CN106749726A - A kind of method for extracting Arillus longan polysaccharide - Google Patents

A kind of method for extracting Arillus longan polysaccharide Download PDF

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Publication number
CN106749726A
CN106749726A CN201611148241.6A CN201611148241A CN106749726A CN 106749726 A CN106749726 A CN 106749726A CN 201611148241 A CN201611148241 A CN 201611148241A CN 106749726 A CN106749726 A CN 106749726A
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arillus longan
mixed
solution
longan polysaccharide
enzymolysis
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CN106749726B (en
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何雪梅
孙健
李丽
刘国明
李昌宝
郑凤锦
盛金凤
唐雅园
李杰民
零东宁
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Guangxi Zhuang Nationality Autonomous Region Academy of Agricultural Sciences
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Institute of Agro Products Processing Science and Technology of Guangxi Academy of Agricultural Sciences
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/006Heteroglycans, 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass

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Abstract

The invention discloses a kind of method for extracting Arillus longan polysaccharide, comprise the following steps:(1) slurrying and activation process:Fresh arillus longan and pure water are mixed, slurrying in homogenizer is poured into, alkali lye is subsequently adding, 10 12h are activated at minus 4 10 DEG C, obtain activating solution;(2) enzymolysis and concentration:The pH value of activating solution is adjusted, cupric oxide zirconia catalyst and tri compound enzyme are then added in filtrate, digested under conditions of 200 500W microwaves, then the enzymolysis liquid obtained after enzymolysis is concentrated by ultrafiltration, obtain concentrate;(3) centrifugal treating:Concentrate and mixed alcohol solution are mixed, centrifugal collection precipitate is used;(4) spray drying treatment.The present invention is assisted the extraction preparation process of technology transfer longan polysaccharide by alkali lye low-temperature activation enzyme, and the yield of target product is significantly improved than routine techniques, with it is efficient, quick, inexpensive the characteristics of, be suitable for large-scale industrial production.

Description

A kind of method for extracting Arillus longan polysaccharide
【Technical field】
The present invention relates to the field of deep of longan, more particularly to a kind of method for extracting Arillus longan polysaccharide.
【Background technology】
Longan is the fruit of Sapindaceae, also known as longan is the famous subtropical fruit of China.Longan originates in China south Portion and the south subtropicses region of North Vietnam, are the evergreen length of important south subtropicses in existing more than the 2000 years cultivation history of China Longevity fruit tree, the in history title of 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 it is main producing region that China's Fujian Guangdong, Guangxi and Taiwan etc. are saved, sea Southern Yunnan Sichuan and Guizhou etc. save also cultivation.
Arillus longan polysaccharide is generally tan amorphous solid, easily the moisture absorption, and white powder is obtained after isolating and purifying, Insoluble in organic solvents such as ethanol, acetone, n-butanols, it is more difficult to be dissolved in cold water, its be 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.At present, both at home and abroad for dragon Using conventional hot water's extraction, polysaccharide material to be difficult to be discharged from longan pulp is intracellular the research of eye meat polysaccharide extracting process more Come, cause yield relatively low;Additionally, Hot water extraction requirement extraction time is long, Extracting temperature is high, easily causes polysaccharide hydrolysis, reduces Polysaccharide material bioactivity.Enzymatic isolation method is one of method of effective component extracting from plant to greatest extent, and enzyme digestion reaction was both More leniently plant tissue can be decomposed, yield is improved by a relatively large margin;It is also less prone to destroy stereochemical structure and the life of polysaccharide simultaneously Thing activity, has been increasingly becoming the focus of active components of plants Study on extraction in recent years.The extractive technique of existing longan polysaccharide Longer time is needed, high cost, the efficiency for separating preparation are low.Therefore, recovery rate, the product yield of longan polysaccharide how to be improved With the bottleneck problem that product purity has turned into longan polysaccharide industrialization urgent need to resolve.
