CN110433190A - A method of the separation and Extraction effective component from cowberry - Google Patents
A method of the separation and Extraction effective component from cowberry Download PDFInfo
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Abstract
The method for separation and Extraction effective component that the invention discloses a kind of from cowberry, including complex enzyme formulation handle cowberry, and column purification processing is extracted and crossed in centrifuge separation, pass through atomizing freeze drying processing to Bilberry fruit P.E after purification.The extracting method extraction efficiency is high, and anthocyanin content has met the requirement of American-European pharmacopeia 36% or more in the Bilberry fruit P.E of acquisition.The present invention selects the combination of enzyme for reducing the dosage of enzyme, improving enzymolysis efficiency and improving recovery rate aspect significant effect, extract is handled by way of atomizing freeze drying, physicochemical property for ensuring product is particularly significant, and the properties of product of Bilberry fruit P.E have obtained apparent improvement.
Description
Technical field
The present invention relates to plant component extraction fields, and in particular to a kind of side of the separation and Extraction effective component from cowberry
Method.
Background technique
Cowberry is also known as blue berry or blueberries, belongs to Ericaceae cowberry platymiscium, whole world cowberry platymiscium there are about
450 kinds, wild species are distributed widely in the areas such as Northern Hemisphere temperate zone, subtropical zone, nutriment rich in cranberry, mesh
The purposes of the preceding Bilberry fruit P.E studied includes that improve eyesight include capillary and improvement circulatory function, anti-oxidant
With remove free radical etc., wherein anthocyanidin has very strong inoxidizability, and researching value is higher.
Anthocyanidin belongs to flavone compound, usually with one or more glucose, rhamnose, galactolipin, arabinose
Anthocyanin is formed Deng by glucosides, mainly there are 5 kinds of anthocyanidin in cowberry, with galactolipin, glucose and arabinose etc. with glucosides
Bond closes and forms anthocyanin.
It include at present extraction, microwave abstracting, supercritical fluid extraction etc. for the processing method of Bilberry fruit P.E, such as Hu Xiao
Plum etc. studies macroporous resin adsorption analysis purifying whortle extract, the whortle extract flower obtained by resin purification
For green cellulose content 25 or more, anthocyanin content is higher than 36%.Anthocyanin class substance can be dissolved in water and ethanol solution, but not dissolve in
The organic solvents such as ether, chloroform, and illumination, temperature, pH etc. can influence the stability of anthocyanin.At eighties of last century 80 years
Generation, anthocyanin have just entered American market as a kind of antioxidant food.
Bilberry fruit P.E as drug or with improve a certain genius morbi play preferable effect generally require purity compared with
Height, simple extraction process is more difficult to meet general international standard (liquid phase measurement anthocyanin >=36%).It is domestic at present also only
There are a small number of several companies that can accomplish the Bilberry fruit P.E of high-content, such as Beijing Jin Ke company, Guilin Rheinland Corporation, Beijing
Anthocyanin content of the Jin Ke company in blueberry extract has reached 36% or more.I.e. for the processing of China's Bilberry fruit P.E and
Speech, high-content, high-purity Bilberry fruit P.E for restricting the main reason for current Bilberry fruit P.E produces.
Summary of the invention
Based on problems of the prior art, the present invention is directed to obtain, a kind of anthocyanin content is high to be separated from cowberry
The method of effective component extracting.
Technical scheme is as follows.
A method of the separation and Extraction effective component from cowberry comprises the following steps that
(1) it takes cowberry to clean, the cold water of 15-30% is added, slurry is made in cowberry using beater；
(2) complex enzyme formulation is added, the group of the complex enzyme formulation becomes cellulase, pectase, mannase and chitin
The combination of matter enzyme, the dosage of the complex enzyme formulation are 0.001-2%, heat up and thermostatic control is in 20-60 DEG C of enzymolysis processing, enzyme
Time control is solved in 0.5-3h；
(3) it is centrifugated, obtains centrifugate and filter residue；
(4) it extracts, the ethanol solution that addition volumetric concentration is 50-80% is into centrifugate, the volume weight of ethanol solution and cowberry
Than adding cowberry quality 1-3% citric acid for 8-15:1, controlled at 50-60 DEG C, 30min-4h is extracted；
(5) column processing is crossed, the extracting solution that step (4) processing obtains is subjected to adsorption treatment using macroreticular resin, elution flow rate is
2BV/h, benefit is washed with distilled water after absorption, and distillation water consumption is 5-10 times of resin column volume, then utilizes 5-10 times of 40-
60% ethanol solution is eluted, and collection obtains eluent；By eluent using polyamide adsorption treatment, elution flow rate
It for 1-2BV/h, is then eluted using 5-10 times of 35-50% ethanol solution, collection obtains eluent；
(6) it is dried and obtains Bilberry fruit P.E.
