CN107286264A - The deep working method of Chinese date nutrient material separation - Google Patents
The deep working method of Chinese date nutrient material separation Download PDFInfo
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- CN107286264A CN107286264A CN201710345852.8A CN201710345852A CN107286264A CN 107286264 A CN107286264 A CN 107286264A CN 201710345852 A CN201710345852 A CN 201710345852A CN 107286264 A CN107286264 A CN 107286264A
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Classifications
-
- 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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/20—Reducing nutritive value; Dietetic products with reduced nutritive value
- A23L33/21—Addition of substantially indigestible substances, e.g. dietary fibres
- A23L33/22—Comminuted fibrous parts of plants, e.g. bagasse or pulp
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H19/00—Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof
- C07H19/02—Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof sharing nitrogen
- C07H19/04—Heterocyclic radicals containing only nitrogen atoms as ring hetero atom
- C07H19/16—Purine radicals
- C07H19/20—Purine radicals with the saccharide radical esterified by phosphoric or polyphosphoric acids
- C07H19/213—Purine radicals with the saccharide radical esterified by phosphoric or polyphosphoric acids containing cyclic phosphate
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Polymers & Plastics (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Sustainable Development (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Materials Engineering (AREA)
- Botany (AREA)
- Mycology (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to a kind of deep working method of Chinese date nutrient material separation, comprise the steps of：Jujube is extracted using ethanol solution, extract solution is passed through macroporous absorbent resin, ion exchange resin and macroporous absorbent resin and isolates and purifies to obtain date polysaccharide and Chinese date cyclic adenosine monophosphate extract successively；Jujube residue is extracted, filtering must be precipitated and supernatant respectively, and precipitation is through decolourizing, washing, dries, crush to obtain jujube insoluble diedairy fiber, and supernatant is concentrated, decolouring, alcohol precipitation, centrifugation, drying, crush to obtain jujube water-soluble dietary fiber；Not only production process is safe, environment-friendly by the present invention, it is often more important that in process of production, farthest make use of the jujube resource of preciousness, each constituents are separated step by step, raw material is fully converted into product, with good economic benefit and social benefit.
Description
Technical field
The invention belongs to the deep working method of food processing technology field, more particularly to a kind of separation of Chinese date nutrient material.
Background technology
Jujube all as this wooden grain of integration of drinking and medicinal herbs, plays an important role in the life of people all the time.
Contain Multiple components in jujube, complex chemical composition, including it is carbohydrate, amino acids, flavonoids, alkaloid and saponins, organic
The bioactive ingredients such as acids, vitamin and mineral element, CAMP, Polyphenols, dietary fiber, all with very good
Medicinal curative effect, Central nervous system, cardiovascular system and immune system have different degrees of regulation and protective effect.
Date polysaccharide is important bioactive substance in jujube, and can classify water-soluble neutral polysaccharide and acidic polysaccharose.It is existing
Show that date polysaccharide has a multiple biological activities for pharmaceutical research, including enhancing macrophage phagocytic function, to accelerate lymph thin
Dysuria with lower abdominal colic is changed and is immunized excitement, antioxidation, regulation cell growth and aging and repairs the effect such as hepatic injury, can be widely used for doctor
Medicine, health food and functional food, with wide market prospects.
CAMP (cAMP) is a kind of important substance with physiologically active being widely present in organism, is nucleosides
The derivative of acid, can wide participation cell function regulation, can diastole smooth muscle, expansion blood vessel, improve liver function, promote nerve
Function, the activity of promotion respiratory chain oxidizing ferment and the improvement heart regenerate, suppressed skin outer layer cell division and convert abnormal cell
Flesh anoxic.Scientists are found, all containing this material of CAMP in most of living species on the earth, but and
Other semiochemicalses are the same, and its content is very small, it is difficult to extract.1979 and two Japanese Scientists discovery jujubes in 1984
In containing abundant CAMP, be tens thousand of times of content in general animals and plants material, the content in more than 180 kinds of natural plants
New direction has been guided in highest, this extraction for being found to be the natural CAMP of scientists study.
