CN106749726B - A method of extracting Arillus longan polysaccharide - Google Patents
A method of extracting Arillus longan polysaccharide Download PDFInfo
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- CN106749726B CN106749726B CN201611148241.6A CN201611148241A CN106749726B CN 106749726 B CN106749726 B CN 106749726B CN 201611148241 A CN201611148241 A CN 201611148241A CN 106749726 B CN106749726 B CN 106749726B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
Abstract
The invention discloses a kind of methods for extracting Arillus longan polysaccharide, the following steps are included: (1) slurrying and activation processing: fresh arillus longan and pure water being mixed, slurrying in homogenizer is poured into, lye is then added, 10-12h is activated at negative 4-10 DEG C, obtains activating solution；(2) enzymatic hydrolysis and concentration: the pH value of activating solution is adjusted, then copper oxide-zirconium oxide catalyst and tri compound enzyme are added in filtrate, it is digested under conditions of 200-500W microwave radiation, then the enzymolysis liquid obtained after enzymatic hydrolysis is concentrated by ultrafiltration, obtains concentrate；(3) centrifugal treating: concentrate and mixing alcoholic solution are mixed, and collect precipitate with centrifuge；(4) spray drying treatment.The extraction preparation process of lye low-temperature activation enzyme association technology transfer longan polysaccharide, the yield of target product are significantly improved by the present invention than routine techniques, have the characteristics that efficient, quick, low cost, are suitable for large-scale industrial production.
Description
[technical field]
The present invention relates to the field of deep of longan, in particular to a kind of method for extracting Arillus longan polysaccharide.
[background technique]
Longan is the fruit also known as longan of Sapindaceae, is the famous subtropical fruit in China.Longan originates in China south
The south subtropics region in portion and North Vietnam has more than 2000 years cultivation histories in China, is important the evergreen length of south subtropics
Longevity fruit tree, the in history title in south " longan " north " ginseng ".The situation of selling well of longan fruit is enjoyed at home and abroad higher in the international market
Reputation, China's Longan Cultivation area and yield occupy first place in the world, and the provinces such as China Fujian Guangdong, Guangxi and Taiwan are main producing regions, sea
Also there are cultivation in the provinces such as southern Yunnan Sichuan and Guizhou.
Arillus longan polysaccharide is generally tan amorphous solid, and easy to absorb moisture obtains white powder after isolating and purifying,
Insoluble in organic solvents such as ethyl alcohol, acetone, n-butanols, it is more difficult to be dissolved in cold water, mainly by rhamnose, glucose, galactolipin,
The Type B pyrans acid heteroglycan of the tool acetylamino structure of the compositions such as xylose, pectinose is constituted.Currently, both at home and abroad for dragon
The research of eye meat polysaccharide extracting process mostly uses conventional hot water's extraction, and polysaccharide material is difficult to release into the cell from longan pulp
Come, causes yield lower；In addition, Hot water extraction requires extraction time long, Extracting temperature is high, easily causes polysaccharide hydrolysis, reduces
Polysaccharide material bioactivity.Enzymatic isolation method is one of the method for the effective component extracting out of plant to greatest extent, and enzyme digestion reaction was both
More leniently plant tissue can be decomposed, improve yield by a relatively large margin；It is also less prone to destroy the stereochemical structure and life of polysaccharide simultaneously
Object activity, has been increasingly becoming the hot spot of active components of plants Study on extraction in recent years.The extractive technique of existing longan polysaccharide
It takes a long time, separates at high cost, the low efficiency of preparation.Therefore, recovery rate, the product yield of longan polysaccharide how to be improved
The bottleneck problem of longan polysaccharide industrialization urgent need to resolve is had become with product purity.
Plant fiber pre-processes in low temperature lye, interaction of hydrogen bond can occur by lye and cellulose, destroy
The crystal structure of cellulose, to increase the dissolubility of cellulose in water.Wuhan University Zhang Lina establishes the low of cellulose
Warm dissolving technology (publication number CN200710052532.X, CN200710051867.X), this method is with lithium hydroxide or Strong oxdiative
Sodium, urea, water are raw material, realize molecular weight under cryogenic lower than 30 × 104Native cellulose or II fiber type element
Dissolution, which is physical process, is not chemically reacted, and waste liquid is easy recycling, is had wider
Application prospect.