For anthocyanin, since it is influenced by illumination, heat etc., it will lead to its stability and destroyed, therefore this
Invention selects the cold water of addition 15-30% in step (1), and reducing caused by the heat that it is generated during slurrying has
The destruction of ingredient is imitated, the temperature of the cold water is 1-4 DEG C.
Further, selection atomizing freeze drying is dried in the step (6)；Eluent is concentrated at 25 DEG C
After lower relative density is 1.10-1.20, atomizing freeze drying is carried out, the spray pattern is air-stream spraying, and air mass flow is
15-25m3/ h, air pressure 0.6-0.8MPa, the temperature of spray chamber are -45 DEG C, and processing is to the extract at needle-shaped production
Object；Then vacuum freeze drying is handled, and treatment temperature is -5 to -10 DEG C, and drying time is that 1-8h obtains Bilberry fruit P.E.
In current existing research, spray drying is the processing mode of relatively conventional Bilberry fruit P.E, however for this
In the performance of final products and pessimistic for mode, its higher temperature may be brought to anthocyanin first
Detrimental effect, secondly from the point of view of the performance of basis in the market, also there is certain shakiness in prolonged storage period physicochemical property
Pledge love condition.Therefore the mode of present invention selection atomizing freeze drying is handled, and the treatment conditions of low temperature can be avoided temperature to pattern
The influence of glycosides, and the product moisture absorption and agglomeration performance are significantly improved.
Further, the drying time is 1-6h, 2-5h, 2-4h etc., the vacuum freeze drying treatment temperature
It can be -6 DEG C, -8 DEG C.
Further, hydrolysis temperature is preferably 35-45 DEG C in the step (2), and enzymatic hydrolysis pH control is in 4-6.
Further, the proportion of the complex enzyme formulation cellulase, pectase, mannonase chitinase
For 10-15:8-10:1-2:1-2.
For the anthocyanin in cowberry, major part is stored in cytoplasm, therefore effectively broken wall hand at the extraction
Section is very crucial for improving recovery rate.As CN101775417A is realized using the complex enzyme of cellulase and pectase
Broken wall improves yield.As CN106749151A is disclosed using pectase, hemicellulase, cellulase rapidly extracting cyanine
The product degree of purity of element, acquisition is high.
And it is reduced by cost and still has larger problem, such as the study found that effectively improve enzymolysis efficiency
The dosage of enzyme has reached 1% or more in CN106749151A.For plant enzymolysis broken wall, cellulase, hemicellulase and
Pectase is the type of relatively conventional enzyme, the present invention on the basis of existing technology, further exploratory development complex enzyme system
Influence of the agent for broken wall or extraction efficiency, the study found that enzyme of the present invention combination can be effectively reduced the use of enzyme
Amount, and the further raising for promoting extraction efficiency.
Therefore, further, the present invention in complex enzyme formulation dosage be 0.005-1%, 0.01-0.08%, 0.008%,
0.01%, 0.05% etc..
Further, extraction time is 1-2h in the step (4), and the Citric Acid Dosage is 1.2-2%.As a result it shows
Show, adds the enough raisings for promoting extraction efficiency to a certain extent of soft acid performance of extraction environment after citric acid.
Further, macroreticular resin is DA201-M8 in the step (5), and the polyamide is 15-25 mesh.
For macroreticular resin, common model includes HP-20, AB-8, DA201, DM21 etc..Macroreticular resin is more satisfactory pure
The method for changing anthocyanin, for target product and impurity, it has apparent difference on absorption property, thus by absorption and
Parsing can obtain the higher product of purity.It has been the common research in this field for resin adsorption, the present invention is into one
Step ground selects the combination of macroreticular resin and polyamide to improve the effect of absorption, and research is found for DA201-M8 and polyamides
The combination of polyimide resin shows ideal result.