Dietary fiber is the various plants material of SNSP, mostlys come from the cell membrane of animals and plants, including fiber
Element, lignin, wax, chitin, pectin, beta glucan, synanthrin and oligosaccharide etc., are generally divided into Water insoluble dietary fiber and water
The major class of soluble dietary fiber two.Dietary fiber has a variety of extensive pharmacotoxicological effects：Cleanable wall of digestive and enhancing digestion work(
Can, keep digestive system health；The chronic diseases such as prevention of cardiovascular disease, cancer, diabetes；Acceleration bodies inner cholesterol is drained,
Adjust blood glucose and cholesterol levels.Dietary fiber content enriches in jujube, meals is extracted in the jujube slag for processing generation from jujube fine
Dimension, realizes effective utilization of waste resource, while also the utilization for red jujube processing byproduct provides new approaches.
China is jujube resource most abundant country in the world, and annual jujube yield is up to 100,000 tons or so, annual jujube
Export volume reaches nearly 10,000 tons or so, is unique jujube exporting country in the world.Current jujube is most of with dry in addition to a small amount of eat raw
Based on product.Traditional processing mode mainly has the forms such as the dry jujube of vacuum packaging, jujube fruit can, Preserved produciton, date powder and jujube piece,
With flourishing for jujube industry, jujube deep processing and comprehensive utilization technique there has also been certain progress, current jujube deep processing side
Formula mainly has the form processings such as jujube sauce, jujube vinegar, jujube wine.It can be seen that, processing of the China to jujube product at this stage is also stopped with exploitation
In artificial and primary process segment, in order to keep up with jujube industry development speed, jujube industry development bottleneck is broken through, is badly in need of expanding
Big jujube process scale, improves new-product development ability and deep processing scientific and technological content.
No. 200610102144.3 patents disclose a kind of method that CAMP is extracted from jujube, and the patented method is used
Ultrasonic extraction, twice mistake ion exchange resin after water immersion, a chromatographic resin, crystallization obtain CAMP；
201410006278.X patents describe from jujube extract CAMP method, this method water extract-alcohol precipitation, centrifugation,
The isolated Chinese date cyclic adenosine monophosphate of macroreticular resin, polyamide column；20121041236.X a number patent describes flash by ethanol
Extract, macroreticular resin isolates and purifies CAMP in extraction separation jujube；201310359528.3 a number patent describes preparation
The method of Red jujube flavor and polysaccharide, the step such as this method is beaten with water, digested, alcohol extracting, filtering, decolouring obtains Red jujube flavor and many
Sugar.Jujube process product is single in above-mentioned several patents, does not carry out the comprehensive utilization of product, and production cost is high, no
It is adapted to the comprehensive utilization of jujube resource.
The content of the invention
Present invention aims to overcome that the deficiencies in the prior art and provide and a kind of separate jujube cycli phosphate gland step by step
Glycosides, date polysaccharide, the comprehensive utilization deep working method of jujube dietary fiber.
The object of the present invention is achieved like this：1st, a kind of deep working method of Chinese date nutrient material separation, its feature exists
In comprising the following steps：
Step 1）, jujube raw material crushed, use ethanol solution heating extraction, filter to obtain jujube slag and extract solution；
Step 2）, by step 1）Obtained extract solution is cooled to high speed centrifugation after room temperature and removes precipitation, obtains supernatant 1, supernatant 1
By macroporous absorbent resin, distilled water washing impurity-removing collects efflux 1 and water lotion 1；Acid solution is eluted, and obtains eluent 1；
Step 3）, by step 2）The eluent 1 of middle gained collects efflux 2 by ion exchange resin, with distillation water washing,
Collection obtains water lotion 2；Efflux 2 and water lotion is 2-in-1 simultaneously, it is passed through macroporous absorbent resin, distilled water washing impurity-removing, then with having
Machine solvent elutes to obtain eluent 2, and eluent 2 is concentrated, and obtains concentrate 1, and concentrate 3 obtains destainer 1, destainer with activated carbon decolorizing
1 drying and crushing obtains Chinese date cyclic adenosine monophosphate extract；
Step 4）, take step 1）In jujube slag, plus distilled water stirs to obtain suspension, and suspension adjusts PH through sodium hydroxide
Afterwards, heating extraction, filtering must precipitate and supernatant 2；Precipitation hydrogen peroxide decolourizes, and gained, which decolourizes to precipitate, uses distillation water washing,
Drying and crushing obtains jujube insoluble diedairy fiber；
Step 5）, by step 4）Middle supernatant 2 is concentrated, and obtains concentrate 2, and concentrate 2 is handled with activated carbon decolorizing, obtains destainer 2,
Destainer 2 adds ethanol solution, and alcohol precipitation is stayed overnight, and centrifuging to precipitate, and drying and crushing obtains jujube water-soluble dietary fiber；
Step 6）, by step 2）Middle gained efflux 1 and water lotion 1 merge, and are concentrated to give concentrate 3, it is molten that concentrate 3 adds ethanol
Liquid, alcohol precipitation is stayed overnight, and centrifuging to precipitate, and drying and crushing obtains date polysaccharide extract.