String is pre-processed in low temperature alkali lye, interaction of hydrogen bond, destruction can occur by alkali lye and cellulose The crystal structure of cellulose, so as to increase dissolubility of the cellulose in water.Wuhan University Zhang Lina establishes the low of cellulose Warm dissolving technology (publication number CN200710052532.X, CN200710051867.X), the method is with lithium hydroxide or Strong oxdiative Sodium, urea, water are raw material, and molecular weight is realized under cryogenic less than 30 × 104Native cellulose or II fiber types element Dissolving, the course of dissolution is physical process, is chemically reacted, the easy recycling use of waste liquid, with wider Application prospect.
【The content of the invention】
Present invention aim at a kind of method for extracting Arillus longan polysaccharide is provided, alkali lye low-temperature activation enzyme is assisted skill by the technology Art introduces the extraction preparation process of longan polysaccharide, and the yield of target product is significantly improved than routine techniques, with efficient, fast The characteristics of speed, low cost, it is suitable for large-scale industrial production.
To reach above-mentioned purpose, the technical solution adopted in the present invention is:A kind of method for extracting Arillus longan polysaccharide, including Following steps:
(1) slurrying and activation process:Fresh arillus longan and pure water are mixed, slurrying in homogenizer, Ran Houjia is poured into Enter alkali lye, 10-12h is activated at negative 4-10 DEG C, obtain activating solution;
(2) enzymolysis and concentration:The pH value of activating solution is adjusted, copper oxide-zirconium oxide catalysis is then added in filtrate Agent and tri compound enzyme, are digested under conditions of 200-500W microwaves, when the reaction temperature of controlled enzymatic hydrolysis and reaction Between, then the enzymolysis liquid obtained after enzymolysis is concentrated by ultrafiltration, obtain concentrate;
(3) centrifugal treating:Concentrate and mixed alcohol solution are mixed, after ultrasonically treated 25-40min, is received with centrifuge Collection precipitate;
(4) spray drying treatment:Precipitate is washed with 85-95 DEG C of deionized water, rotation throwing disc is put into after cooling and is turned Speed obtains Arillus longan polysaccharide to dry 10-30s in the rotation type atomization drier of 15000-25000r/min.
In the present invention, as further illustrating, the copper oxide-zirconium oxide catalyst described in step (2) is by following methods Prepare:Count by weight, 35-50 parts of anhydrous cupric sulfate, 30-45 parts of zirconium oxychloride are added to 200-300 parts of deionized water In, it is the sodium hydroxide solution of 40-50% that mass fraction is added dropwise while stirring, and regulation pH value is 9-12, and filtering takes filter residue, uses Deionized water is washed 2-4 times, is dried, microwave drying 10-20min, finally with 1100-1300 DEG C of roasting 2-4h in Muffle furnace, Obtain copper oxide-zirconium oxide catalyst.
In the present invention, as further illustrating, the alkali lye described in step (1) is by weight 1:1-3:The hydrogen of 10-15 Potassium oxide, mass fraction are that 25% ammoniacal liquor and deionized water are mixed.
In the present invention, as further illustrating, the tri compound enzyme described in step (2) is by weight 50-70:20- 35:The acidic cellulase of 15-30, fructosidase and protease are mixed.
In the present invention, as further illustrating, the pH value described in step (2) is 4.5-5.5, and described reaction temperature is 50-75 DEG C, the described reaction time is 40-60min.
In the present invention, as further illustrating, the ultrafiltration concentration described in step (2) is to retain 5-50KD using milipore filter The enzymolysis liquid of molecular weight, temperature be 40-60 DEG C, pressure be -0.09MPa under conditions of vacuum distillation to solid content be 80-95%.
In the present invention, as further illustrating, the mixing alcoholic solution described in step (3) is by weight 10-16:1:1- 2 mass fraction be 95% ethanol water, mass fraction for 70-80% the normal propyl alcohol aqueous solution and mass fraction be 70- 90% isopropanol water solution is mixed.
In the present invention, as further illustrating, described fresh arillus longan, pure water, alkali 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, is a kind of new high polymer coagulant, and it combines the characteristic of starch and polyacrylamide, with good Flocculating property.