Further, the vacuum drying time is 2-5h.
Further, the Bilberry fruit P.E effective component that preparation method of the present invention obtains includes Cyanidin class flower
Green element, delphinidin class anthocyanidin, high mallow element class anthocyanidin, petunidin class anthocyanidin.For the present invention, it further grinds
The composition for studying carefully active material in extract is very important for the property for ensuring product.
The invention has the benefit that extracting method extraction efficiency of the present invention is high, anthocyanin in the Bilberry fruit P.E of acquisition
Content has met the requirement of American-European related pharmacopeia 36% or more.The present invention selects the combination of enzyme for reducing the dosage of enzyme, mentioning
Significant effect in terms of high enzymolysis efficiency and raising recovery rate.The present invention selects the mode of atomizing freeze drying to handle extract, right
Particularly significant in the physicochemical property for ensuring product, the properties of product of Bilberry fruit P.E have obtained significantly changing in terms of especially agglomerating
It is kind.The residual of organic solvent-free of the present invention, and it is pollution-free, the active constituent also not further assured that using solution such as strong acid
Stablize.
Specific embodiment
Embodiment 1
A method of the separation and Extraction effective component from whortle comprises the following steps that
(1) it takes cowberry to clean, the cold water of 15-30% is added, cold water temperature is 2 DEG C, and slurry is made in cowberry using beater；
(2) complex enzyme formulation is added, the group of the complex enzyme formulation becomes cellulase, pectase, mannase and chitin
The combination of matter enzyme, the dosage of the complex enzyme formulation are 0.005%, and at 40 DEG C, enzymolysis time is controlled in 1h, fiber for thermostatic control
Plain enzyme, pectase, mannonase chitinase proportion be 15:8:1:1；
(3) it is centrifugated, obtains centrifugate and filter residue；
(4) it extracts, the ethanol solution that addition volumetric concentration is 60%, the envelope-bulk to weight ratio of ethanol solution and cowberry is 10:1, addition
1% citric acid of cowberry quality extracts 2h controlled at 50-60 DEG C；
(5) column processing is crossed, the extracting solution that step (4) processing obtains is subjected to adsorption treatment using DA201-M8 macroreticular resin, is washed
Separation of flow speed is 2BV/h, and benefit is washed with distilled water after absorption, and distillation water consumption is 8 times of resin column volumes, then utilizes 10 times
40-60% ethanol solution is eluted, and collection obtains eluent；By eluent using polyamide adsorption treatment, elution stream
Speed is 2BV/h, is then eluted using 10 times of 50% ethanol solution, and collection obtains eluent；
(6) it is dried and obtains Bilberry fruit P.E, be specifically chosen atomizing freeze drying；Eluent is concentrated at 25 DEG C relatively
After density is 1.10-1.20, atomizing freeze drying is carried out, the spray pattern is air-stream spraying, air mass flow 15-
25m3/ h, air pressure 0.6-0.8MPa, the temperature of spray chamber are -45 DEG C, and processing is to the extract at needle-shaped product；
Then vacuum freeze drying is handled, and for treatment temperature to -10 DEG C, drying time is that 4h obtains Bilberry fruit P.E.
Embodiment 2
A method of the separation and Extraction effective component from linberry comprises the following steps that
(1) it takes cowberry to clean, 25% cold water is added, cold water temperature is 2 DEG C, and slurry is made in cowberry using beater；
(2) complex enzyme formulation is added, the group of the complex enzyme formulation becomes cellulase, pectase, mannase and chitin
The combination of matter enzyme, the dosage of the complex enzyme formulation are 0.008%, and at 40 DEG C, enzymolysis time is controlled in 1h, fiber for thermostatic control
Plain enzyme, pectase, mannonase chitinase proportion be 15:8:1:1；
(3) it is centrifugated, obtains centrifugate and filter residue；
(4) it extracts, the ethanol solution that addition volumetric concentration is 60%, the envelope-bulk to weight ratio of ethanol solution and cowberry is 10:1, addition
The citric acid of cowberry quality 1.2% extracts 2h controlled at 50-60 DEG C；
(5) column processing is crossed, the extracting solution that step (4) processing obtains is subjected to adsorption treatment using DA201-M8 macroreticular resin, is washed
Separation of flow speed is 2BV/h, and benefit is washed with distilled water after absorption, and distillation water consumption is 10 times of resin column volumes, then utilizes 10
Times 40-60% ethanol solution is eluted, and collection obtains eluent；By eluent using polyamide adsorption treatment, elution
Flow velocity is 2BV/h, is then eluted using 10 times of 50% ethanol solution, and collection obtains eluent；
(6) it is dried and obtains Bilberry fruit P.E, be specifically chosen atomizing freeze drying；Eluent is concentrated at 25 DEG C relatively
After density is 1.20, atomizing freeze drying is carried out, the spray pattern is air-stream spraying, air mass flow 25m3/ h, air
Pressure is 0.8MPa, and the temperature of spray chamber is -45 DEG C, and processing is to the extract at needle-shaped product；Then vacuum refrigeration is dry
Dry processing, for treatment temperature to -10 DEG C, drying time is that 3.5h obtains Bilberry fruit P.E.
