CN108250315A - Dendrobium candidum extract and preparation method thereof - Google Patents
Dendrobium candidum extract and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of dendrobium candidum extract and preparation method thereof.The preparation method is as follows：(1) after dendrobium candidum is extracted with ethyl alcohol, filtering obtains extracting solution and filter residue；(2) feed liquid of the filter residue and water composition, through cellulase, amylase, protease hydrolyzed, obtains enzymolysis liquid.The preparation method can synchronize extraction Dendrobium officinale polysaccharide and polyphenols, and operating procedure is simple and convenient, rational technology.
Description
Technical field
The present invention relates to a kind of dendrobium candidum extracts and preparation method thereof.
Background technology
Dendrobium candidum (Dendrobium candidium wall ex lindl) is that orchid family Dendrobium perennial herb is planted
Object is China's tradition rare Chinese medicine.Global Dendrobium Sw has more than 1100 kinds, is mainly distributed on East Asia, Southeast Asia, New Guinea
And Australia.Dendrobium candidum is abounded in Yunnan Province of China southern areas, with purple dendrobium and firm arthrolith dry measure used in former times belong to by《The Chinese people
Republic's pharmacopeia》The Dendrobium Sw included has " nourishing Yin and promoting production of body fluid, the shield that wets one's whistle throat, warm stomach improving eyesight, kidney tonifying benefit power, macrobiosis benefit
The effect of longevity ".Taoist school that Tang was opened between the first year is classical《Taoist Scriptures》Once dendrobium candidum was classified as " first of Chinese nine big celestial grass ".
Favored on the market about the healthy food or drug of dendrobium candidum concept by consumers in general at present, product
Form is mainly the Tiepi Fengdou or dendrobium candidum ultrafine powder that dendrobium candidum stem obtains after overbaking is dried, but it is edible not
It is convenient, and it is mouldy easily to make moist, there are edible safety problems.In addition there are some dendrobium wines, be only capable of the low pole in the extraction stem of noble dendrobium
Property substance, cannot efficiently use the main composition polysaccharose substance of dendrobium candidum.
Chinese patent literature CN104740337A provides a kind of dendrobium candidum extract, specifically includes following four steps：Have
Dodged after solvent degreasing, alcohol solution dipping carry, Sevage reagents removing protein and activated carbon decolorizing.Chinese patent literature
CN100497396C is related to a kind of dendrobium candidum polysaccharide extractive and preparation method thereof, uses organic solvent petroleum ether, acetic acid second instead
Ester degreasing, water carry, ethanol precipitation and organic solvent petroleum ether, acetone, ether etc. are washed, and are then dried to obtain polysaccharide；This
Place it should be noted that the purpose of the column absorption in the patent document just for the sake of purified polysaccharide, can not by polysaccharide with
Outer ingredient carries out separation reservation.Chinese patent literature CN103190623A provides a kind of dendrobium candidum extract, and described carries
The content for taking Dendrobium officinale polysaccharide in object is 70.0%-90.0%, and the content of general flavone is 0.5-1.0%, also provides above-mentioned carry
The preparation method of object is taken, specifically includes following four steps：After organic solvent (such as petroleum ether) degreasing, alcohol solution dipping dodge carry,
Sevage reagents removing protein and activated carbon decolorizing.
The technique of foregoing invention patent all refers to the technique of organic solvent degreasing and Sevage reagent removing proteins, uses
Poisonous and hazardous chemical reagent, there are safety problems for production process, are unfavorable for industrialized production, and serious environment can be caused dirty
Dye.
In addition, all technique of the prior art is only capable of extraction Dendrobium officinale polysaccharide, can still be incited somebody to action without a kind of technique
Polyphenol component in dendrobium candidum extracts.
Invention content
The technical problems to be solved by the invention are the preparation methods in order to overcome dendrobium candidum extract in the prior art
It extracts using hazardous organic solvents, unsuitable industrialized production, pollution environment and only for a kind of ingredient of polysaccharose substance
The defects of, and provide it is a kind of without using hazardous organic solvents, be suitble to the big production of industry and can by the polysaccharide in dendrobium candidum and
The method that polyphenol component extracts.The preparation method can synchronize extraction Dendrobium officinale polysaccharide and polyphenols, and operate
Step is simple and convenient, rational technology.The preparation method of the present invention can also obtain Dendrobium officinale polysaccharide and dendrobium candidum in high yield
Polyphenol has certain economic and social benefit.
The present invention provides a kind of preparation method of dendrobium candidum extract, and the preparation method includes the following steps：
(1) after dendrobium candidum is extracted with ethyl alcohol, filtering obtains extracting solution and filter residue；
(2) feed liquid of the filter residue and water composition, through cellulase degradation, obtains enzymolysis liquid.
In step (1), the places of origin of raw materials of the dendrobium candidum can be Yunnan.
In step (1), the operation of the dendrobium candidum ethyl alcohol extraction and condition can be the behaviour of plant field extraction polyphenol
Work and condition.
In step (1), the dendrobium candidum with ethyl alcohol before being extracted, and preferably by dendrobium candidum herb, (fresh grass is dry
Grass) it is crushed to 1-3cm.
In step (1), the ethyl alcohol that the extraction uses is generally ethanol water, the body of ethyl alcohol in the ethanol water
Fraction can be 30%-95%, may be, for example, 50%, 70%, 85% or 90%, the quality of the ethanol water and the iron
The ratio of the quality of the skin stem of noble dendrobium can be (10-40)：1, it may be, for example, 10:1、12.5:1、15:1 or 20:1.
In step (1), the temperature of the extraction can be 40 DEG C -75 DEG C, may be, for example, 40 DEG C, 50 DEG C, 55 DEG C, 60 DEG C or 75
℃；The time of the extraction can be 1-3 hours, may be, for example, 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours.