[summary of the invention]
It is an object of that present invention to provide a kind of method for extracting Arillus longan polysaccharide, which assists skill for lye low-temperature activation enzyme
Art introduces the extraction preparation process of longan polysaccharide, and the yield of target product is significantly improved than routine techniques, has efficiently, fastly
The feature of speed, low cost, is suitable for large-scale industrial production.
In order to achieve the above objectives, the technical scheme adopted by the invention is that: a method of extract Arillus longan polysaccharide, including
Following steps:
(1) slurrying and activation processing: fresh arillus longan and pure water are mixed, and pour into slurrying in homogenizer, then plus
Enter lye, activates 10-12h at negative 4-10 DEG C, obtain activating solution；
(2) enzymatic hydrolysis and concentration: adjusting the pH value of activating solution, and copper oxide-zirconium oxide catalysis is then added in filtrate
Agent and tri compound enzyme are digested under conditions of 200-500W microwave radiation, when the reaction temperature and reaction of controlled enzymatic hydrolysis
Between, then the enzymolysis liquid obtained after enzymatic hydrolysis is concentrated by ultrafiltration, obtains concentrate；
(3) centrifugal treating: concentrate and mixing alcoholic solution are mixed, after being ultrasonically treated 25-40min, received with centrifuge
Collect precipitate；
(4) spray drying treatment: precipitate is washed with 85-95 DEG C of deionized water, and rotation throwing disc is put into after cooling and is turned
Speed is dry 10-30s in the rotation type atomization drier of 15000-25000r/min, obtains Arillus longan polysaccharide.
In the present invention, as further explanation, copper oxide-zirconium oxide catalyst described in step (2) is by following methods
Preparation: according to parts by weight, 35-50 parts of anhydrous cupric sulfates, 30-45 parts of zirconium oxychlorides are added to 200-300 parts of deionized waters
In, the sodium hydroxide solution that mass fraction is 40-50% is added dropwise while stirring, adjusting pH value is 9-12, and filtering takes filter residue, is used
Deionized water is washed 2-4 times, is dried, microwave drying 10-20min, finally in Muffle furnace with 1100-1300 DEG C of roasting 2-4h,
Obtain copper oxide-zirconium oxide catalyst.
In the present invention, as further explanation, lye described in step (1) is the hydrogen by weight 1:1-3:10-15
Potassium oxide, the ammonium hydroxide that mass fraction is 25% and deionized water mix.
In the present invention, as further explanation, tri compound enzyme described in step (2) is by weight 50-70:20-
Acidic cellulase, fructosidase and the protease of 35:15-30 mixes.
In the present invention, as further explanation, pH value described in step (2) is 4.5-5.5, and the reaction temperature is
50-75 DEG C, the reaction time is 40-60min.
In the present invention, as further explanation, ultrafiltration concentration described in step (2) is to retain 5-50KD using ultrafiltration membrane
The enzymolysis liquid of molecular weight is 40-60 DEG C in temperature, and vacuum distillation to solid content is under conditions of pressure is -0.09MPa
80-95%.
In the present invention, as further explanation, mixing alcoholic solution described in step (3) is by weight 10-16:1:1-
The normal propyl alcohol aqueous solution and mass fraction that ethanol water that 2 mass fraction is 95%, mass fraction are 70-80% are 70-
90% isopropanol water solution mixes.
In the present invention, as further explanation, the fresh arillus longan, pure water, lye, copper oxide-zirconium oxide
The weight ratio of catalyst, tri compound enzyme and mixing alcoholic solution is 100:250-500:20-40:1-3:5-8:500-700.Part
The function introduction of raw material is as follows:
Starch branch polyacrylamide flocculant is the copolymer of starch grafted polyacrylamide, is divided into gel-type and line style
Two kinds of grafted chain, be a kind of novel high polymer coagulant, it combines the characteristic of starch and polyacrylamide, has good
Flocculating property.
Acidic cellulase is to be extracted to be made by liquid submerged fermentation purification by koning trichoderma bacterium.Product is widely applied
In industries such as weaving, feed, alcohol, alcohol fuel, brewing, traditional Chinese medicine extractions.
Fructosidase, a kind of ectoenzyme, the levulan molecule that specifically catalyzing hydrolysis is made of β-D-Fructose can also water
Solve synanthrin, sucrose, gossypose etc..