Described step（1）Described in ethanol solution concentration be 10 wt%-50 wt%, ethanol solution and jujube raw material
Envelope-bulk to weight ratio is 8~12 times（V/M）, Extracting temperature is 50~80 DEG C.
Described step 2）Described in macroporous absorbent resin for be combined with skeleton quaternary amine base, primary amine groups, secondary amine or
The styrene resin of tertiary amine groups.
Described step 2）Described in acid solution for 0.1-2.0 mol/L hydrochloric acid solution, formic acid solution, acetic acid it is molten
One or more in liquid.
Described step 3）Described in ion exchange resin to be combined with sulfonic acid on skeleton（-SO3H）Or carboxylic acid（-
COOH）The ion exchange resin of function base.
Described step 3）Described in organic solvent be 30 wt%-60 wt% ethanol solutions；Described jujube cycli phosphate
C-AMP content >=20% in adenosine extract.
Described step 4）The envelope-bulk to weight ratio of middle distilled water and jujube slag raw material is 6-8 times（V/M）；Suspension is through hydroxide
After sodium regulation, PH is 8~10；Extracting temperature is 25~80 DEG C.
Described step（5）Described ethanol solution is 95 wt% ethanol, and ethanol solution is 3- with the volume ratio of destainer 2
5 times.
Described step（6）Described ethanol solution is 95wt% ethanol, and ethanol solution is 3-5 with the volume ratio of concentrate 3
Times；Described date polysaccharide extract polyoses content >=40%.
The present invention has following good effect：
（1）The present invention isolates and purifies cAMP using resin method from jujube, and the technique being only used in conjunction by resin just can obtain
The Fructus Jujubae extract of cAMP content >=20%, technique is simple, and the cAMP rates of transform are high, and product quality is stable, it is easy to long-term to preserve；
（2）The present invention obtains polyoses content using the ingenious polysaccharide reclaimed in macroreticular resin efflux and water lotion of alcohol precipitating method
>=40% byproduct, realizes the recycling of resource；
（3）The present invention extracts the dietary fiber in separation jujube slag using chemical method, respectively obtains insoluble diedairy fiber and water
Soluble dietary fiber, product is completely converted into by jujube slag；
（4）Production process of the present invention safety, it is environment-friendly, can isolated CAMP, polysaccharide, the class of dietary fiber three step by step
Product, product is fully converted into by raw material, and jujube resource is make use of to greatest extent, adds the scientific and technological content of jujube product,
With good economic benefit and social benefit.
Embodiment
Embodiment 1, a kind of deep working method of Chinese date nutrient material separation, it is characterised in that comprise the following steps：
Step 1）, jujube raw material crushed, 50~80 DEG C of extractions are heated to 10 wt%-50 wt% ethanol solutions, jujube is filtered to obtain
Slag and extract solution；Jujube raw material pulverized particles are unfavorable for c-AMP dissolution when excessive, come when particle is meticulous for follow-up filter bag
Difficulty, therefore jujube is ground into 0.5~1.0cm2 fritter；Described ethanol solution concentration is 10 wt%-50 wt%, ethanol
The envelope-bulk to weight ratio of solution and jujube raw material is 8~12 times（V/M）, Extracting temperature is 50~80 DEG C, and extraction time is 3 h.