Acidic cellulase, is obtained by refined extraction of liquid submerged fermentation by koning trichoderma bacterium.Product extensive use 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 are made up of β-D-Fructose can also water Solution 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 the way of it degrades polypeptide The class of peptase two.The former can cut off the polypeptide chain of macromolecule from centre, form the less protein of molecular weight and peptone;The latter can divide again It is carboxypeptidase and aminopeptidase, peptide chain is hydrolyzed generate respectively by they one by one from the free carboxy termini or free amine end of polypeptide Amino acid.
Ethanol, is commonly called as alcohol, and it is a kind of inflammable, volatile colourless transparent liquid under normal temperature, normal pressure, it water-soluble Liquid has special, pleasant fragrance, and slightly excitant.Having many uses for ethanol, can manufacture acetic acid, drink with ethanol Material, essence, dyestuff, fuel etc..Volume fraction is medically also commonly used for the ethanol of 70%-75% makees disinfectant etc..
Normal propyl alcohol, colourless transparent liquid, 97.15 DEG C of boiling point.Water is dissolved in, 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, cosmetic Product etc..40% is used to produce medicine, the intermediate n-propylamine of agricultural chemicals.20% is used to produce feed addictive, synthetic perfume etc..
Isopropanol, colourless transparent liquid is dissolved in the organic solvents such as water, alcohol, ether, benzene, is important chemical products and raw material, It is mainly used in being used as dehydrating agent and cleaning agent in pharmacy, cosmetics, plastics, spices and coating and electronics industry.
The invention has the advantages that:
1. the present invention uses alkali lye low-temperature activation technology, can be interacted by alkali lye and cellulose, destroys cellulose Crystal structure, so as to increase dissolubility of the cellulose in water, the dissolution rate of Arillus longan polysaccharide can be effectively improved.Institute of the present invention Ammoniacal liquor in the alkali lye of use can effectively break the unstable chemical bond between cellulose in arillus longan, and ammoniacal liquor acts on fibre Dimension element causes its swelling and crystalline solid phase transformation, and ammoniacal liquorization can significantly increase the porosity of biomass, increases cellulose to enzyme Absorption, increase the accessible area of cellulose and enzyme, so as 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 so as to improve enzymatic hydrolyzation;On the other hand, under the conditions of cryogenic freezing, become big into the molecular structure water inside pulp, directly Connect from inside and strut pulp organization, make the structure of pulp by closely becoming loose, so as in increased pulp The accessible area of cellulose and enzyme, improves enzymolysis efficiency, further improves the yield of Arillus longan polysaccharide;This three's phase interworking Close, interact, it is indispensable, enzymolysis efficiency is improved from different perspectives, the yield of the pulp polysaccharide of acquirement is far above single bar The yield of the Arillus longan polysaccharide produced by part.
2. copper oxide-zirconium oxide catalyst is prepared invention applies the precipitation method, the technology is sunk by alkaline solution 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 cupric oxide-zirconia catalyst by 1100-1300 DEG C of high-temperature roasting again, because At 1100 DEG C, the crystal formation of zirconium oxide is transformed into tetragonal structure from monoclinic form, and the zirconium oxide of tetragonal structure can more excite enzyme Zirconium oxide is fixed at a temperature of activity, promotes to digest, therefore its effect for producing is far above 400-600 DEG C that prior art is used Effect, and the copper oxide-zirconium oxide catalyst prepared by the precipitation method can be effectively increased and tri compound enzyme Contact area, further improves enzymolysis efficiency.
3. the ultrafiltration concentration process that the present invention is used applies Ultra filtration membrane technology, and selective retention molecular weight is 5-50KD Enzymolysis liquid, while effectively catching Arillus longan polysaccharide, in eliminating cellulose, xylan, the extract for digesting Small molecular weight impurity and production in extra addition complex enzyme, 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 sulfates, 30g zirconium oxychlorides are added to 200g deionizations In water, while stirring be added dropwise mass fraction be 40% sodium hydroxide solution, regulation 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 with 1100 DEG C of roasting 2h in Muffle furnace Catalyst.