In step (1), the main component in the extracting solution is dendrobium candidum polyphenols.
In step (2), the enzymolysis is referred to the substantially all decomposition of cellulose in the filter residue.
In step (2), the quality of the water and the ratio of the quality of the filter residue can be (5-40)：1, it may be, for example, 5:1、
10:1、12.5:1、15:1 or 20:1.
In step (2), the cellulase can be commercially available cellulase.Preferably, the cellulase is resistance to
It is 40 DEG C -60 DEG C by temperature, pH tolerant 4.0-6.0；Alternatively, the tolerable temperature of the cellulase is 40 DEG C -60 DEG C, it is resistance to
It is 4.0-6.0, and unit of activity >=300000U/g by pH value.More preferably, the pH value of the enzymolysis is 4.0-6.0, be may be, for example,
4.0th, 4.5,5.0,5.5 or 6.0；The temperature of the enzymolysis be 40 DEG C -60 DEG C, may be, for example, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C or
60℃；The time of the enzymolysis is 2-6 hours, be may be, for example, 2 hours, 3 hours, 4 hours, 5 hours or 6 hours；The fiber
0.05%-10% of the quality of plain enzyme for the quality of the water, may be, for example, 0.05%, 2%, 4%, 7% or 10%.
In step (2), preferably, the fibrous residue after dry and ultramicro grinding to get dendrobium candidum fiber powder, the iron
Skin dendrobium fiber powder can be used for functional food.
After step (2), preferably, carrying out step (3), in the step (3), the enzymolysis liquid is through alpha-amylase enzyme
Solution, after enzyme deactivation, filtering obtains fibrous residue and polysaccharide extraction liquid.
In step (3), the enzymolysis is referred to the substantially all decomposition of alphalise starch in the enzymolysis liquid.
In step (3), the alpha-amylase can be commercially available alpha-amylase.Preferably, the alpha-amylase is resistance to
It is 70 DEG C -85 DEG C by temperature, pH tolerant 5.0-6.0；Alternatively, the tolerable temperature of the alpha-amylase is 70 DEG C -85 DEG C, it is resistance to
It is 5.0-6.0, and unit of activity >=13000AAU/g by pH value.More preferably, the temperature of the enzymolysis is 70 DEG C -85 DEG C, such as
It can be 70 DEG C, 75 DEG C, 80 DEG C, 82 DEG C or 85 DEG C；The time of the enzymolysis be 1-3 hours, may be, for example, 1 hour, 1.5 hours, 2
Hour, 2.5 hours or 3 hours；0.1%-10% of the quality of the alpha-amylase for the quality of the enzymolysis liquid, may be, for example,
0.1%th, 2%, 6%, 8% or 10%.
In step (3), the enzyme deactivation refers to losing activity the cellulase and the alpha-amylase, the enzyme deactivation
Temperature higher than the deactivation temperature of the cellulase and the alpha-amylase, may be, for example, 90 DEG C -95 DEG C, the enzyme deactivation
Time continue all to inactivate to the cellulase and the alpha-amylase, may be, for example, 30 minutes.
More preferably, step (4) is carried out after the step (3), in the step (4), the polysaccharide extraction liquid is through macropore
After adsorbing resin, efflux is collected, until without polysaccharide in the efflux；Wherein, the macroporous absorbent resin for nonpolarity or
Low pole resin.
In step (4), the model of the macroporous absorbent resin is preferably D101, AB8, H-60, H103 or XDA-1B, institute
The flow velocity for stating polysaccharide extraction liquid can be 1BV/h-3BV/h, may be, for example, 1BV/h, 1.5BV/h, 2BV/h, 2.5BV/h or 3BV/h.
In step (4), preferably, the efflux obtains refined filtration liquid through secondary filter for the first time；The refined filtration liquid through nanofiltration,
Obtain nanofiltration retentate fluid；The nanofiltration retentate fluid after nanofiltration is washed, then carries out nanofiltration concentration with water, obtains nanofiltration concentrate；It is described
Nanofiltration concentrate is after protease hydrolyzed, through secondary filter again to get polysaccharide refined filtration liquid.
Wherein, the secondary filter for the first time uses the aperture of filter membrane to be preferably 0.22 μm -0.45 μm.
Wherein, the molecular cut off of NF membrane is preferably 300-500 used by the nanofiltration and the nanofiltration are washed.
Wherein, the ratio of the volume and the volume of the nanofiltration retentate fluid of nanofiltration washing water used is preferably 2-
10 times, it may be, for example, 2 times, 4 times, 6 times, 8 times or 10 times.
Wherein, the volume of the nanofiltration concentrate is preferably 2-5 times of the volume of the dendrobium candidum, may be, for example, 2
Again, 3 times, 3.5 times, 4 times or 5 times.
Wherein, the protease can be commercially available protease.Preferably, the tolerable temperature of the protease is 40
DEG C -60 DEG C, pH tolerant 4.0-6.0；Alternatively, the tolerable temperature of the protease is 40 DEG C -60 DEG C, pH tolerant 4.0-
6.0, and unit of activity >=500000HUT/g.More preferably, the pH value of the enzymolysis is 4.0-6.0, be may be, for example,；The enzymolysis
Temperature for 40 DEG C -60 DEG C, may be, for example, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C or 60 DEG C；The time of the enzymolysis is 2-6 hours,
It may be, for example, 2 hours, 3 hours, 4 hours, 5 hours or 6 hours；The quality of the protease is the quality of the nanofiltration concentrate
0.05%-2%, may be, for example, 0.05%, 0.5%, 1.0%, 1.5% or 2.0%.
Wherein, the secondary filter again uses the aperture of filter membrane to be preferably 0.22 μm -0.45 μm.