Protease is the general name of the class of enzymes of aminosal peptide chain.It is divided into endopeptidase and end in such a way that it degrades polypeptide
Two class of peptase.The former can cut off the polypeptide chain of macromolecule from centre, form the lesser protein of molecular weight and peptone；The latter can divide again
For carboxypeptidase and aminopeptidase, peptide chain is hydrolyzed from the free carboxy termini of polypeptide or free amine end one by one generate respectively by they
Amino acid.
Ethyl alcohol is commonly called as alcohol, it is a kind of inflammable, volatile colourless transparent liquid under room temperature, normal pressure, it water-soluble
Liquid has special, pleasant fragrance, and slightly irritation.Ethyl alcohol has many uses, and acetic acid, drink can be manufactured with ethyl alcohol
Material, essence, dyestuff, fuel etc..It medically also commonly uses the ethyl alcohol that volume fraction is 70%-75% and makees disinfectant etc..
Normal propyl alcohol, colourless transparent liquid, 97.15 DEG C of boiling point.It is dissolved in water, it is inflammable.It is mainly used as in solvent and organic synthesis
Mesosome.In the U.S., normal propyl alcohol about 40% is directly used as solvent or synthesis propyl acetate, for paint solvent, printing ink, makeup
Product etc..40% for producing the intermediate n-propylamine of medicine, pesticide.20% for producing feed addictive, synthetic perfume etc..
Isopropanol, colourless transparent liquid are dissolved in the organic solvents such as water, alcohol, ether, benzene, be important chemical products and raw material,
It is mainly used for being used as dehydrating agent and cleaning agent in pharmacy, cosmetics, plastics, fragrance and coating and electronics industry.
The invention has the following advantages:
1. the present invention uses lye low-temperature activation technology, it can be interacted by lye and cellulose, destroy cellulose
Crystal structure can effectively improve the dissolution rate of Arillus longan polysaccharide to increase the dissolubility of cellulose in water.Institute of the present invention
Ammonium hydroxide in the lye of use can effectively break the unstable chemical bond in arillus longan between cellulose, and ammonium hydroxide acts on fibre
Dimension element causes the phase transformation of its swelling and crystalline solid, and ammonium hydroxideization can significantly increase the porosity of biomass, increases cellulose to enzyme
Absorption, increase cellulose and enzyme accessible area, to improve enzymolysis speed；Potassium hydroxide can dissolve pulp,
Make pulp short texture, moreover it is possible to break the hydrogen bond between cellulose, reduce the crystallinity of cellulose, increase cellulose can
And property is to improve enzymatic hydrolyzation；On the other hand, under the conditions of cryogenic freezing, become larger into the molecular structure water inside pulp, directly
It connects and is strutted from inside by pulp organization, make the structure of pulp by closely becoming loose, to increase in pulp
The accessible area of cellulose and enzyme improves enzymolysis efficiency, further increases the yield of Arillus longan polysaccharide；This three's phase interworking
It closes, interaction is indispensable, improves enzymolysis efficiency from different perspectives, and the yield of the pulp polysaccharide of acquirement is much higher than single item
The yield of Arillus longan polysaccharide caused by part.
2. invention applies the precipitation method to prepare copper oxide-zirconium oxide catalyst, the technology in alkaline solution by sinking
Shallow lake copper oxide-zirconium oxide catalyst, by microwave treatment, can make the internal structure of copper oxide-zirconium oxide catalyst in it is loose,
Cellular finally fixes the shape of copper oxide-zirconium oxide catalyst by 1100-1300 DEG C of high-temperature roasting again, because
At 1100 DEG C, the crystal form of zirconium oxide is transformed into tetragonal structure from monoclinic form, and the zirconium oxide of tetragonal structure can more excite enzyme
Activity, promotion enzymatic hydrolysis, therefore its effect generated, which are much higher than used by the prior art, fixes zirconium oxide at a temperature of 400-600 DEG C
Effect, and the copper oxide-zirconium oxide catalyst prepared by the precipitation method can effectively increase and tri compound enzyme
Contact area further increases enzymolysis efficiency.
3. the ultrafiltration concentration process that the present invention uses applies Ultra filtration membrane technology, selective retention molecular weight is 5-50KD
Enzymolysis liquid eliminated in the cellulose, xylan, extract not digested while effectively catching Arillus longan polysaccharide
Small molecular weight impurity and production in the complex enzyme that additionally adds, significantly improve the purity of Arillus longan polysaccharide.
