03-23 | 常州大学 | Method for extracting and purifying stevioside from stevia rebaudiana |
-
2016
- 2016-06-17 CN CN201610446983.0A patent/CN106046075A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105418703A (en) * | 2015-12-12 | 2016-03-23 | 常州大学 | Method for extracting and purifying stevioside from stevia rebaudiana |
Non-Patent Citations (6)
| Title |
|---|
| 伏军芳: "甜菊糖苷的提取纯化工艺研究", 《西北师范大学硕士学位论文》 * |
| 何海芬，等: "甜菊糖苷的柱色谱法纯化", 《食品与发酵工业》 * |
| 刘东强，等: "甜菊糖苷的超声波提取及纯化工艺研究", 《中国调味品》 * |
| 吕鑫华: "甜菊糖苷类甜味剂的分离纯化与生物转化", 《北京化工大学硕士研究生学位论文》 * |
| 常颖，等: "《净水工艺》", 31 October 2014, 华南理工大学出版 * |
| 张雪颖，等: "酶法浸提甜菊糖甙的研究", 《食品工业科技》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674307A (en) * | 2016-11-03 | 2017-05-17 | 明光市大全甜叶菊专业合作社 | Method for extracting stevioside from stevia rebaudiana |
| CN106632539A (en) * | 2016-11-03 | 2017-05-10 | 明光市大全甜叶菊专业合作社 | A stevia rebaudiana glucoside extracting method |
| CN107371672A (en) * | 2017-06-14 | 2017-11-24 | 湖南祥民制药有限公司 | A kind of method for improving STEVIA REBAUDIANA REB D yield |
| CN108033986A (en) * | 2018-02-07 | 2018-05-15 | 内蒙古昶辉生物科技股份有限公司 | The preparation method of Steviosin |
| CN108676042B (en) * | 2018-07-09 | 2023-09-05 | 济宁市瑞信堂大禹药业有限公司 | Device for extracting stevioside from stevia rebaudiana and extraction method thereof |
| CN108676042A (en) * | 2018-07-09 | 2018-10-19 | 山东端信堂大禹药业有限公司 | A kind of device and its extracting method extracting stevioside from STEVIA REBAUDIANA |
| CN109293712A (en) * | 2018-09-30 | 2019-02-01 | 晨光生物科技集团股份有限公司 | The industrialized utilization method and its steviol glycoside and chlorogenic acid of a kind of STEVIA REBAUDIANA |
| CN109432153A (en) * | 2018-10-25 | 2019-03-08 | 东台市浩瑞生物科技有限公司 | A method of stevia rebaudianum polyphenol is prepared with recombination chitosan flocculence |
| CN109432153B (en) * | 2018-10-25 | 2021-07-27 | 东台市浩瑞生物科技有限公司 | Method for preparing stevia rebaudiana polyphenol by using composite chitosan flocculation method |
| 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 |
| CN110959863A (en) * | 2019-12-13 | 2020-04-07 | 徐明德 | Stevia rebaudiana leaf mixed nutrient syrup and preparation method and application thereof |
| CN111349127A (en) * | 2020-03-28 | 2020-06-30 | 蚌埠市华东生物科技有限公司 | Method for producing stevioside |
| CN113440548A (en) * | 2021-08-16 | 2021-09-28 | 桂林莱茵生物科技股份有限公司 | Method for obtaining total chlorogenic acid and stevioside from stevia rebaudiana |
| CN114403319A (en) * | 2022-02-18 | 2022-04-29 | 北京鲜汽十族食品科技有限公司 | Preparation method of sugar-free bubble water |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106046075A (en) | Method for extracting stevioside from stevia rebaudiana leaves | |
| CN106146574B (en) | A kind of method that microwave-ULTRASONIC COMPLEX extracts steviol glycoside in stevioside leaf | |
| CN107397103A (en) | A kind of preparation method of Momordica grosvenori decolouring flavor inspissated juice | |
| CN101690573B (en) | Production method of fructus monordicae extract with over 60% of mogroside V content | |
| CN102924544B (en) | Method for preparing stevioside and chlorogenic acid from stevia step by step | |
| CN105294790A (en) | Method for extracting high-purity steviol glycosides from stevia rebaudiana | |
| CN110684128B (en) | Method for extracting and refining polygonatum sibiricum polysaccharide | |
| CN102977163B (en) | Industrialized preparation method of stevioside | |
| CN106083940A (en) | A kind of method extracting high purity novel aurantiamarin from Fructus Aurantii Immaturus | |
| CN105053952B (en) | A kind of processing technology of the dried orange peel extracts of no bitter taste | |
| CN104262425B (en) | A kind of method for extracting Rubusoside | |
| CN103965096B (en) | A kind of preparation method being applicable to industrial 1-DNJ | |
| CN104592416A (en) | High-quality natural pectin extraction technology | |
| CN111153474A (en) | Stevioside extraction flocculant and extraction process thereof | |
| CN109369733B (en) | Method for simultaneously extracting multiple flavonoid compounds from tartary buckwheat leaves | |
| CN103739720B (en) | A kind of method producing pueraria starch from the root of kudzu vine | |
| CN116459286B (en) | Method for extracting moringa flavone from moringa leaves | |
| EP3505525B1 (en) | Method for preparing rubusoside | |
| WO2022247097A1 (en) | Method for separating active ingredients from siraitia grosvenorii flowers | |
| CN101455291A (en) | Fructose and oligo-fructose production method using garlic fructosan hydrolase | |
| CN106831906A (en) | A kind of ultrasonic wave added method extraction of steviosides from STEVIA REBAUDIANA | |
| AU2010318820B2 (en) | Method for producing white sugar, light brown sugar and dark brown sugar using direct recovery process | |
| CN103408614A (en) | Novel preparation technique of steviosin and Rebaudioside-A | |
| CN109336997B (en) | Method for extracting inulin from jerusalem artichoke at low temperature | |
| CN110664705A (en) | Preparation method of sweet potato anthocyanin eye shadow |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20161026 |
|
| WW01 | Invention patent application withdrawn after publication |