Wherein, preferably, the polysaccharide refined filtration liquid obtains polysaccharide concentrate after reduced pressure.More preferably, the polysaccharide is dense
Contracting liquid and ethyl alcohol, the mixed liquor of inorganic salts, it is agitated, precipitation is precipitated, obtains Dendrobium officinale polysaccharide crude product；Wherein, the mixed liquor
In, the mass fraction of ethyl alcohol is 50%-90%, may be, for example, 50%, 60%, 70%, 80%, 90%, the quality point of inorganic salts
Number is 0.5%-5%, may be, for example, 0.5%, 2%, 3%, 4%, 5%, the inorganic salts may be, for example, sodium chloride and/or acetic acid
Sodium.Further more preferably, after the Dendrobium officinale polysaccharide crude product is centrifuged, filters, Dendrobium officinale polysaccharide wet product is obtained.It is described
Dendrobium officinale polysaccharide wet product after drying to get Dendrobium officinale polysaccharide, the drying may be, for example, freeze-drying, vacuum drying or
Heated-air drying.
Further more preferably, step (5) is carried out after the step (4), in the step (5), the macroporous absorption tree
Fat is eluted through the ethanol water that volume fraction is 60%-80%, collects eluent, until the eluent is without flavones reaction
It can.In above-mentioned technical proposal, the cooperation of each technical characteristic and other features could cause polysaccharide extraction liquid through macroporous absorption tree
After fat, effectively polysaccharide and polyphenol component are detached, while remove removing heavy metals.
In step (5), the volume fraction of ethyl alcohol may be, for example, 70% in the ethanol water.
After step (5), preferably, by the eluent with after extracting solution merges described in step (1), through secondary filter
Refined filtration liquid is obtained, then through being concentrated under reduced pressure into no ethyl alcohol, obtains refined filtration concentrate.Wherein, the secondary filter uses the aperture of filter membrane
It can be 0.22 μm -0.45 μm；The vacuum degree of the reduced pressure can be 0.08pa-0.1pa, and the temperature of the reduced pressure can be
50 DEG C -70 DEG C, it may be, for example, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C or 70 DEG C.
Wherein, the refined filtration concentrate is mixed with polyalcohol, preservative and water, can obtain dendrobium candidum polyphenol solution；It is described
Polyalcohol may be, for example, propylene glycol and/or butanediol, and the preservative is to allow the preservative used in cosmetics, be may be, for example,
It is one or more in Phenoxyethanol, 9010 and A631.Further more preferably, in the dendrobium candidum polyphenol solution, iron sheet stone
The mass fraction of dry measure used in former times polyphenol is 1%-10%, and the mass fraction of the polyalcohol is 5%-50%.
Wherein, the refined filtration concentrate after drying, can obtain dendrobium candidum polyphenol solid powder, the dendrobium candidum polyphenol
Solid powder is rich in dendrobium candidum polyphenol and dendrobine；The drying may be, for example, freeze-drying or vacuum drying.
The present invention also provides a kind of using dendrobium candidum fiber powder described made from aforementioned preparation method.
The present invention also provides a kind of using Dendrobium officinale polysaccharide described made from aforementioned preparation method.
The present invention also provides a kind of using dendrobium candidum polyphenol solution described made from aforementioned preparation method.
The present invention also provides a kind of using dendrobium candidum polyphenol solid powder described made from aforementioned preparation method.
Without prejudice to the field on the basis of common sense, above-mentioned each optimum condition can be combined arbitrarily each preferably to get the present invention
Example.
The reagents and materials used in the present invention are commercially available.
The positive effect of the present invention is：The present invention provides a kind of dendrobium candidum extract and preparation method thereof.It should
Preparation method can synchronize extraction Dendrobium officinale polysaccharide and polyphenols, and operating procedure is simple and convenient, rational technology.This
The preparation method of invention can also obtain Dendrobium officinale polysaccharide and dendrobium candidum polyphenol in high yield, have certain economy and society
Benefit.
Specific embodiment
It is further illustrated the present invention below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.Test method without specific conditions in the following example, according to conventional methods and conditions or according to quotient
Product specification selects.
In following embodiments, the places of origin of raw materials of dendrobium candidum is Yunnan；Cellulase is that commercially available tolerable temperature is
40 DEG C -60 DEG C and pH tolerant are the cellulase of 4.0-6.0, and unit of activity >=300000U/g；Alpha-amylase for it is commercially available can
The alpha-amylase that the tolerable temperature obtained is 70 DEG C -85 DEG C and pH tolerant is 5.0-6.0, and unit of activity >=13000AAU/g；
Protease is the protease that commercially available tolerable temperature is 40 DEG C -60 DEG C and pH tolerant is 4.0-6.0, and unit of activity >=
500000HUT/g。
In following embodiments, in step (2), the mass percent of the cellulase refers to the matter of the cellulase
The ratio of amount and the quality of the water；In step (3), the mass percent of the alpha-amylase refers to the alpha-amylase
The ratio of quality and the quality of the enzymolysis liquid；In the preparation method of Dendrobium officinale polysaccharide, the mass percent of the protease
Refer to the ratio of the quality of the protease and the quality of the nanofiltration concentrate.
In following embodiments, the calculation formula of the yield of Dendrobium officinale polysaccharide is：The quality divided by original of Dendrobium officinale polysaccharide
Expect the quality of dendrobium candidum；The calculation formula of the yield of dendrobium candidum polyphenol solution is：The quality of dendrobium candidum polyphenol solution is removed
With the quality of raw material dendrobium candidum；The calculation formula of the yield of dendrobium candidum polyphenol solid powder is：Dendrobium candidum polyphenol solid
The quality of powder divided by the quality of raw material dendrobium candidum.
Embodiment 1
First, separation method
(1) dendrobium candidum herb (fresh grass) is taken to carry out precomminution with Chinese medicine boulder crusher, is ground into staple fiber shape 1-3cm；It will
In the good dendrobium candidum 200g input extractors of precomminution, the ethyl alcohol of 2000mL 70v% is added in, 50 DEG C of heat preservations are extracted 1 hour,
Filtering, obtains extracting solution and filter residue；It is mainly dendrobium candidum polyphenols in the extracting solution.