[specific embodiment]
Embodiment 1:
1. early-stage preparations:
The preparation of copper oxide-zirconium oxide catalyst: 35g anhydrous cupric sulfate, 30g zirconium oxychloride are added to 200g deionization
In water, while stirring be added dropwise mass fraction be 40% sodium hydroxide solution, adjust pH value be 9, filtering, take filter residue, spend from
Sub- water washing 2 times, dries, microwave drying 10min, finally obtains copper oxide-zirconium oxide in Muffle furnace with 1100 DEG C of roasting 2h
Catalyst.
The preparation of lye: 10g potassium hydroxide, the ammonium hydroxide that 10g mass fraction is 25% and 100g deionized water are mixed, stirred
It mixes and uniformly obtains lye.
The preparation of tri compound enzyme: 50g acidic cellulase, 20g fructosidase and 15g protease are uniformly mixed, obtained
To tri compound enzyme.
Mix alcoholic solution preparation: by 1000g mass fraction be 95% ethanol water, 100g mass fraction be 70%
Normal propyl alcohol aqueous solution and 100g mass fraction be 70% isopropanol water solution mix, stir evenly, obtain mixing alcoholic solution.
The substance that above-mentioned early period is prepared is used for following methods for extracting Arillus longan polysaccharide.
2. a kind of method for extracting Arillus longan polysaccharide, comprising the following steps:
(1) slurrying and activation processing: the fresh arillus longan of 100g and 250g pure water are mixed, pours into homogenizer and makes
Then slurry is added 20g lye, activates 10h at minus 4 DEG C, obtain activating solution；
(2) enzymatic hydrolysis and concentration: the pH value for adjusting activating solution is 4.5, and 1g copper oxide-oxidation is then added in filtrate
Zr catalyst and 5g tri compound enzyme, are digested under conditions of 200W microwave radiation, and the reaction temperature of controlled enzymatic hydrolysis is 50
DEG C and the reaction time be 40min, then the enzymolysis liquid obtained after enzymatic hydrolysis is concentrated by ultrafiltration, with ultrafiltration membrane retention 5-50KD point
The enzymolysis liquid of son amount is 40 DEG C in temperature, and vacuum distillation is 80% to solid content under conditions of pressure is -0.09MPa, is obtained
To concentrate；
(3) centrifugal treating: concentrate and 500g mixing alcoholic solution are mixed, and after being ultrasonically treated 25min, are received with centrifuge
Collect precipitate；
(4) spray drying treatment: precipitate is washed with 85 DEG C of deionized water, and rotation throwing disc revolving speed is put into after cooling and is
Dry 10s, obtains Arillus longan polysaccharide in the rotation type atomization drier of 15000r/min.
Embodiment 2:
1. early-stage preparations:
The preparation of copper oxide-zirconium oxide catalyst: 38g anhydrous cupric sulfate, 35g zirconium oxychloride are added to 240g deionization
In water, while stirring be added dropwise mass fraction be 45% sodium hydroxide solution, adjust pH value be 10, filtering, take filter residue, spend from
Sub- water washing 3 times, dries, microwave drying 13min, finally obtains copper oxide-oxidation in Muffle furnace with 1200 DEG C of roasting 2.5h
Zr catalyst.
The preparation of lye: 10g potassium hydroxide, the ammonium hydroxide that 18g mass fraction is 25% and 120g deionized water are mixed, stirred
It mixes and uniformly obtains lye.
The preparation of tri compound enzyme: 65g acidic cellulase, 23g fructosidase and 20g protease are uniformly mixed, obtained
To tri compound enzyme.
Mix alcoholic solution preparation: by 1200g mass fraction be 95% ethanol water, 100g mass fraction be 75%
Normal propyl alcohol aqueous solution and 133g mass fraction be 78% isopropanol water solution mix, stir evenly, obtain mixing alcoholic solution.
The substance that above-mentioned early period is prepared is used for following methods for extracting Arillus longan polysaccharide.