The preparation of alkali lye:10g potassium hydroxide, the ammoniacal liquor that 10g mass fractions are 25% and 100g deionized waters are mixed, is stirred Mix and uniformly obtain alkali lye.
The preparation of tri compound enzyme:50g acidic cellulases, 20g fructosidases and 15g protease are well mixed, are obtained To tri compound enzyme.
Mix the preparation of alcoholic solution:It is 70% by ethanol water that 1000g mass fractions are 95%, 100g mass fractions The normal propyl alcohol aqueous solution and the mixing of isopropanol water solution that 100g mass fractions are 70%, stir, obtain mixing alcoholic solution.
The method that the material that above-mentioned early stage is prepared is used for following extraction Arillus longan polysaccharides.
2. a kind of method for extracting Arillus longan polysaccharide, comprises the following steps:
(1) slurrying and activation process:The fresh arillus longans of 100g and 250g pure water are mixed, is poured into homogenizer and is made Slurry, is subsequently adding 20g alkali lye, and 10h is activated at minus 4 DEG C, obtains activating solution;
(2) enzymolysis and concentration:The pH value for adjusting activating solution is 4.5, and 1g cupric oxide-oxidation is then added in filtrate Zr catalyst and 5g tri compound enzymes, are digested under conditions of 200W microwaves, and the reaction temperature of controlled enzymatic hydrolysis is 50 DEG C and the reaction time be 40min, then the enzymolysis liquid obtained after enzymolysis is concentrated by ultrafiltration, retain 5-50KD point with milipore filter Son amount enzymolysis liquid, temperature be 40 DEG C, pressure be -0.09MPa under conditions of vacuum distillation to solid content be 80%, obtain To concentrate;
(3) centrifugal treating:Concentrate and 500g mixed alcohol solution are mixed, after ultrasonically treated 25min, is received with centrifuge Collection precipitate;
(4) spray drying treatment:Precipitate is washed with 85 DEG C of deionized water, rotation throwing disc rotating speed is put into after cooling is 10s is dried in the rotation type atomization drier of 15000r/min, Arillus longan polysaccharide is obtained.
Embodiment 2:
1. early-stage preparations:
The preparation of copper oxide-zirconium oxide catalyst:38g anhydrous cupric sulfates, 35g zirconium oxychlorides are added to 240g deionizations In water, while stirring be added dropwise mass fraction be 45% sodium hydroxide solution, regulation pH value be 10, filtering, take filter residue, spend from Sub- water washing 3 times, dries, microwave drying 13min, finally obtains cupric oxide-oxidation with 1200 DEG C of roasting 2.5h in Muffle furnace Zr catalyst.
The preparation of alkali lye:10g potassium hydroxide, the ammoniacal liquor that 18g mass fractions are 25% and 120g deionized waters are mixed, is stirred Mix and uniformly obtain alkali lye.
The preparation of tri compound enzyme:65g acidic cellulases, 23g fructosidases and 20g protease are well mixed, are obtained To tri compound enzyme.
Mix the preparation of alcoholic solution:It is 75% by ethanol water that 1200g mass fractions are 95%, 100g mass fractions The normal propyl alcohol aqueous solution and the mixing of isopropanol water solution that 133g mass fractions are 78%, stir, obtain mixing alcoholic solution.
The method that the material that above-mentioned early stage is prepared is used for following extraction Arillus longan polysaccharides.
2. a kind of method for extracting Arillus longan polysaccharide, comprises the following steps:
(1) slurrying and activation process:The fresh arillus longans of 100g and 400g pure water are mixed, is poured into homogenizer and is made Slurry, is subsequently adding 33g alkali lye, and 10.5h is activated at minus 5 DEG C, obtains activating solution;
(2) enzymolysis and concentration:The pH value for adjusting activating solution is 5, and 1.5g cupric oxide-oxidation is then added in filtrate Zr catalyst and 6g tri compound enzymes, are digested under conditions of 400W microwaves, and the reaction temperature of controlled enzymatic hydrolysis is 63 DEG C and the reaction time be 51min, then the enzymolysis liquid obtained after enzymolysis is concentrated by ultrafiltration, retain 5-50KD point with milipore filter Son amount enzymolysis liquid, temperature be 49 DEG C, pressure be -0.09MPa under conditions of vacuum distillation to solid content be 87%, obtain To concentrate;
(3) centrifugal treating:Concentrate and 650g mixed alcohol solution are mixed, after ultrasonically treated 33min, is received with centrifuge Collection precipitate;
(4) spray drying treatment:Precipitate is washed with 90 DEG C of deionized water, rotation throwing disc rotating speed is put into after cooling is 19s is dried in the rotation type atomization drier of 18000r/min, Arillus longan polysaccharide is obtained.