(2) 4000mL pure water is added in the filter residue, obtains feed liquid；The pH value for adjusting feed liquid is 5.0, and feed liquid is warming up to 40
DEG C, add in 7% cellulase, keep the temperature 3 hours, obtain enzymolysis liquid.
(3) pH value for adjusting the enzymolysis liquid is 5.0, is heated to 75 DEG C, adds in 2% high-temperatureα-amylase, heat preservation
3h, extraction terminate, and are warming up to 95 DEG C, and enzyme deactivation 30 minutes filters, obtains fibrous residue and polysaccharide extraction liquid while hot.
(4) polysaccharide extraction liquid carries out column chromatography for separation, and macroreticular resin D101, adsorption flow rate 1BV/h inhale
Attached end with pure water resin, is washed to efflux detection and is reacted without polysaccharide, collect efflux whole in the above process.
(5) ethanol water elution of the macroporous absorbent resin through 70v%, collects eluent, until the eluent
No flavones reaction.
2nd, the preparation method of dendrobium candidum fiber powder
By the fibrous residue in step (3) to get dendrobium candidum fiber powder after drying, ultramicro grinding, available for functionality
Food.
3rd, the preparation method of Dendrobium officinale polysaccharide
By the efflux in step (4), secondary filter (0.22 μm -0.45 μm) is carried out, collects refined filtration liquid；The refined filtration liquid
With NF membrane (molecular cut off：It 300-500) filters, obtains nanofiltration retentate fluid；The nanofiltration retentate fluid is mixed with 2 times of pure water,
After nanofiltration is washed, then nanofiltration concentration is carried out, and 2 times that the volume for being concentrated into nanofiltration concentrate is dendrobium candidum volume.
The pH value of above-mentioned nanofiltration concentrate is adjusted to 4.0,40 DEG C is warming up to, adds in 0.05% protease, heat preservation 2 is small
When, after secondary filter (0.22 μm -0.45 μm), collect refined filtration liquid, as polysaccharide refined filtration liquid.
After above-mentioned polysaccharide refined filtration liquid is concentrated under reduced pressure, polysaccharide concentrate is obtained, ethyl alcohol is added in extremely into the polysaccharide concentrate
The wherein volume fraction of ethyl alcohol is up to 50%, then adds in 0.5% sodium chloride thereto, and precipitation is precipitated in stirring, obtains Dendrobium officinale polysaccharide
Crude product.
The Dendrobium officinale polysaccharide crude product is centrifuged, is filtered, obtains Dendrobium officinale polysaccharide wet product.
By the Dendrobium officinale polysaccharide wet product it is freeze-dried after to get Dendrobium officinale polysaccharide.
Effect data：The yield of Dendrobium officinale polysaccharide is 25.67%.
4th, the preparation method of dendrobium candidum polyphenol solution
Eluent in step (5) is merged with the extracting solution in step (1), secondary filter (0.22 μm of filter sizes-
0.45 μm), and at vacuum degree 0.08pa-0.1pa and 65 DEG C, no ethyl alcohol is concentrated under reduced pressure into, obtain refined filtration concentrate；
Propylene glycol, preservative (Phenoxyethanol), pure water are added in into above-mentioned refined filtration concentrate, is deployed into dendrobium candidum polyphenol
Solution, wherein：The content 1wt% of dendrobium candidum polyphenol, content of propylene glycol 5wt%, Phenoxyethanol content 0.4wt%.
Effect data：The yield of dendrobium candidum polyphenol solution is：153.5%.
Embodiment 2
First, separation method
(1) dendrobium candidum herb (fresh grass) is taken to carry out precomminution with Chinese medicine boulder crusher, is ground into staple fiber shape 1-3cm；It will
In the good dendrobium candidum 200g input extractors of precomminution, the ethyl alcohol of 4000mL 30v% is added in, 75 DEG C of heat preservations are extracted 2 hours,
Filtering, obtains extracting solution and filter residue；It is mainly dendrobium candidum polyphenols in the extracting solution.
(2) 1000mL pure water is added in the filter residue, obtains feed liquid；The pH value for adjusting feed liquid is 5.5, and feed liquid is warming up to 60
DEG C, add in 10% cellulase, keep the temperature 5 hours, obtain enzymolysis liquid.
(3) pH value for adjusting the enzymolysis liquid is 6.0, is heated to 82 DEG C, adds in 0.1% high-temperatureα-amylase, is protected
Warm 2.5h, extraction terminate, and are warming up to 95 DEG C, and enzyme deactivation 30 minutes filters, obtains fibrous residue and polysaccharide extraction liquid while hot.
(4) polysaccharide extraction liquid carries out column chromatography for separation, and macroreticular resin AB8, adsorption flow rate 3BV/h inhale
Attached end with pure water resin, is washed to efflux detection and is reacted without polysaccharide, collect efflux whole in the above process.
(5) ethanol water elution of the macroporous absorbent resin through 70v%, collects eluent, until the eluent
No flavones reaction.
2nd, the preparation method of dendrobium candidum fiber powder
By the fibrous residue in step (3) to get dendrobium candidum fiber powder after drying, ultramicro grinding, available for functionality
Food.
3rd, the preparation method of Dendrobium officinale polysaccharide
By the efflux in step (4), secondary filter (0.22 μm -0.45 μm) is carried out, collects refined filtration liquid；The refined filtration liquid
With NF membrane (molecular cut off：It 300-500) filters, obtains nanofiltration retentate fluid；The nanofiltration retentate fluid is mixed with 6 times of pure water,
After nanofiltration is washed, then nanofiltration concentration is carried out, and 3.5 times that the volume for being concentrated into nanofiltration concentrate is dendrobium candidum volume.