2. a kind of method for extracting Arillus longan polysaccharide, comprising the following steps:
(1) slurrying and activation processing: the fresh arillus longan of 100g and 400g pure water are mixed, pours into homogenizer and makes
Then slurry is added 33g lye, activates 10.5h at minus 5 DEG C, obtain activating solution；
(2) enzymatic hydrolysis and concentration: the pH value for adjusting activating solution is 5, and 1.5g copper oxide-oxidation is then added in filtrate
Zr catalyst and 6g tri compound enzyme, are digested under conditions of 400W microwave radiation, and the reaction temperature of controlled enzymatic hydrolysis is 63
DEG C and the reaction time be 51min, then the enzymolysis liquid obtained after enzymatic hydrolysis is concentrated by ultrafiltration, with ultrafiltration membrane retention 5-50KD point
The enzymolysis liquid of son amount is 49 DEG C in temperature, and vacuum distillation is 87% to solid content under conditions of pressure is -0.09MPa, is obtained
To concentrate；
(3) centrifugal treating: concentrate and 650g mixing alcoholic solution are mixed, and after being ultrasonically treated 33min, are received with centrifuge
Collect precipitate；
(4) spray drying treatment: precipitate is washed with 90 DEG C of deionized water, and rotation throwing disc revolving speed is put into after cooling and is
Dry 19s, obtains Arillus longan polysaccharide in the rotation type atomization drier of 18000r/min.
Embodiment 3:
1. early-stage preparations:
The preparation of copper oxide-zirconium oxide catalyst: 43g anhydrous cupric sulfate, 37g zirconium oxychloride are added to 260g deionization
In water, while stirring be added dropwise mass fraction be 44% sodium hydroxide solution, adjust pH value be 11, filtering, take filter residue, spend from
Sub- water washing 3 times, dries, microwave drying 15min, finally obtains copper oxide-zirconium oxide in Muffle furnace with 1150 DEG C of roasting 3h
Catalyst.
The preparation of lye: 10g potassium hydroxide, the ammonium hydroxide that 24g mass fraction is 25% and 130g deionized water are mixed, stirred
It mixes and uniformly obtains lye.
The preparation of tri compound enzyme: 66g acidic cellulase, 30g fructosidase and 26g protease are uniformly mixed, obtained
To tri compound enzyme.
Mix alcoholic solution preparation: by 1450g mass fraction be 95% ethanol water, 100g mass fraction be 75%
Normal propyl alcohol aqueous solution and 170g mass fraction be 82% isopropanol water solution mix, stir evenly, obtain mixing alcoholic solution.
The substance that above-mentioned early period is prepared is used for following methods for extracting Arillus longan polysaccharide.
2. a kind of method for extracting Arillus longan polysaccharide, comprising the following steps:
(1) slurrying and activation processing: the fresh arillus longan of 100g and 360g pure water are mixed, pours into homogenizer and makes
Then slurry is added 26g lye, activates 11.5h at minus 6 DEG C, obtain activating solution；
(2) enzymatic hydrolysis and concentration: the pH value for adjusting activating solution is 5, and 1.5g copper oxide-oxidation is then added in filtrate
Zr catalyst and 7g tri compound enzyme, are digested under conditions of 390W microwave radiation, and the reaction temperature of controlled enzymatic hydrolysis is 60
DEG C and the reaction time be 54min, then the enzymolysis liquid obtained after enzymatic hydrolysis is concentrated by ultrafiltration, with ultrafiltration membrane retention 5-50KD point
The enzymolysis liquid of son amount is 49 DEG C in temperature, and vacuum distillation is 92% to solid content under conditions of pressure is -0.09MPa, is obtained
To concentrate；
(3) centrifugal treating: concentrate and 640g mixing alcoholic solution are mixed, and after being ultrasonically treated 36min, are received with centrifuge
Collect precipitate；
(4) spray drying treatment: precipitate is washed with 91 DEG C of deionized water, and rotation throwing disc revolving speed is put into after cooling and is
Dry 22s, obtains Arillus longan polysaccharide in the rotation type atomization drier of 20000r/min.
Embodiment 4:
1. early-stage preparations:
The preparation of copper oxide-zirconium oxide catalyst: 47g anhydrous cupric sulfate, 40g zirconium oxychloride are added to 255g deionization
In water, while stirring be added dropwise mass fraction be 43% sodium hydroxide solution, adjust pH value be 10, filtering, take filter residue, spend from
Sub- water washing 2 times, dries, microwave drying 13min, finally obtains copper oxide-oxidation in Muffle furnace with 1250 DEG C of roasting 3.5h
Zr catalyst.
The preparation of lye: 10g potassium hydroxide, the ammonium hydroxide that 25g mass fraction is 25% and 110g deionized water are mixed, stirred
It mixes and uniformly obtains lye.