Embodiment 3
A method of the separation and Extraction effective component from whortle comprises the following steps that
(1) it takes cowberry to clean, 15% cold water is added, cold water temperature is 1 DEG C, and slurry is made in cowberry using beater；
(2) complex enzyme formulation is added, the group of the complex enzyme formulation becomes cellulase, pectase, mannase and chitin
The combination of matter enzyme, the dosage of the complex enzyme formulation are 0.08%, and thermostatic control is at 40 DEG C, and enzymolysis time control is in 1.5h, enzymatic hydrolysis
PH control in 4-6, complex enzyme formulation cellulase, pectase, mannonase chitinase proportion be 10:8:1:1；
(3) it is centrifugated, obtains centrifugate and filter residue；
(4) it extracts, the ethanol solution that addition volumetric concentration is 50-80%, the envelope-bulk to weight ratio of ethanol solution and cowberry is 8-15:
1,1.5% citric acid of cowberry quality is added, controlled at 50-60 DEG C, extracts 2h；
(5) column processing is crossed, the extracting solution that step (4) processing obtains is subjected to adsorption treatment using DA201-M8 macroreticular resin, is washed
Separation of flow speed is 2BV/h, and benefit is washed with distilled water after absorption, and distillation water consumption is 8 times of resin column volumes, then utilizes 10 times
40-60% ethanol solution is eluted, and collection obtains eluent；By eluent using 20 mesh polyamide adsorption treatments, wash
Separation of flow speed is 2BV/h, is then eluted using 10 times of 35-50% ethanol solutions, and collection obtains eluent；
(6) it is dried and obtains Bilberry fruit P.E, be dried selection atomizing freeze drying, eluent is concentrated at 25 DEG C
After relative density is 1.10, atomizing freeze drying is carried out, the spray pattern is air-stream spraying, air mass flow 18m3/ h,
Air pressure is 0.7MPa, and the temperature of spray chamber is -45 DEG C, and processing is to the extract at needle-shaped product；Then vacuum is cold
Freeze and be dried, treatment temperature is -8 DEG C, and drying time is that 4h obtains Bilberry fruit P.E.
The product is analyzed, effective component includes Cyanidin class anthocyanidin, delphinidin class anthocyanidin, high mallow element class cyanine
Element, petunidin class anthocyanidin.
Comparative example 1
A method of the separation and Extraction effective component from whortle comprises the following steps that
(1) it takes cowberry to clean, the cold water of 15-30% is added, cold water temperature is 2 DEG C, and slurry is made in cowberry using beater；
(2) complex enzyme formulation is added, the group of the complex enzyme formulation becomes cellulase, pectase, hemicellulase combination, institute
The dosage for stating complex enzyme formulation is 0.5%, and thermostatic control is at 40 DEG C, and enzymolysis time control is in 1h, cellulase, pectase and half
The ratio of cellulase is 1:1:1；
(3) it is centrifugated, obtains centrifugate and filter residue；
(4) it extracts, the ethanol solution that addition volumetric concentration is 60%, the envelope-bulk to weight ratio of ethanol solution and cowberry is 10:1, addition
1% citric acid of cowberry quality extracts 2h controlled at 50-60 DEG C；
(5) column processing is crossed, the extracting solution that step (4) processing obtains is subjected to adsorption treatment using DA201-M8 macroreticular resin, is washed
Separation of flow speed is 2BV/h, and benefit is washed with distilled water after absorption, and distillation water consumption is 8 times of resin column volumes, then utilizes 10 times
40-60% ethanol solution is eluted, and collection obtains eluent；By eluent using polyamide adsorption treatment, elution stream
Speed is 2BV/h, is then eluted using 10 times of 50% ethanol solution, and collection obtains eluent；
(6) it is dried and obtains Bilberry fruit P.E, be specifically chosen atomizing freeze drying；Eluent is concentrated at 25 DEG C relatively
After density is 1.10-1.20, atomizing freeze drying is carried out, the spray pattern is air-stream spraying, air mass flow 15-
25m3/ h, air pressure 0.6-0.8MPa, the temperature of spray chamber are -45 DEG C, and processing is to the extract at needle-shaped product；
Then vacuum freeze drying is handled, and for treatment temperature to -10 DEG C, drying time is that 4h obtains Bilberry fruit P.E.