Step 2）, by step 1）Obtained extract solution is cooled to high speed centrifugation after room temperature and removes precipitation, r/ points of rotating speed 5000
Clock -10000 r/ minutes, the min of centrifugal treating 5 removes precipitation, obtains supernatant 1, supernatant 1 passes through macroporous absorbent resin, macropore
Polymeric adsorbent is the styrene resin that quaternary amine base, primary amine groups, secondary amine or tertiary amine groups are combined with skeleton；Distillation water washing is removed
It is miscellaneous, collect efflux 1 and water lotion 1；Eluted, must washed with 0.1-2.0 mol/L hydrochloric acid solution, formic acid solution or acetic acid solution
De- liquid 1；
Step 3）, by step 2）The eluent 1 of middle gained is by ion exchange resin, and ion exchange resin is to be combined with skeleton
Sulfonic acid（-SO3H）Or carboxylic acid（-COOH）The ion exchange resin of function base；Efflux 2 is collected, with distillation water washing, is collected
To water lotion 2；Efflux 2 and water lotion is 2-in-1 simultaneously, it is passed through macroporous absorbent resin；Distilled water washing impurity-removing, then use 30 wt%-
60 wt% ethanol solutions elute to obtain eluent 2, and eluent 2 is concentrated, and obtain concentrate 1, and concentrate 3 obtains destainer with activated carbon decolorizing
1, activated carbon can further remove the impurity such as depigmentation, improve the content of CAMP in product；The drying and crushing of destainer 1 is obtained
Chinese date cyclic adenosine monophosphate extract；
Step 4）, take step 1）In jujube slag, stirred by the envelope-bulk to weight ratio of distilled water and jujube slag raw material for 6-8 extraordinarily distilled water
It is uniform to obtain suspension, after suspension is 8~10 through sodium hydroxide regulation PH to PH, it is heated to 25~80 DEG C of extractions, extraction time
For 2 ~ 3 hours, filtering must precipitate and supernatant 2；Precipitation hydrogen peroxide decolourizes, and gained decolourizes precipitation with water washing is distilled, and does
It is dry to crush to obtain jujube insoluble diedairy fiber；
Step 5）, by step 4）Middle supernatant 2 is concentrated, and obtains concentrate 2, and concentrate 2 is handled with activated carbon decolorizing, obtains destainer 2,
Destainer 2 adds 95 wt% ethanol solution, and ethanol solution is 3-5 times with the volume ratio of destainer 2；Alcohol precipitation is stayed overnight, and is centrifuged
It must precipitate, drying and crushing obtains jujube water-soluble dietary fiber；
Step 6）, by step 2）Middle gained efflux 1 and water lotion 1 merge, and are concentrated to give concentrate 3, and concentrate 3 adds 95wt%
Ethanol solution, ethanol solution and the volume ratio of concentrate 3 are 3-5 times, and alcohol precipitation is stayed overnight, and centrifuging to be precipitated, and drying and crushing is obtained
Date polysaccharide extract.
Embodiment 2, a kind of deep working method of Chinese date nutrient material separation, it is characterised in that comprise the following steps：
Step 1）1.0 kg jujubes are taken, 0.5~1.0 cm2 fritter is ground into, 8 L concentration of addition are 10wt% ethanol solutions, 50
3 h are extracted in stirring at DEG C, filter to obtain jujube slag and extract solution.
Step 2）Extract solution is cooled to after room temperature, 5000 r/ minutes, and the min of centrifugal treating 5 removes precipitation, obtains transparent supernatant
Liquid 1.1.0L macroporous absorbent resins on supernatant 1, with 2.0 L distilled water washing impurity-removings, collect efflux 1 and water lotion 1 are standby
With, then the hydrochloric acid solution elution for being 0.1mol/L with 2.0 L concentration, obtain eluent 1.
Step 3）By 0.5 L ion exchange resin on eluent 1, efflux 2 is collected, water washing is distilled with 1.0 L, is collected
Obtain water lotion 2, merge efflux 2 and water lotion 2, be passed through 0.8 L macroporous absorbent resins, with 2.4 L distilled water washing impurity-removings,
Eluted again with 4.0 L concentration for 30 wt% ethanol solutions, obtain eluent 2.Eluent 2 is concentrated except after alcohol, 0.5 g of addition is active
Charcoal is stirred, and decolourize 1 h, filters out activated carbon, the drying and crushing of destainer 1 is obtained into Chinese date cyclic adenosine monophosphate extract, c-AMP is detected to obtain
Content is 22.01%.