The pH value of above-mentioned nanofiltration concentrate is adjusted to 5.5,55 DEG C is warming up to, adds in 1.5% protease, heat preservation 4 is small
When, after secondary filter (0.22 μm -0.45 μm), collect refined filtration liquid, as polysaccharide refined filtration liquid.
After above-mentioned polysaccharide refined filtration liquid is concentrated under reduced pressure, polysaccharide concentrate is obtained, ethyl alcohol is added in extremely into the polysaccharide concentrate
The wherein volume fraction of ethyl alcohol is up to 80%, then adds in 3% sodium acetate thereto, and precipitation is precipitated in stirring, and it is thick to obtain Dendrobium officinale polysaccharide
Product.
The Dendrobium officinale polysaccharide crude product is centrifuged, is filtered, obtains Dendrobium officinale polysaccharide wet product.
By the Dendrobium officinale polysaccharide wet product it is freeze-dried after to get Dendrobium officinale polysaccharide.
Effect data：The yield of Dendrobium officinale polysaccharide is 29.28%.
4th, the preparation method of dendrobium candidum polyphenol solution
Eluent in step (5) is merged with the extracting solution in step (1), secondary filter (0.22 μm of filter sizes-
0.45 μm), and at vacuum degree 0.08pa-0.1pa and 55 DEG C, no ethyl alcohol is concentrated under reduced pressure into, obtain refined filtration concentrate；
Butanediol, preservative 9010, pure water are added in into above-mentioned refined filtration concentrate, is deployed into dendrobium candidum polyphenol solution,
Wherein：The content 10wt% of dendrobium candidum polyphenol, butanediol content 50wt%, 9010 content 0.8wt% of preservative.
Effect data：The yield of dendrobium candidum polyphenol solution is：216.7%.
Embodiment 3
First, separation method
(1) dendrobium candidum herb (fresh grass) is taken to carry out precomminution with Chinese medicine boulder crusher, is ground into staple fiber shape 1-3cm；It will
In the good dendrobium candidum 200g input extractors of precomminution, the ethyl alcohol of 2000mL 90v% is added in, 40 DEG C of heat preservations are extracted 3 hours,
Filtering, obtains extracting solution and filter residue；It is mainly dendrobium candidum polyphenols in the extracting solution.
(2) 3000mL pure water is added in the filter residue, obtains feed liquid；The pH value for adjusting feed liquid is 4.0, and feed liquid is warming up to 50
DEG C, add in 0.05% cellulase, keep the temperature 6 hours, obtain enzymolysis liquid.
(3) pH value for adjusting the enzymolysis liquid is 5.5, is heated to 85 DEG C, adds in 8% high-temperatureα-amylase, heat preservation
1h, extraction terminate, and are warming up to 95 DEG C, and enzyme deactivation 30 minutes filters, obtains fibrous residue and polysaccharide extraction liquid while hot.
(4) polysaccharide extraction liquid carries out column chromatography for separation, and macroreticular resin H103, adsorption flow rate 2BV/h inhale
Attached end with pure water resin, is washed to efflux detection and is reacted without polysaccharide, collect efflux whole in the above process.
(5) ethanol water elution of the macroporous absorbent resin through 70v%, collects eluent, until the eluent
No flavones reaction.
2nd, the preparation method of dendrobium candidum fiber powder
By the fibrous residue in step (3) to get dendrobium candidum fiber powder after drying, ultramicro grinding, available for functionality
Food.
3rd, the preparation method of Dendrobium officinale polysaccharide
By the efflux in step (4), secondary filter (0.22 μm -0.45 μm) is carried out, collects refined filtration liquid；The refined filtration liquid
With NF membrane (molecular cut off：It 300-500) filters, obtains nanofiltration retentate fluid；The nanofiltration retentate fluid is mixed with 10 times of pure water,
After nanofiltration is washed, then nanofiltration concentration is carried out, and 5 times that the volume for being concentrated into nanofiltration concentrate is dendrobium candidum volume.
The pH value of above-mentioned nanofiltration concentrate is adjusted to 6.0,45 DEG C is warming up to, adds in 0.5% protease, heat preservation 6 is small
When, after secondary filter (0.22 μm -0.45 μm), collect refined filtration liquid, as polysaccharide refined filtration liquid.
After above-mentioned polysaccharide refined filtration liquid is concentrated under reduced pressure, polysaccharide concentrate is obtained, ethyl alcohol is added in extremely into the polysaccharide concentrate
The wherein volume fraction of ethyl alcohol is up to 90%, then adds in 2% sodium acetate thereto, and precipitation is precipitated in stirring, and it is thick to obtain Dendrobium officinale polysaccharide
Product.
The Dendrobium officinale polysaccharide crude product is centrifuged, is filtered, obtains Dendrobium officinale polysaccharide wet product.
By the Dendrobium officinale polysaccharide wet product it is freeze-dried after to get Dendrobium officinale polysaccharide.
Effect data：The yield of Dendrobium officinale polysaccharide is 31.42%.
4th, the preparation method of dendrobium candidum polyphenol solution
Eluent in step (5) is merged with the extracting solution in step (1), secondary filter (0.22 μm of filter sizes-
0.45 μm), and at vacuum degree 0.08pa-0.1pa and 50 DEG C, no ethyl alcohol is concentrated under reduced pressure into, obtain refined filtration concentrate；
Butanediol, preservative A631, pure water are added in into above-mentioned refined filtration concentrate, is deployed into dendrobium candidum polyphenol solution,
Wherein：The content 5wt% of dendrobium candidum polyphenol, the content 1.5wt% of butanediol content 20wt%, preservative A631.
Effect data：The yield of dendrobium candidum polyphenol solution is：185.7%.