Embodiment 3:
1. early-stage preparations:
The preparation of copper oxide-zirconium oxide catalyst:43g anhydrous cupric sulfates, 37g zirconium oxychlorides are added to 260g deionizations In water, while stirring be added dropwise mass fraction be 44% sodium hydroxide solution, regulation 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 with 1150 DEG C of roasting 3h in Muffle furnace Catalyst.
The preparation of alkali lye:10g potassium hydroxide, the ammoniacal liquor that 24g mass fractions are 25% and 130g deionized waters are mixed, is stirred Mix and uniformly obtain alkali lye.
The preparation of tri compound enzyme:66g acidic cellulases, 30g fructosidases and 26g protease are well mixed, are obtained To tri compound enzyme.
Mix the preparation of alcoholic solution:It is 75% by ethanol water that 1450g mass fractions are 95%, 100g mass fractions The normal propyl alcohol aqueous solution and the mixing of isopropanol water solution that 170g mass fractions are 82%, stir, obtain mixing alcoholic solution.
The method that the material that above-mentioned early stage is prepared is used for following extraction Arillus longan polysaccharides.
2. a kind of method for extracting Arillus longan polysaccharide, comprises the following steps:
(1) slurrying and activation process:The fresh arillus longans of 100g and 360g pure water are mixed, is poured into homogenizer and is made Slurry, is subsequently adding 26g alkali lye, and 11.5h is activated at minus 6 DEG C, obtains activating solution;
(2) enzymolysis and concentration:The pH value for adjusting activating solution is 5, and 1.5g cupric oxide-oxidation is then added in filtrate Zr catalyst and 7g tri compound enzymes, are digested under conditions of 390W microwaves, and the reaction temperature of controlled enzymatic hydrolysis is 60 DEG C and the reaction time be 54min, then the enzymolysis liquid obtained after enzymolysis is concentrated by ultrafiltration, retain 5-50KD point with milipore filter Son amount enzymolysis liquid, temperature be 49 DEG C, pressure be -0.09MPa under conditions of vacuum distillation to solid content be 92%, obtain To concentrate;
(3) centrifugal treating:Concentrate and 640g mixed alcohol solution are mixed, after ultrasonically treated 36min, is received with centrifuge Collection precipitate;
(4) spray drying treatment:Precipitate is washed with 91 DEG C of deionized water, rotation throwing disc rotating speed is put into after cooling is 22s is dried in the rotation type atomization drier of 20000r/min, Arillus longan polysaccharide is obtained.
Embodiment 4:
1. early-stage preparations:
The preparation of copper oxide-zirconium oxide catalyst:47g anhydrous cupric sulfates, 40g zirconium oxychlorides are added to 255g deionizations In water, while stirring be added dropwise mass fraction be 43% sodium hydroxide solution, regulation pH value be 10, filtering, take filter residue, spend from Sub- water washing 2 times, dries, microwave drying 13min, finally obtains cupric oxide-oxidation with 1250 DEG C of roasting 3.5h in Muffle furnace Zr catalyst.
The preparation of alkali lye:10g potassium hydroxide, the ammoniacal liquor that 25g mass fractions are 25% and 110g deionized waters are mixed, is stirred Mix and uniformly obtain alkali lye.
The preparation of tri compound enzyme:63g acidic cellulases, 24g fructosidases and 28g protease are well mixed, are obtained To tri compound enzyme.