Step 4）Take step 1）In jujube slag, plus 6.0 L distilled water stir, with the hydrogen-oxygen that mass fraction is 5.0 %
Change sodium and adjust 2 h of stirring extraction at PH to 8.0,25 DEG C, filtering must precipitate and supernatant 2.4.0 L mass point are added in precipitation
Number is 1.5% hydrogen peroxide, and stirring 1 h of decolouring is centrifugally separating to obtain decolouring precipitation, then decolourized with 3.0 L distillation water washings
Precipitation, centrifuges precipitation, and precipitation drying and crushing is obtained into jujube insoluble diedairy fiber.
Step 5）Take step 4）In supernatant 2 be concentrated into 1.0 L, add the stirring of 1.0 g activated carbons, decolourize 2 h, filters out
Activated carbon, obtains destainer 2, it is 95 wt% ethanol solutions that destainer 2, which adds 3.0 L concentration, alcohol precipitation is stayed overnight, and centrifuging to sink
Form sediment, drying and crushing obtains jujube water-soluble dietary fiber.
Step 6）By step 2）The efflux 1 and water lotion 1 of middle collection merge, and are concentrated into 0.5 L, are concentrated to give concentrate 3,
1.5 L concentration are added for 95 wt% ethanol solutions, alcohol precipitation is stayed overnight, and centrifuging to precipitate, drying and crushing obtains date polysaccharide extraction
Thing, detect date polysaccharide content be 45.6%.
Embodiment 3, a kind of deep working method of Chinese date nutrient material separation, it is characterised in that comprise the following steps：
Step 1）2.0 kg jujubes are taken, 0.5~1.0 cm2 fritter is ground into, it is that 30wt% ethanol is molten to add 24.0 L concentration
Liquid, 3 h are extracted in stirring at 80 DEG C, filter to obtain jujube slag and extract solution.
Step 2）Extract solution is cooled to after room temperature, 8000 r/ minutes, and the min of centrifugal treating 5 removes precipitation, obtains transparent supernatant
Liquid 1.2.5 L macroporous absorbent resins on supernatant 1, with 7.5 L distilled water washing impurity-removings, collect efflux 1 and water lotion 1 are standby
With, then the hydrochloric acid solution elution for being 2.0mol/L with 5.0L concentration, obtain eluent 1.
Step 3）By 1.5L ion exchange resin on eluent 1, efflux 2 is collected, water washing is distilled with 6.0 L, is collected
Obtain water lotion 2, merge efflux 2 and water lotion 2, be passed through 2.0 L macroporous absorbent resins, with 6.0 L distilled water washing impurity-removings,
Eluted again with 6.0L concentration for 60 wt% ethanol solutions, obtain eluent 2.Eluent 2 is concentrated except after alcohol, 1.5 g of addition are active
Charcoal is stirred, and decolourize 1 h, filters out activated carbon, the drying and crushing of destainer 1 is obtained into Chinese date cyclic adenosine monophosphate extract, c-AMP is detected to obtain
Content is 20.91%.
Step 4）Take step 1）In jujube slag, plus 14.0 L distilled water stir, with the hydrogen-oxygen that mass fraction is 5.0 %
Change sodium and adjust 2 h of stirring extraction at PH to 10.0,60 DEG C, filtering must precipitate and supernatant 2.8.0 L mass point are added in precipitation
Number is 1.5% hydrogen peroxide, and stirring 1 h of decolouring is centrifugally separating to obtain decolouring precipitation, then decolourized with 8.0 L distillation water washings
Precipitation, centrifuges precipitation, and precipitation drying and crushing is obtained into jujube insoluble diedairy fiber.
Step 5）Take step 4）In supernatant 2 be concentrated into 2.0 L, add the stirring of 1.5 g activated carbons, decolourize 2 h, filters out
Activated carbon, obtains destainer 2, it is 95 wt% ethanol solutions that destainer 2, which adds 8.0 L concentration, alcohol precipitation is stayed overnight, and centrifuging to sink
Form sediment, drying and crushing obtains jujube water-soluble dietary fiber.