Comparative example 2
A method of the separation and Extraction effective component from whortle comprises the following steps that
(1) it takes cowberry to clean, the cold water of 15-30% is added, cold water temperature is 2 DEG C, and slurry is made in cowberry using beater；
(2) complex enzyme formulation is added, the group of the complex enzyme formulation becomes cellulase, pectase, mannase and chitin
The combination of matter enzyme, the dosage of the complex enzyme formulation are 0.005%, and at 40 DEG C, enzymolysis time is controlled in 1h, fiber for thermostatic control
Plain enzyme, pectase, mannonase chitinase proportion be 15:8:1:1；
(3) it is centrifugated, obtains centrifugate and filter residue；
(4) it extracts, the ethanol solution that addition volumetric concentration is 60%, the envelope-bulk to weight ratio of ethanol solution and cowberry is 10:1, addition
1% citric acid of cowberry quality extracts 2h controlled at 50-60 DEG C；
(5) column processing is crossed, the extracting solution that step (4) processing obtains is subjected to adsorption treatment, elution stream using AB-8 macroreticular resin
Speed is 2BV/h, and benefit is washed with distilled water after absorption, and distillation water consumption is 8 times of resin column volumes, then utilizes 10 times of 40-
60% ethanol solution is eluted, and collection obtains eluent；By eluent using polyamide adsorption treatment, elution flow rate
It for 2BV/h, is then eluted using 10 times of 50% ethanol solution, collection obtains eluent；
(6) it is dried and obtains Bilberry fruit P.E, be specifically chosen atomizing freeze drying；Eluent is concentrated at 25 DEG C relatively
After density is 1.10-1.20, atomizing freeze drying is carried out, the spray pattern is air-stream spraying, air mass flow 15-
25m3/ h, air pressure 0.6-0.8MPa, the temperature of spray chamber are -45 DEG C, and processing is to the extract at needle-shaped product；
Then vacuum freeze drying is handled, and for treatment temperature to -10 DEG C, drying time is that 4h obtains Bilberry fruit P.E.
Comparative example 3
A method of the separation and Extraction effective component from whortle comprises the following steps that
(1) it takes cowberry to clean, the cold water of 15-30% is added, cold water temperature is 2 DEG C, and slurry is made in cowberry using beater；
(2) complex enzyme formulation is added, the group of the complex enzyme formulation becomes cellulase, pectase, mannase and chitin
The combination of matter enzyme, the dosage of the complex enzyme formulation are 0.005%, and at 40 DEG C, enzymolysis time is controlled in 1h, fiber for thermostatic control
Plain enzyme, pectase, mannonase chitinase proportion be 15:8:1:1；
(3) it is centrifugated, obtains centrifugate and filter residue；
(4) it extracts, the ethanol solution that addition volumetric concentration is 60%, the envelope-bulk to weight ratio of ethanol solution and cowberry is 10:1, addition
1% citric acid of cowberry quality extracts 2h controlled at 50-60 DEG C；
(5) column processing is crossed, the extracting solution that step (4) processing obtains is subjected to adsorption treatment using DA201-M8 macroreticular resin, is washed
Separation of flow speed is 2BV/h, and benefit is washed with distilled water after absorption, and distillation water consumption is 8 times of resin column volumes, then utilizes 10 times
40-60% ethanol solution is eluted, and collection obtains eluent；By eluent using polyamide adsorption treatment, elution stream
Speed is 2BV/h, is then eluted using 10 times of 50% ethanol solution, and collection obtains eluent；
(6) it is dried and obtains Bilberry fruit P.E, specific choice spray drying；Controlling intake air temperature is 170-220 DEG C, outlet air
Mouth temperature is 70-120 DEG C.