Mix the preparation of alcoholic solution:It is 73% by ethanol water that 1500g mass fractions are 95%, 100g mass fractions The normal propyl alcohol aqueous solution and the mixing of isopropanol water solution that 140g mass fractions are 84%, stir, obtain mixing alcoholic solution.
The method that the material that above-mentioned early stage is prepared is used for following extraction Arillus longan polysaccharides.
2. a kind of method for extracting Arillus longan polysaccharide, comprises the following steps:
(1) slurrying and activation process:The fresh arillus longans of 100g and 360g pure water are mixed, is poured into homogenizer and is made Slurry, is subsequently adding 24g alkali lye, and 10h is activated at minus 7 DEG C, obtains activating solution;
(2) enzymolysis and concentration:The pH value for adjusting activating solution is 4.5, and 2.5g cupric oxide-oxygen is then added in filtrate Change Zr catalyst and 6.5g tri compound enzymes, digested under conditions of 300W microwaves, the reaction temperature of controlled enzymatic hydrolysis It is 55min with the reaction time to be 66 DEG C, and then the enzymolysis liquid obtained after enzymolysis is concentrated by ultrafiltration, and 5- is retained with milipore filter The enzymolysis liquid of 50KD molecular weight, temperature be 52 DEG C, pressure be -0.09MPa under conditions of vacuum distillation to solid content be 87%, obtain concentrate;
(3) centrifugal treating:Concentrate and 580g mixed alcohol solution are mixed, after ultrasonically treated 32min, is received with centrifuge Collection precipitate;
(4) spray drying treatment:Precipitate is washed with 90 DEG C of deionized water, rotation throwing disc rotating speed is put into after cooling is 23s is dried in the rotation type atomization drier of 19000r/min, Arillus longan polysaccharide is obtained.
Embodiment 5:
1. early-stage preparations:
The preparation of copper oxide-zirconium oxide catalyst:44g anhydrous cupric sulfates, 36g zirconium oxychlorides are added to 250g deionizations In water, while stirring be added dropwise mass fraction be 47% sodium hydroxide solution, regulation pH value be 11, filtering, take filter residue, spend from Sub- water washing 4 times, dries, microwave drying 19min, finally obtains cupric oxide-oxidation with 1300 DEG C of roasting 3.5h in Muffle furnace Zr catalyst.
The preparation of alkali lye:10g potassium hydroxide, the ammoniacal liquor that 25g mass fractions are 25% and 135g deionized waters are mixed, is stirred Mix and uniformly obtain alkali lye.
The preparation of tri compound enzyme:68g acidic cellulases, 30g fructosidases and 22g protease are well mixed, are obtained To tri compound enzyme.
Mix the preparation of alcoholic solution:It is 76% by ethanol water that 1550g mass fractions are 95%, 100g mass fractions The normal propyl alcohol aqueous solution and the mixing of isopropanol water solution that 176g mass fractions are 85%, stir, obtain mixing alcoholic solution.
The method that the material that above-mentioned early stage is prepared is used for following extraction Arillus longan polysaccharides.
2. a kind of method for extracting Arillus longan polysaccharide, comprises the following steps:
(1) slurrying and activation process:The fresh arillus longans of 100g and 368g pure water are mixed, is poured into homogenizer and is made Slurry, is subsequently adding 32g alkali lye, and 10h is activated at minus 9 DEG C, obtains activating solution;
(2) enzymolysis and concentration:The pH value for adjusting activating solution is 5, and 2g copper oxide-zirconium oxides are then added in filtrate Catalyst and 7g tri compound enzymes, are digested under conditions of 260W microwaves, 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 enzymolysis is concentrated by ultrafiltration, 5-50KD molecules is retained with milipore filter The enzymolysis liquid of amount, temperature be 48 DEG C, pressure be -0.09MPa under conditions of vacuum distillation to solid content be 92%, obtain Concentrate;
(3) centrifugal treating:Concentrate and 590g mixed alcohol solution are mixed, after ultrasonically treated 30min, is received with centrifuge Collection precipitate;
(4) spray drying treatment:Precipitate is washed with 88 DEG C of deionized water, rotation throwing disc rotating speed is put into after cooling is 23s is dried in the rotation type atomization drier of 22000r/min, Arillus longan polysaccharide is obtained.