Embodiment 4
First, separation method
(1) dendrobium candidum herb (fresh grass) is taken to carry out precomminution with Chinese medicine boulder crusher, is ground into staple fiber shape 1-3cm；It will
In the good dendrobium candidum 200g input extractors of precomminution, the ethyl alcohol of 3000mL 85v% is added in, 55 DEG C of heat preservation extractions 2.5 are small
When, filtering obtains extracting solution and filter residue；It is mainly dendrobium candidum polyphenols in the extracting solution.
(2) 2000mL pure water is added in the filter residue, obtains feed liquid；The pH value for adjusting feed liquid is 4.5, and feed liquid is warming up to 45
DEG C, add in 2% cellulase, keep the temperature 4 hours, obtain enzymolysis liquid.
(3) pH value for adjusting the enzymolysis liquid is 5.7, is heated to 70 DEG C, adds in 10% high-temperatureα-amylase, heat preservation
1.5h, extraction terminate, and are warming up to 95 DEG C, and enzyme deactivation 30 minutes filters, obtains fibrous residue and polysaccharide extraction liquid while hot.
(4) polysaccharide extraction liquid carries out column chromatography for separation, macroreticular resin XDA-1B, adsorption flow rate 2.5BV/
H, absorption terminate, and with pure water resin, wash to efflux detection and are reacted without polysaccharide, collect outflow whole in the above process
Liquid.
(5) ethanol water elution of the macroporous absorbent resin through 70v%, collects eluent, until the eluent
No flavones reaction.
2nd, the preparation method of dendrobium candidum fiber powder
By the fibrous residue in step (3) to get dendrobium candidum fiber powder after drying, ultramicro grinding, available for functionality
Food.
3rd, the preparation method of Dendrobium officinale polysaccharide
By the efflux in step (4), secondary filter (0.22 μm -0.45 μm) is carried out, collects refined filtration liquid；The refined filtration liquid
With NF membrane (molecular cut off：It 300-500) filters, obtains nanofiltration retentate fluid；The nanofiltration retentate fluid is mixed with 4 times of pure water,
After nanofiltration is washed, then nanofiltration concentration is carried out, and 3 times that the volume for being concentrated into nanofiltration concentrate is dendrobium candidum volume.
The pH value of above-mentioned nanofiltration concentrate is adjusted to 4.5,60 DEG C is warming up to, adds in 2.0% protease, heat preservation 3 is small
When, after secondary filter (0.22 μm -0.45 μm), collect refined filtration liquid, as polysaccharide refined filtration liquid.
After above-mentioned polysaccharide refined filtration liquid is concentrated under reduced pressure, polysaccharide concentrate is obtained, ethyl alcohol is added in extremely into the polysaccharide concentrate
The wherein volume fraction of ethyl alcohol is up to 60%, then adds in 4% sodium chloride thereto, and precipitation is precipitated in stirring, and it is thick to obtain Dendrobium officinale polysaccharide
Product.
The Dendrobium officinale polysaccharide crude product is centrifuged, is filtered, obtains Dendrobium officinale polysaccharide wet product.
By the Dendrobium officinale polysaccharide wet product it is freeze-dried after to get Dendrobium officinale polysaccharide.
Effect data：The yield of Dendrobium officinale polysaccharide is 27.85%.
4th, the preparation method of dendrobium candidum polyphenol solid powder
Eluent in step (5) is merged with the extracting solution in step (1), secondary filter (0.22 μm of filter sizes-
0.45 μm), and at vacuum degree 0.08pa-0.1pa and 70 DEG C, no ethyl alcohol is concentrated under reduced pressure into, obtain refined filtration concentrate；By above-mentioned essence
Filter concentration liquid is freeze-dried, and obtains dendrobium candidum polyphenol solid powder.
Effect data：The yield of dendrobium candidum polyphenol solid powder is：2.45%.
Embodiment 5
First, separation method
(1) dendrobium candidum herb (fresh grass) is taken to carry out precomminution with Chinese medicine boulder crusher, is ground into staple fiber shape 1-3cm；It will
In the good dendrobium candidum 200g input extractors of precomminution, the ethyl alcohol of 2500mL 50v% is added in, 60 DEG C of heat preservation extractions 1.5 are small
When, filtering obtains extracting solution and filter residue；It is mainly dendrobium candidum polyphenols in the extracting solution.
(2) 2500mL pure water is added in the filter residue, obtains feed liquid；The pH value for adjusting feed liquid is 6.0, and feed liquid is warming up to 55
DEG C, add in 4% cellulase, keep the temperature 2 hours, obtain enzymolysis liquid.
(3) pH value for adjusting the enzymolysis liquid is 5.8, is heated to 80 DEG C, adds in 6% high-temperatureα-amylase, heat preservation
2h, extraction terminate, and are warming up to 95 DEG C, and enzyme deactivation 30 minutes filters, obtains fibrous residue and polysaccharide extraction liquid while hot.
(4) the polysaccharide extraction liquid progress column chromatography for separation, macroreticular resin H-6, adsorption flow rate 1.5BV/h,
Absorption terminates, and with pure water resin, washs to efflux detection and is reacted without polysaccharide, collect outflow whole in the above process
Liquid.
(5) ethanol water elution of the macroporous absorbent resin through 70v%, collects eluent, until the eluent
No flavones reaction.
2nd, the preparation method of dendrobium candidum fiber powder
By the fibrous residue in step (3) to get dendrobium candidum fiber powder after drying, ultramicro grinding, available for functionality
Food.
3rd, the preparation method of Dendrobium officinale polysaccharide
By the efflux in step (4), secondary filter (0.22 μm -0.45 μm) is carried out, collects refined filtration liquid；The refined filtration liquid
With NF membrane (molecular cut off：It 300-500) filters, obtains nanofiltration retentate fluid；The nanofiltration retentate fluid is mixed with 8 times of pure water,
After nanofiltration is washed, then nanofiltration concentration is carried out, and 4 times that the volume for being concentrated into nanofiltration concentrate is dendrobium candidum volume.