Step 6）By step 2）The efflux 1 and water lotion 1 of middle collection merge, and are concentrated into 1 L, are concentrated to give concentrate 3, plus
Enter 4 L concentration for 95 wt% ethanol solutions, alcohol precipitation is stayed overnight, and centrifuging to precipitate, and drying and crushing obtains date polysaccharide extract,
Detect date polysaccharide content be 41.9%.
Embodiment 4, a kind of deep working method of Chinese date nutrient material separation, it is characterised in that comprise the following steps：
Step 1）4.0 kg jujubes are taken, 0.5~1.0 cm2 fritter is ground into, it is 50wt% ethanol solutions, 65 to add 40L concentration
3 h are extracted in stirring at DEG C, filter to obtain jujube slag and extract solution.
Step 2）Extract solution is cooled to after room temperature, 10000 r/ minutes, and the min of centrifugal treating 5 removes precipitation, obtains on transparent
Clear liquid 1.4.0 L macroporous absorbent resins on supernatant 1, with 16.0 L distilled water washing impurity-removings, collect efflux 1 and water lotion 1
It is standby, then the hydrochloric acid solution elution for being 1.0mol/L with 12.0 L concentration, obtain eluent 1.
Step 3）By 4.0 L ion exchange resin on eluent 1, efflux 2 is collected, water washing is distilled with 8.0 L, is collected
Water lotion 2 is obtained, merges efflux 2 and water lotion 2, is passed through 6.0 L macroporous absorbent resins, is removed with 12.0 L distillations water washing
It is miscellaneous, then eluted with 8.0 L concentration for 50 wt% ethanol solutions, obtain eluent 2.Eluent 2 is concentrated except after alcohol, addition 3.0g lives
Property charcoal stirring, decolourize 1 h, filter out activated carbon, the drying and crushing of destainer 1 obtained into Chinese date cyclic adenosine monophosphate extract, detect to obtain c-
AMP contents are 21.4%.
Step 4）Take step 1）In jujube slag, plus 32.0 L distilled water stir, with the hydrogen-oxygen that mass fraction is 5.0 %
Change sodium and adjust 2 h of stirring extraction at PH to 9.0,80 DEG C, filtering must precipitate and supernatant 2.12.0 L mass point are added in precipitation
Number is 1.5% hydrogen peroxide, and stirring 1 h of decolouring is centrifugally separating to obtain decolouring precipitation, then decolourized with 10.0 L distillation water washings
Precipitation, centrifuges precipitation, and precipitation drying and crushing is obtained into jujube insoluble diedairy fiber.
Step 5）Take step 4）In supernatant 2 be concentrated into 4.0 L, add the stirring of 3.0 g activated carbons, decolourize 2 h, filters out
Activated carbon, obtains destainer 2, it is 95 wt% ethanol solutions that destainer 2, which adds 20.0 L concentration, alcohol precipitation is stayed overnight, and centrifuging to sink
Form sediment, drying and crushing obtains jujube water-soluble dietary fiber.
Step 6）By step 2）The efflux 1 and water lotion 1 of middle collection merge, and are concentrated into 2.0 L, are concentrated to give concentrate 3,
10.0 L concentration are added for 95 wt% ethanol solutions, alcohol precipitation is stayed overnight, and centrifuging to precipitate, and drying and crushing obtains date polysaccharide and carried
Take thing, detect date polysaccharide content be 43.4%.