The preparation of tri compound enzyme: 63g acidic cellulase, 24g fructosidase and 28g protease are uniformly mixed, obtained
To tri compound enzyme.
Mix alcoholic solution preparation: by 1500g mass fraction be 95% ethanol water, 100g mass fraction be 73%
Normal propyl alcohol aqueous solution and 140g mass fraction be 84% isopropanol water solution mix, stir evenly, obtain mixing alcoholic solution.
The substance that above-mentioned early period is prepared is used for following methods for extracting Arillus longan polysaccharide.
2. a kind of method for extracting Arillus longan polysaccharide, comprising the following steps:
(1) slurrying and activation processing: the fresh arillus longan of 100g and 360g pure water are mixed, pours into homogenizer and makes
Then slurry is added 24g lye, activates 10h at minus 7 DEG C, obtain activating solution；
(2) enzymatic hydrolysis and concentration: the pH value for adjusting activating solution is 4.5, and 2.5g copper oxide-oxygen is then added in filtrate
Change Zr catalyst and 6.5g tri compound enzyme, is digested under conditions of 300W microwave radiation, the reaction temperature of controlled enzymatic hydrolysis
Be 66 DEG C and reaction time it is 55min, then the enzymolysis liquid obtained after enzymatic hydrolysis is concentrated by ultrafiltration, retains 5- with ultrafiltration membrane
The enzymolysis liquid of 50KD molecular weight is 52 DEG C in temperature, and vacuum distillation to solid content is under conditions of pressure is -0.09MPa
87%, obtain concentrate；
(3) centrifugal treating: concentrate and 580g mixing alcoholic solution are mixed, and after being ultrasonically treated 32min, are received with centrifuge
Collect precipitate；
(4) spray drying treatment: precipitate is washed with 90 DEG C of deionized water, and rotation throwing disc revolving speed is put into after cooling and is
Dry 23s, obtains Arillus longan polysaccharide in the rotation type atomization drier of 19000r/min.
Embodiment 5:
1. early-stage preparations:
The preparation of copper oxide-zirconium oxide catalyst: 44g anhydrous cupric sulfate, 36g zirconium oxychloride are added to 250g deionization
In water, while stirring be added dropwise mass fraction be 47% sodium hydroxide solution, adjust pH value be 11, filtering, take filter residue, spend from
Sub- water washing 4 times, dries, microwave drying 19min, finally obtains copper oxide-oxidation in Muffle furnace with 1300 DEG C of roasting 3.5h
Zr catalyst.
The preparation of lye: 10g potassium hydroxide, the ammonium hydroxide that 25g mass fraction is 25% and 135g deionized water are mixed, stirred
It mixes and uniformly obtains lye.
The preparation of tri compound enzyme: 68g acidic cellulase, 30g fructosidase and 22g protease are uniformly mixed, obtained
To tri compound enzyme.
Mix alcoholic solution preparation: by 1550g mass fraction be 95% ethanol water, 100g mass fraction be 76%
Normal propyl alcohol aqueous solution and 176g mass fraction be 85% isopropanol water solution mix, stir evenly, obtain mixing alcoholic solution.
The substance that above-mentioned early period is prepared is used for following methods for extracting Arillus longan polysaccharide.
2. a kind of method for extracting Arillus longan polysaccharide, comprising the following steps:
(1) slurrying and activation processing: the fresh arillus longan of 100g and 368g pure water are mixed, pours into homogenizer and makes
Then slurry is added 32g lye, activates 10h at minus 9 DEG C, obtain activating solution；
(2) enzymatic hydrolysis and concentration: the pH value for adjusting activating solution is 5, and 2g copper oxide-zirconium oxide is then added in filtrate
Catalyst and 7g tri compound enzyme, are digested under conditions of 260W microwave radiation, and the reaction temperature of controlled enzymatic hydrolysis is 70 DEG C
It is 46min with the reaction time, then the enzymolysis liquid obtained after enzymatic hydrolysis is concentrated by ultrafiltration, retains 5-50KD molecule with ultrafiltration membrane
The enzymolysis liquid of amount is 48 DEG C in temperature, and vacuum distillation is 92% to solid content under conditions of pressure is -0.09MPa, is obtained
Concentrate；
(3) centrifugal treating: concentrate and 590g mixing alcoholic solution are mixed, and after being ultrasonically treated 30min, are received with centrifuge
Collect precipitate；
(4) spray drying treatment: precipitate is washed with 88 DEG C of deionized water, and rotation throwing disc revolving speed is put into after cooling and is
Dry 23s, obtains Arillus longan polysaccharide in the rotation type atomization drier of 22000r/min.