The pH value of above-mentioned nanofiltration concentrate is adjusted to 5.0,50 DEG C is warming up to, adds in 1.0% protease, heat preservation 5 is small
When, after secondary filter (0.22 μm -0.45 μm), collect refined filtration liquid, as polysaccharide refined filtration liquid.
After above-mentioned polysaccharide refined filtration liquid is concentrated under reduced pressure, polysaccharide concentrate is obtained, ethyl alcohol is added in extremely into the polysaccharide concentrate
The wherein volume fraction of ethyl alcohol is up to 70%, then adds in 5% sodium chloride thereto, and precipitation is precipitated in stirring, and it is thick to obtain Dendrobium officinale polysaccharide
Product.
The Dendrobium officinale polysaccharide crude product is centrifuged, is filtered, obtains Dendrobium officinale polysaccharide wet product.
By the Dendrobium officinale polysaccharide wet product it is freeze-dried after to get Dendrobium officinale polysaccharide.
Effect data：The yield of Dendrobium officinale polysaccharide is 28.87%.
4th, the preparation method of dendrobium candidum polyphenol solid powder
Eluent in step (5) is merged with the extracting solution in step (1), secondary filter (0.22 μm of filter sizes-
0.45 μm), and at vacuum degree 0.08pa-0.1pa and 60 DEG C, no ethyl alcohol is concentrated under reduced pressure into, obtain refined filtration concentrate；
Above-mentioned refined filtration concentrate is freeze-dried, obtains dendrobium candidum polyphenol solid powder.
Effect data：The yield of dendrobium candidum polyphenol solid powder is：2.08%.
Embodiment 6
Said extracted liquid is concentrated after removing ethyl alcohol, is carried with polysaccharide with embodiment 1, step (4) by step (1), (2) and (3)
Liquid is taken to mix, continues to be concentrated into certain volume, is spray-dried, obtains dendrobium candidum extract dry product.
Effect data：Yield is：32.21%.
Embodiment 7
The protease hydrolyzed of step (5) in embodiment 3 is not used, other steps are the same as embodiment 3.
Effect data：The yield of Dendrobium officinale polysaccharide is 30.87%；The yield of dendrobium candidum polyphenol solution is 174.5%.
However, protein content increases in Dendrobium officinale polysaccharide, the M-band allergy risk of product when in use can be increased.
Comparative example 1
Step (1) merges with embodiment 2, step (2) and step (3), is extracted only with pure water high temperature, obtains extracting solution and filter
Slag；It is digested without cellulase and high-temperatureα-amylase, directly by the step (4) in extracting solution progress embodiment 2 and subsequently
Step.
Effect data：The yield of Dendrobium officinale polysaccharide is：18.59%.The yield of Dendrobium officinale polysaccharide compared to the examples,
It significantly reduces, total starches and mannose content reduce (concrete numerical value is shown in Table 1).Dendrobium candidum polyphenol solution yield 200.3%.
1 Dendrobium officinale polysaccharide quality index of table
Note：Mannose content and total starches content assaying method：2015 editions Chinese Pharmacopoeias, one dendrobium candidum；Nitrogen content is surveyed
Determine method：Kjeldahl's method；Molecular weight determination：Dextrane gel chromatography (using pulullan polysaccharide as standard items).
2 dendrobium candidum polyphenol quality index of table
Note：Determination of Polyphenols assay method：Folin＆Clocalteu ' s pHenol reagent,《Brewing science and technology》,
2011,2011(4):29-32。
Embodiment 1,2,3,7 and 1 gained polyphenol product of comparative example are dendrobium candidum polyphenol solution, then, it is total more in table 2
Phenol content refers to the polyphenol content in butt dendrobium candidum polyphenol solid powder.
4 and 5 gained polyphenol product of embodiment is dendrobium candidum polyphenol solid powder, and the Determination of Polyphenols in table 2 refers to
Polyphenol content in dendrobium candidum polyphenol solid powder.
Although specific embodiments of the present invention have been described above, it will be appreciated by those of skill in the art that this is only
For example, protection scope of the present invention is to be defined by the appended claims.Those skilled in the art without departing substantially from
Under the premise of the principle and substance of the present invention, various changes or modifications can be made to these embodiments, but these changes and
Modification each falls within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of dendrobium candidum extract, which is characterized in that the preparation method includes the following steps：
(1) after dendrobium candidum is extracted with ethyl alcohol, filtering obtains extracting solution and filter residue；
(2) feed liquid of the filter residue and water composition, through cellulase degradation, obtains enzymolysis liquid.
2. preparation method as described in claim 1, which is characterized in that in step (1), the dendrobium candidum is extracted with ethyl alcohol
Before, dendrobium candidum herb is first crushed to 1-3cm；
And/or in step (1), the ethyl alcohol used that extracts is ethanol water, the volume of ethyl alcohol in the ethanol water
Score is 30%-95%, and the ratio of the quality of the ethanol water and the quality of the dendrobium candidum is (10-40)：1；
And/or in step (1), the temperature of the extraction is 40 DEG C -75 DEG C, and the time of the extraction is 1-3 hours.
3. preparation method as described in claim 1, which is characterized in that in step (2), the quality of the water and the filter residue
The ratio of quality is (10-40)：1；
Preferably, in step (2), the tolerable temperature of the cellulase is 40 DEG C -60 DEG C, pH tolerant 4.0-6.0；Or
Person, the tolerable temperature of the cellulase is 40 DEG C -60 DEG C, pH tolerant 4.0-6.0, and unit of activity >=300000U/g；
The pH value of the enzymolysis is 4.0-6.0, and the temperature of the enzymolysis is 40 DEG C -60 DEG C, and the time of the enzymolysis is 2-6 hours, institute
State 0.05%-10% of the quality of cellulase for the quality of the water；
More preferably, in step (2), the fibrous residue is after dry and ultramicro grinding to get dendrobium candidum fiber powder.