Embodiment 6:
1. early-stage preparations:
The preparation of copper oxide-zirconium oxide catalyst:50g anhydrous cupric sulfates, 45g zirconium oxychlorides are added to 300g deionizations In water, the sodium hydroxide solution that 25g mass fractions are 50% is added dropwise while stirring, regulation pH value is 12, and filtering takes filter residue, uses Deionized water is washed 4 times, is dried, microwave drying 20min, finally obtains cupric oxide-oxygen with 1250 DEG C of roasting 4h in Muffle furnace Change Zr catalyst.
The preparation of alkali lye:10g potassium hydroxide, the ammoniacal liquor that 30g mass fractions are 25% and 150g deionized waters are mixed, is stirred Mix and uniformly obtain alkali lye.
The preparation of tri compound enzyme:70g acidic cellulases, 35g fructosidases and 30g protease are well mixed, are obtained To tri compound enzyme.
Mix the preparation of alcoholic solution:It is 80% by ethanol water that 1600g mass fractions are 95%, 100g mass fractions The normal propyl alcohol aqueous solution and the mixing of isopropanol water solution that 200g mass fractions are 90%, stir, obtain mixing alcoholic solution.
The method that the material that above-mentioned early stage is prepared is used for following extraction Arillus longan polysaccharides.
2. a kind of method for extracting Arillus longan polysaccharide, comprises the following steps:
(1) slurrying and activation process:The fresh arillus longans of 100g and 500g pure water are mixed, is poured into homogenizer and is made Slurry, is subsequently adding 40g alkali lye, and 12h is activated at minus 10 DEG C, obtains activating solution;
(2) enzymolysis and concentration:The pH value for adjusting activating solution is 5.5, and 3g cupric oxide-oxidation is then added in filtrate Zr catalyst and 8g tri compound enzymes, are digested under conditions of 500W microwaves, and the reaction temperature of controlled enzymatic hydrolysis is 75 DEG C and the reaction time be 60min, then the enzymolysis liquid obtained after enzymolysis is concentrated by ultrafiltration, retain 5-50KD point with milipore filter Son amount enzymolysis liquid, temperature be 60 DEG C, pressure be -0.09MPa under conditions of vacuum distillation to solid content be 95%, obtain To concentrate;
(3) centrifugal treating:Concentrate and 700g mixed alcohol solution are mixed, after ultrasonically treated 40min, is received with centrifuge Collection precipitate;
(4) spray drying treatment:Precipitate is washed with 95 DEG C of deionized water, rotation throwing disc rotating speed is put into after cooling is 30s is dried in the rotation type atomization drier of 25000r/min, Arillus longan polysaccharide is obtained.
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 alkali 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 use Rotary Evaporators concentration.
Contrast test 1:
The Arillus longan polysaccharide in 100 fresh arillus longans, inspection are respectively extracted by the technical method of comparative example 1-3 and embodiment 1-6 The purity of Arillus longan polysaccharide yield and Arillus longan polysaccharide is surveyed, testing result is shown in Table 1.
Table 1:
The result of table 1 shows:The yield of Arillus longan polysaccharide is higher, illustrates that the production efficiency of the technical method is higher, longan Meat polysaccharide yield is arranged as from high to low:Embodiment 4>Embodiment 3=embodiments 6>Embodiment 2>Embodiment 1>Embodiment 5>It is right Ratio 2>Comparative example 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 It is high to Low to be arranged as:Embodiment 4>Embodiment 5>Embodiment 2>Embodiment 6>Embodiment 3>Embodiment 1>Comparative example 3>Comparative example 3> Comparative example 1.
Described above is directed to the detailed description of preferably possible embodiments of the invention, but embodiment is not limited to this hair Bright patent claim, the equal change completed under the technical spirit suggested by all present invention or modification change, all should belong to Cover the scope of the claims in the present invention.