Embodiment 6:
1. early-stage preparations:
The preparation of copper oxide-zirconium oxide catalyst: 50g anhydrous cupric sulfate, 45g zirconium oxychloride are added to 300g deionization
In water, the sodium hydroxide solution that 25g mass fraction is 50% is added dropwise while stirring, adjusting pH value is 12, and filtering takes filter residue, is used
Deionized water is washed 4 times, is dried, microwave drying 20min, is finally obtained copper oxide-oxygen in Muffle furnace with 1250 DEG C of roasting 4h
Change Zr catalyst.
The preparation of lye: 10g potassium hydroxide, the ammonium hydroxide that 30g mass fraction is 25% and 150g deionized water are mixed, stirred
It mixes and uniformly obtains lye.
The preparation of tri compound enzyme: 70g acidic cellulase, 35g fructosidase and 30g protease are uniformly mixed, obtained
To tri compound enzyme.
Mix alcoholic solution preparation: by 1600g mass fraction be 95% ethanol water, 100g mass fraction be 80%
Normal propyl alcohol aqueous solution and 200g mass fraction be 90% isopropanol water solution mix, stir evenly, obtain mixing alcoholic solution.
The substance that above-mentioned early period is prepared is used for following methods for extracting Arillus longan polysaccharide.
2. a kind of method for extracting Arillus longan polysaccharide, comprising the following steps:
(1) slurrying and activation processing: the fresh arillus longan of 100g and 500g pure water are mixed, pours into homogenizer and makes
Then slurry is added 40g lye, activates 12h at minus 10 DEG C, obtain activating solution；
(2) enzymatic hydrolysis and concentration: the pH value for adjusting activating solution is 5.5, and 3g copper oxide-oxidation is then added in filtrate
Zr catalyst and 8g tri compound enzyme, are digested under conditions of 500W microwave radiation, and the reaction temperature of controlled enzymatic hydrolysis is 75
DEG C and the reaction time be 60min, then the enzymolysis liquid obtained after enzymatic hydrolysis is concentrated by ultrafiltration, with ultrafiltration membrane retention 5-50KD point
The enzymolysis liquid of son amount is 60 DEG C in temperature, and vacuum distillation is 95% to solid content under conditions of pressure is -0.09MPa, is obtained
To concentrate；
(3) centrifugal treating: concentrate and 700g mixing alcoholic solution are mixed, and after being ultrasonically treated 40min, are received with centrifuge
Collect precipitate；
(4) spray drying treatment: precipitate is washed with 95 DEG C of deionized water, and rotation throwing disc revolving speed is put into after cooling and is
Dry 30s, obtains Arillus longan polysaccharide in the rotation type atomization drier of 25000r/min.
Comparative example 1: the method for extracting Arillus longan polysaccharide is substantially the same manner as Example 1, and difference is: step does not have in (1)
Have using low temperature lye activating technology；
Comparative example 2: the method for extracting Arillus longan polysaccharide is substantially the same manner as Example 1, and difference is: step does not have in (2)
There is addition solid catalyst；
Comparative example 3: the method for extracting Arillus longan polysaccharide is substantially the same manner as Example 1, and difference is: step does not have in (2)
Have using ultrafiltration concentration technology, but Rotary Evaporators is used to be concentrated.
Comparative test 1:
The Arillus longan polysaccharide in 100 fresh arillus longans is respectively extracted by the technical method of comparative example 1-3 and embodiment 1-6, is examined
The purity of Arillus longan polysaccharide yield and Arillus longan polysaccharide is surveyed, testing result is shown in Table 1.
Table 1:
Table 1 the result shows that: the yield of Arillus longan polysaccharide is higher, illustrates that the production efficiency of the technical method is higher, longan
Meat polysaccharide yield arranges from high to low are as follows: 1 > embodiment of embodiment 4 > embodiment 3=embodiment 6 > embodiment, 2 > embodiment 5 > right
2 > comparative example of ratio, 3 > comparative example 1；
The purity of Arillus longan polysaccharide is higher, illustrates that the production efficiency of the technical method is higher, the purity of Arillus longan polysaccharide from
High to Low arrangement are as follows: 3 > comparative example of embodiment 4 > embodiment, 5 > embodiment, 2 > embodiment, 6 > embodiment, 3 > embodiment, 1 > comparative example 3 >
Comparative example 1.