4. preparation method as described in claim 1, which is characterized in that after the step (2), carry out step (3), the step
Suddenly the process of (3) is as follows：The enzymolysis liquid is through enzymolyzing alpha-amylase, and after enzyme deactivation, filtering obtains fibrous residue and polysaccharide extraction liquid；
Preferably, after the step (3), step (4) is carried out, the process of the step (4) is as follows：The polysaccharide extraction liquid warp
After macroporous absorbent resin, efflux is collected, until without polysaccharide in the efflux；Wherein, the macroporous absorbent resin is non-pole
Property or low pole resin；
More preferably, after the step (4), step (5) is carried out, the process of the step (5) is as follows：The macroporous absorbent resin
It is eluted through the ethanol water that volume fraction is 60%-80%, collects eluent, until the eluent is without flavones reaction
It can.
5. preparation method as claimed in claim 4, which is characterized in that in step (3), the tolerable temperature of the alpha-amylase is
70 DEG C -85 DEG C, pH tolerant 5.0-6.0；Alternatively, the tolerable temperature of the alpha-amylase is 70 DEG C -85 DEG C, pH tolerant is
5.0-6.0 and unit of activity >=13000AAU/g；The temperature of the enzymolysis is 70 DEG C -85 DEG C, and the time of the enzymolysis is 1-3
Hour, the quality of the alpha-amylase is the 0.1%-10% of the quality of the enzymolysis liquid；
And/or in step (4), model D101, AB8, H-60, H103 or XDA-1B of the macroporous absorbent resin is described more
The flow velocity of sugared extracting solution is 1BV/h-3BV/h；
Preferably, in step (4), the efflux obtains refined filtration liquid through secondary filter for the first time；The refined filtration liquid must be received through nanofiltration
Filter trapped fluid；The nanofiltration retentate fluid after nanofiltration is washed, then carries out nanofiltration concentration with water, obtains nanofiltration concentrate；The nanofiltration
Concentrate is after protease hydrolyzed, through secondary filter again to get polysaccharide refined filtration liquid；
Wherein, the secondary filter for the first time uses the aperture of filter membrane to be preferably 0.22 μm -0.45 μm；
Wherein, the molecular cut off of NF membrane is preferably 300-500 used by the nanofiltration and the nanofiltration are washed；
Wherein, the ratio of the volume and the volume of the nanofiltration retentate fluid of nanofiltration washing water used is preferably 2-10
Times；
Wherein, the volume of the nanofiltration concentrate is preferably 2-5 times of the volume of the dendrobium candidum；
Wherein, preferably, the tolerable temperature of the protease is 40 DEG C -60 DEG C, pH tolerant 4.0-6.0；Alternatively, the egg
The tolerable temperature of white enzyme is 40 DEG C -60 DEG C, pH tolerant 4.0-6.0, and unit of activity >=500000HUT/g；The enzymolysis
PH value for 4.0-6.0, the temperature of the enzymolysis is 40 DEG C -60 DEG C, and the time of the enzymolysis is 2-6 hours, the protease
Quality for the nanofiltration concentrate quality 0.05%-2%；
Wherein, the secondary filter again uses the aperture of filter membrane to be preferably 0.22 μm -0.45 μm；
Wherein, preferably, the polysaccharide refined filtration liquid after reduced pressure to get polysaccharide concentrate；More preferably, the polysaccharide concentration
Liquid and ethyl alcohol, the mixed liquor of inorganic salts, it is agitated, precipitation is precipitated, obtains Dendrobium officinale polysaccharide crude product；In the mixed liquor, ethyl alcohol
Mass fraction for 50%-90%, the mass fraction of inorganic salts is 0.5%-5%, and the inorganic salts are sodium chloride and/or acetic acid
Sodium；Further more preferably, the Dendrobium officinale polysaccharide crude product be centrifuged, filter after to get Dendrobium officinale polysaccharide wet product；Institute
Dendrobium officinale polysaccharide wet product is stated after drying to get Dendrobium officinale polysaccharide.
6. preparation method as claimed in claim 4, which is characterized in that in step (5), the body of ethyl alcohol in the ethanol water
Fraction is 70%；
And/or after step (5), by the eluent with after extracting solution merges described in step (1), being obtained through secondary filter smart
Filtrate, then through being concentrated under reduced pressure into no ethyl alcohol, obtain refined filtration concentrate；
Wherein, preferably, the secondary filter uses the aperture of filter membrane as 0.22 μm -0.45 μm；The reduced pressure it is true
Reciprocal of duty cycle is 0.08pa-0.1pa, and the temperature of the reduced pressure is 50 DEG C -70 DEG C；
Wherein, preferably, the refined filtration concentrate is mixed with polyalcohol, preservative and water to get dendrobium candidum polyphenol solution；More
Goodly, the polyalcohol be propylene glycol and/or butanediol, the preservative for Phenoxyethanol, 9010 and one kind in A631 or
It is a variety of；Further more preferably, in the dendrobium candidum polyphenol solution, the mass fraction of dendrobium candidum polyphenol is 1%-10%, institute
The mass fraction for stating polyalcohol is 5%-50%；
Wherein, preferably, the refined filtration concentrate is after drying to get dendrobium candidum polyphenol solid powder.
It is 7. a kind of using the dendrobium candidum fiber powder made from preparation method as claimed in claim 3.
It is 8. a kind of using the Dendrobium officinale polysaccharide made from preparation method as claimed in claim 5.
It is 9. a kind of using the dendrobium candidum polyphenol solution made from preparation method as claimed in claim 6.
It is 10. a kind of using the dendrobium candidum polyphenol solid powder made from preparation method as claimed in claim 6.
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