Claims (8)

1. it is a kind of extract Arillus longan polysaccharide method, it is characterised in that:Comprise the following steps:
(1) slurrying and activation process:Fresh arillus longan and pure water are mixed, slurrying in homogenizer is poured into, alkali is subsequently adding Liquid, 10-12h is activated at negative 4-10 DEG C, obtains activating solution;
(2) enzymolysis and concentration:Adjust activating solution pH value, then in filtrate add copper oxide-zirconium oxide catalyst and Tri compound enzyme, is digested under conditions of 200-500W microwaves, the reaction temperature of controlled enzymatic hydrolysis and reaction time, is connect The enzymolysis liquid that will be obtained after enzymolysis to be concentrated by ultrafiltration, obtain concentrate;
(3) centrifugal treating:Concentrate and mixed alcohol solution are mixed, after ultrasonically treated 25-40min, is analysed with centrifugal collection Go out thing;
(4) spray drying treatment:Precipitate is washed with 85-95 DEG C of deionized water, rotation throwing disc rotating speed is put into after cooling is 10-30s is dried in the rotation type atomization drier of 15000-25000r/min, Arillus longan polysaccharide is obtained.
2. it is according to claim 1 it is a kind of extract Arillus longan polysaccharide method, it is characterised in that:Oxygen described in step (2) Change copper-zirconia catalyst to be prepared by following methods:Count by weight, by 35-50 parts of anhydrous cupric sulfate, 30-45 parts of oxygen chlorine Change zirconium to be added in 200-300 parts of deionized water, it is the sodium hydroxide solution of 40-50% that mass fraction is added dropwise while stirring, is adjusted Section pH value is 9-12, and filtering takes filter residue, is washed with deionized 2-4 times, dries, microwave drying 10-20min, finally in Muffle With 1100-1300 DEG C of roasting 2-4h in stove, copper oxide-zirconium oxide catalyst is obtained.
3. it is according to claim 1 it is a kind of extract Arillus longan polysaccharide method, it is characterised in that:Alkali described in step (1) Liquid is by weight 1:1-3:The potassium hydroxide of 10-15, mass fraction are that 25% ammoniacal liquor and deionized water are mixed.
4. it is according to claim 1 it is a kind of extract Arillus longan polysaccharide method, it is characterised in that:Described in step (2) three First complex enzyme is by weight 50-70:20-35:The acidic cellulase of 15-30, fructosidase and protease are mixed.
5. it is according to claim 1 it is a kind of extract Arillus longan polysaccharide method, it is characterised in that:PH described in step (2) It is 4.5-5.5 to be worth, and described reaction temperature is 50-75 DEG C, and the described reaction time is 40-60min.
6. it is according to claim 1 it is a kind of extract Arillus longan polysaccharide method, it is characterised in that:It is super described in step (2) Filter concentration is the enzymolysis liquid that 5-50KD molecular weight is retained using milipore filter, is 40-60 DEG C in temperature, and pressure is the bar of -0.09MPa Vacuum distillation to solid content is 80-95% under part.
7. it is according to claim 1 it is a kind of extract Arillus longan polysaccharide method, it is characterised in that:It is mixed described in step (3) It is by weight 10-16 to close alcoholic solution:1:The mass fraction of 1-2 be 95% ethanol water, mass fraction be 70-80% The normal propyl alcohol aqueous solution and the isopropanol water solution that mass fraction is 70-90% are mixed.
8. the method for a kind of extraction Arillus longan polysaccharide according to claim 1-7 any one, it is characterised in that:Described Fresh arillus longan, pure water, alkali lye, copper oxide-zirconium oxide catalyst, tri compound enzyme and mixing alcoholic solution weight ratio be 100:250-500:20-40:1-3:5-8:500-700.
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CN108841477A (en) * 2018-06-29 2018-11-20 广西壮族自治区农业科学院农产品加工研究所 A method of western melon wine is made using micro-aerobe fermentation technology
CN108913420A (en) * 2018-06-29 2018-11-30 广西壮族自治区农业科学院农产品加工研究所 A kind of fragrance high-fidelity type Fragrant fruit wine and its brewing method
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