Comparative example 4
A method of the separation and Extraction effective component from whortle comprises the following steps that
(1) it takes cowberry to clean, the normal-temperature water of 15-30% is added, slurry is made in cowberry using beater；
(2) complex enzyme formulation is added, the group of the complex enzyme formulation becomes the combination of cellulase, pectase, the complex enzyme
The dosage of preparation is 1.2%, thermostatic control at 40 DEG C, enzymolysis time control in 1h, cellulase, pectase proportion be 1:1；
(3) it is centrifugated, obtains centrifugate and filter residue；
(4) it extracts, the ethanol solution that addition volumetric concentration is 60%, the envelope-bulk to weight ratio of ethanol solution and cowberry is 10:1, control
Temperature is 50-60 DEG C, extracts 2h；
(5) column processing is crossed, the extracting solution that step (4) processing obtains is subjected to adsorption treatment using DA201-M8 macroreticular resin, is washed
Separation of flow speed is 2BV/h, and benefit is washed with distilled water after absorption, and distillation water consumption is 8 times of resin column volumes, then utilizes 10 times
40-60% ethanol solution is eluted, and collection obtains eluent；By eluent using polyamide adsorption treatment, elution stream
Speed is 2BV/h, is then eluted using 10 times of 50% ethanol solution, and collection obtains eluent；
(6) it is dried and obtains Bilberry fruit P.E, be specifically chosen atomizing freeze drying；Eluent is concentrated at 25 DEG C relatively
After density is 1.10-1.20, atomizing freeze drying is carried out, the spray pattern is air-stream spraying, air mass flow 15-
25m3/ h, air pressure 0.6-0.8MPa, the temperature of spray chamber are -45 DEG C, and processing is to the extract at needle-shaped product；
Then vacuum freeze drying is handled, and for treatment temperature to -10 DEG C, drying time is that 4h obtains Bilberry fruit P.E.
Interpretation of result
Utilize the content of anthocyanin in HPLC method measurement extract.Although HPLC method is relatively complicated compared with UV-vis, it is surveyed
It fixes really, therefore HPLC method is selected to analyze its content, be with C-3-G standard reference material and corn flower standard
Reference substance is reference, the peak of various anthocyanin and anthocyanidin monomer is demarcated respectively under 535nm wavelength, by calculating accordingly
Method calculates the content of single anthocyanin and anthocyanidin, and addition obtains Anthocyanin content.The partial parameters of test method are as follows:
Chromatographic column: octadecyl silane chromatographic column, length 250mm；
Mobile phase: A Xiang Weishui: formic acid=91.5:8.5 mixes 915ml water and 85ml formic acid, deaerates spare；B phase is 225ml
Methanol, 225ml acetonitrile, 100ml formic acid and 400ml water mix, and deaerate spare；
Detection wavelength is 535nm；Flow velocity is 1ml/min.
The result (general international standard) for measuring embodiment and comparative example respectively, according to single chlorination anthocyanin or chlorination flower
The ratio of the molecular weight of the molecular weight and chlorination Cyanidin -3-O- glucoside standard items or chlorination Cyanidin standard items of pigment
Value measures the content of single anthocyanin, and Anthocyanin content is the summation of single anthocyanin content, as a result as follows.
| Project | Anthocyanin content |
| Embodiment 1 | 52% |
| Comparative example 1 | 41% |
| Comparative example 2 | 44% |
| Comparative example 4 | 39% |
It can thus be seen that the anthocyanin content of the invention in the Bilberry fruit P.E product of acquisition is high, with comparative example phase
Than entire technique obtains good extraction effect, with comparative example comparative analysis it is found that the present invention is in the combination of enzyme, resin
More preferably effect is achieved in terms of combination and the improvement (addition of cold water, addition of citric acid etc. in pulping process) of technique.