Above description is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair
Bright patent claim, it is all the present invention suggested by technical spirit under completed same changes or modifications change, should all belong to
In the covered the scope of the patents of the present invention.
Claims (7)
1. a kind of method for extracting Arillus longan polysaccharide, it is characterised in that: the following steps are included:
(1) slurrying and activation processing: fresh arillus longan and pure water are mixed, and pour into slurrying in homogenizer, alkali is then added
Liquid activates 10-12h at negative 4-10 DEG C, obtains activating solution；
(2) enzymatic hydrolysis and concentration: adjust the pH value of activating solution, then in filtrate be added copper oxide-zirconium oxide catalyst and
Tri compound enzyme is digested under conditions of 200-500W microwave radiation, the reaction temperature of controlled enzymatic hydrolysis and reaction time, is connect
The enzymolysis liquid obtained after enzymatic hydrolysis is concentrated by ultrafiltration, obtain concentrate；
The copper oxide-zirconium oxide catalyst is prepared by the following method: according to parts by weight, by 35-50 parts of anhydrous cupric sulfates,
30-45 parts of zirconium oxychlorides are added in 200-300 parts of deionized waters, and the hydroxide that mass fraction is 40-50% is added dropwise while stirring
Sodium solution, adjusting pH value are 9-12, and filtering takes filter residue, is washed with deionized 2-4 times, dries, microwave drying 10-20min,
Copper oxide-zirconium oxide catalyst is finally obtained with 1100-1300 DEG C of roasting 2-4h in Muffle furnace；
(3) centrifugal treating: concentrate and mixing alcoholic solution are mixed, and after being ultrasonically treated 25-40min, are collected and are analysed with centrifuge
Object out；
(4) spray drying treatment: precipitate is washed with 85-95 DEG C of deionized water, and rotation throwing disc revolving speed is put into after cooling and is
Dry 10-30s, obtains Arillus longan polysaccharide in the rotation type atomization drier of 15000-25000r/min.
2. a kind of method for extracting Arillus longan polysaccharide according to claim 1, it is characterised in that: alkali described in step (1)
Liquid is that the ammonium hydroxide that potassium hydroxide, the mass fraction of 1:1-3:10-15 by weight is 25% and deionized water mix.
3. a kind of method for extracting Arillus longan polysaccharide according to claim 1, it is characterised in that: three described in step (2)
First complex enzyme is that acidic cellulase, fructosidase and the protease of 50-70:20-35:15-30 by weight mixes.
4. a kind of method for extracting Arillus longan polysaccharide according to claim 1, it is characterised in that: pH described in step (2)
Value is 4.5-5.5, and the reaction temperature is 50-75 DEG C, and the reaction time is 40-60min.
5. a kind of method for extracting Arillus longan polysaccharide according to claim 1, it is characterised in that: surpass described in step (2)
Filter concentration is the enzymolysis liquid that 5-50KD molecular weight is retained using ultrafiltration membrane, is 40-60 DEG C in temperature, pressure is the item of -0.09MPa
Vacuum distillation to solid content is 80-95% under part.
6. the method for a kind of extraction Arillus longan polysaccharide according to claim 1, it is characterised in that: described in step (3)
Mixing ethanol water, mass fraction that alcoholic solution is 95% for the mass fraction by weight 10-16:1:1-2 is 70-80%'s
The isopropanol water solution that normal propyl alcohol aqueous solution and mass fraction are 70-90% mixes.
7. a kind of method of extraction Arillus longan polysaccharide described in -6 any one according to claim 1, it is characterised in that: described
Fresh arillus longan, pure water, lye, copper oxide-zirconium oxide catalyst, tri compound enzyme and mix alcoholic solution weight ratio be
100:250-500:20-40:1-3:5-8:500-700.
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| CN108841560B (en) * | 2018-06-29 | 2021-10-26 | 广西壮族自治区农业科学院农产品加工研究所 | Fragrant high-fidelity passion fruit vinegar and brewing method thereof |
| CN116854835B (en) * | 2023-04-04 | 2024-02-02 | 华南农业大学 | High-immunocompetence acetylated longan water-soluble glucan, and preparation method and application thereof |
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