Examples detailed above is only the preferred embodiment of the present invention, is not intended to limit the invention, for the technology of this area
For personnel, the present invention can have various modifications and variations, within the spirit and principles of the invention, and that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (9)
1. a kind of deep working method of Chinese date nutrient material separation, it is characterised in that comprise the following steps：
Step 1）, jujube raw material crushed, use ethanol solution heating extraction, filter to obtain jujube slag and extract solution；
Step 2）, by step 1）Obtained extract solution is cooled to high speed centrifugation after room temperature and removes precipitation, obtains supernatant 1, supernatant 1
By macroporous absorbent resin, distilled water washing impurity-removing collects efflux 1 and water lotion 1；Acid solution is eluted, and obtains eluent 1；
Step 3）, by step 2）The eluent 1 of middle gained collects efflux 2 by ion exchange resin, with distillation water washing,
Collection obtains water lotion 2；Efflux 2 and water lotion is 2-in-1 simultaneously, it is passed through macroporous absorbent resin, distilled water washing impurity-removing, then with having
Machine solvent elutes to obtain eluent 2, and eluent 2 is concentrated, and obtains concentrate 1, and concentrate 3 obtains destainer 1, destainer with activated carbon decolorizing
1 drying and crushing obtains Chinese date cyclic adenosine monophosphate extract；
Step 4）, take step 1）In jujube slag, plus distilled water stirs to obtain suspension, and suspension adjusts PH through sodium hydroxide
Afterwards, heating extraction, filtering must precipitate and supernatant 2；Precipitation hydrogen peroxide decolourizes, and gained, which decolourizes to precipitate, uses distillation water washing,
Drying and crushing obtains jujube insoluble diedairy fiber；
Step 5）, by step 4）Middle supernatant 2 is concentrated, and obtains concentrate 2, and concentrate 2 is handled with activated carbon decolorizing, obtains destainer 2,
Destainer 2 adds ethanol solution, and alcohol precipitation is stayed overnight, and centrifuging to precipitate, and drying and crushing obtains jujube water-soluble dietary fiber；
Step 6）, by step 2）Middle gained efflux 1 and water lotion 1 merge, and are concentrated to give concentrate 3, it is molten that concentrate 3 adds ethanol
Liquid, alcohol precipitation is stayed overnight, and centrifuging to precipitate, and drying and crushing obtains date polysaccharide extract.
2. the deep working method of Chinese date nutrient material separation according to claim 1, it is characterised in that：Described step
（1）Described in ethanol solution concentration be 10 wt%-50 wt%, the envelope-bulk to weight ratio of ethanol solution and jujube raw material is 8~12
Times（V/M）, Extracting temperature is 50~80 DEG C.
3. the deep working method of Chinese date nutrient material separation according to claim 1, it is characterised in that：Described step 2）
Described in macroporous absorbent resin to be combined with the styrene resin of quaternary amine base, primary amine groups, secondary amine or tertiary amine groups on skeleton.
4. the deep working method of Chinese date nutrient material separation according to claim 1, it is characterised in that：Described step 2）
Described in acid solution be 0.1-2.0 mol/L hydrochloric acid solution, the one or more in formic acid solution, acetic acid solution.
5. the deep working method of Chinese date nutrient material separation according to claim 1, it is characterised in that：Described step 3）
Described in ion exchange resin to be combined with sulfonic acid on skeleton（-SO3H）Or carboxylic acid（-COOH）The amberlite of function base
Fat.
6. the deep working method of Chinese date nutrient material separation according to claim 1, it is characterised in that：Described step 3）
Described in organic solvent be 30 wt%-60 wt% ethanol solutions；C-AMP contents in described Chinese date cyclic adenosine monophosphate extract
≥20%。
7. the deep working method of Chinese date nutrient material separation according to claim 1, it is characterised in that：Described step 4）
The envelope-bulk to weight ratio of middle distilled water and jujube slag raw material is 6-8 times（V/M）；After suspension is adjusted through sodium hydroxide, PH is 8~10；
Extracting temperature is 25~80 DEG C.
8. the deep working method of Chinese date nutrient material separation according to claim 1, it is characterised in that：Described step
（5）Described ethanol solution is 95 wt% ethanol, and ethanol solution is 3-5 times with the volume ratio of destainer 2.
9. the deep working method of Chinese date nutrient material separation according to claim 1, it is characterised in that：Described step
（6）Described ethanol solution is 95wt% ethanol, and ethanol solution is 3-5 times with the volume ratio of concentrate 3；Described date polysaccharide
Extract polyoses content >=40%.
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| CN114521651A (en) * | 2022-02-21 | 2022-05-24 | 沧州恩际生物制品有限公司 | New red date extracting solution extracted by red date extraction process |
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