Stability analysis
Sample is placed in 40 ± 1 DEG C, carries out stability analysis (accelerated test) under conditions of relative humidity 75%, with 1 He of embodiment
Comparative example 3 is measured for experimental subjects, measures the 0th day, 30 days, 60 days, 90 days agglomeration situations respectively, sample is crossed 60 mesh
Sieve, the quality/product quality * 100% of caking rate=stay on sieve, test result is as follows:
Embodiment 1 the 0th day, 30 days, 60 days, 90 days agglomeration situations be respectively 0,0,0 and 0.14%, comparative example 3 the 0th day, 30
It, 60 days, 90 days agglomeration situations be respectively 0,0.15%, 0.68%, 1.79%.It can be seen that the application selection processing mode with it is right
Comparing than file has larger improvement in product agglomeration performance, and properties of product are preferable.
Claims (8)
1. a kind of method of the separation and Extraction effective component from cowberry, it is characterised in that comprise the following steps that
(1) it takes cowberry to clean, the cold water of 15-30% is added, slurry is made in cowberry using beater；
(2) complex enzyme formulation is added, the group of the complex enzyme formulation becomes cellulase, pectase, mannase and chitin
The combination of matter enzyme, the dosage of the complex enzyme formulation are 0.001-2%, and thermostatic control is in 20-60 DEG C of progress enzymolysis processing, enzymatic hydrolysis
Time controls in 0.5-3h；
(3) it is centrifugated, obtains centrifugate and filter residue；
(4) it extracts, the ethanol solution that addition volumetric concentration is 50-80%, the envelope-bulk to weight ratio of ethanol solution and cowberry is 8-15:
1, cowberry quality 1-3% citric acid is added, controlled at 50-60 DEG C, extracts 30min-4h；
(5) column processing is crossed, the extracting solution that step (4) processing obtains is subjected to adsorption treatment using macroreticular resin, elution flow rate is
2BV/h, benefit is washed with distilled water after absorption, and distillation water consumption is 5-10 times of resin column volume, then utilizes 5-10 times of 40-
60% ethanol solution is eluted, and collection obtains eluent；By eluent using polyamide adsorption treatment, elution flow rate
It for 1-2BV/h, is then eluted using 5-10 times of 35-50% ethanol solution, collection obtains eluent；
(6) it is dried and obtains Bilberry fruit P.E.
2. the method for the separation and Extraction effective component according to claim 1 from cowberry, it is characterised in that the step
(6) selection atomizing freeze drying is dried in；Eluent is concentrated at 25 DEG C after relative density is 1.10-1.20, into
Row atomizing freeze drying, the spray pattern are air-stream spraying, air mass flow 15-25m3/ h, air pressure 0.6-
0.8MPa, the temperature of spray chamber are -45 DEG C, and processing is to the extract at needle-shaped product；Then vacuum freeze drying is handled,
Treatment temperature is -5 to -10 DEG C, and drying time is that 1-8h obtains Bilberry fruit P.E.
3. the method for the separation and Extraction effective component according to claim 1 from cowberry, it is characterised in that the step
(2) hydrolysis temperature is 35-45 DEG C in, and enzymatic hydrolysis pH control is in 4-6.
4. the method for the separation and Extraction effective component according to claim 1 from cowberry, it is characterised in that described is compound
Enzyme preparation cellulase, pectase, mannonase chitinase proportion be 10-15:8-10:1-2:1-2.
5. the method for the separation and Extraction effective component according to claim 1 from cowberry, it is characterised in that the step
(5) macroreticular resin is DA201-M8 in, and the polyamide is 15-25 mesh.
6. the method for the separation and Extraction effective component according to claim 1 from cowberry, it is characterised in that the step
(4) extraction time is 1-2h in, and the Citric Acid Dosage is 1.2-2%.
7. the method for the separation and Extraction effective component according to claim 2 from cowberry, it is characterised in that the vacuum
Drying time is 2-5h.
8. the Bilberry fruit P.E that the method for the separation and Extraction effective component described in claim 1 from cowberry is prepared, special
Sign is that effective component includes Cyanidin class anthocyanidin, delphinidin class anthocyanidin, high mallow element class anthocyanidin, petunidin class
Anthocyanidin.
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| CN114886886A (en) * | 2022-05-09 | 2022-08-12 | 中国计量大学 | Application of cowberry anthocyanin for relieving ultraviolet irradiation damage |
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