CN107375361A - Seabuckthorn fruit peel residue, its preparation method and the method for extracting flavones therefrom - Google Patents
Seabuckthorn fruit peel residue, its preparation method and the method for extracting flavones therefrom Download PDFInfo
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- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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Abstract
The present invention relates to the extraction field of Hippophate flavone, it is proposed that a kind of seabuckthorn fruit peel residue and preparation method thereof, preparation method includes：After being freezed by the leftover bits and pieces after the quick-frozen pressure extracting juice of fructus hippophae, be dried in vacuo and crush for the first time, seabuckthorn fruit peel residue powder is obtained, degreasing after seabuckthorn fruit peel residue powder is mixed with petroleum ether.The seabuckthorn fruit peel residue of processing formation is carried out to leftover bits and pieces by way of fructus hippophae is chilled, vacuum drying for the first time, crushing and degreasing, greatly maintain the activity of Hippophate flavone, it is easy to preserve and uses, as raw material, the value of seabuckthorn fruit peel residue is improved, realizes Economic Value Added and the utilization of seabuckthorn fruit peel residue.In addition, extracting the method for flavones in a kind of residue from seabuckthorn fruit peel provided by the invention, it includes：Using above-mentioned seabuckthorn fruit peel residue as raw material, digested successively, extracting and developing purifying and third time be dried in vacuo, provide a new source and approach for Hippophate flavone.
Description
Technical field
The present invention relates to the extraction field of Hippophate flavone, in particular to a kind of seabuckthorn fruit peel residue, its preparation method
And the method for extracting flavones therefrom.
Background technology
Sea-buckthorn (Hippophae rhamnoides Linn.) belongs to Elaeangnaceae in Plant Taxonomy, and Hippophne is planted
Thing, it is a kind of fallen leaves property shrub, its characteristic is drought-enduring, anti-blown sand, can be survived on wetland with saline-alkaline, therefore is widely used in
Water and soil conservation.Bright vinegar willow, acid pierce sub, black thorn to fructus hippophae again, and the province such as Qinghai, Tibet, Inner Mongol, Shanxi is distributed mainly in China
Area.Sea-buckthorn is medicinal and edible plant, and its root, stem, leaf, flower, fruit, particularly sea buckthorn fruit contain abundant nutriment and biology
Active material, it can be widely applied to many fields of the national economy such as food, medicine, light industry, space flight, agriculture and animal husbandry fishery.It is modern
Medical research shows, sea-buckthorn is reducing cholesterol, treatment gastric ulcer, removing interior free yl, anti-aging, relieving cough and reducing sputum, living
Blood, which dissipates the stasis of blood, allevating angina pectoris, preventing and treating coronary atherosclerotic heart disease etc., has the effect of certain.
Contain abundant flavones ingredient in fructus hippophae.Main component through analysis shows Hippophate flavone is Quercetin, different
Rhamnetin, catechin, Kaempferol etc., there is reducing blood lipid, strengthen blood vessel elasticity and improve the functions such as blood circulation.Hippophate flavone,
With safe and nontoxic, pharmacological action outstanding feature, there is huge application potential in food, cosmetic, medicine etc..
In recent years, domestic and foreign scholars have carried out substantial amounts of research work in Hippophate flavone extraction separation.Hippophate flavone carries
The methods of taking including water extraction, organic solvent extraction, ultrasonic extraction, but the above method possesses extraction time length, carried
The shortcoming such as take efficiency low.
The content of the invention
The first object of the present invention is to provide a kind of preparation method of seabuckthorn fruit peel residue, by by fructus hippophae through a system
Column processing forms seabuckthorn fruit peel residue, can be used as raw material, improve the value of seabuckthorn fruit peel residue, realize sea-buckthorn
The Economic Value Added of pericarp residue and utilization.
The second object of the present invention is to provide a kind of seabuckthorn fruit peel residue as made from above-mentioned preparation method, and it is easier
Preserve and put into production, improve the value of seabuckthorn fruit peel residue.
The third object of the present invention can carry in a kind of method that flavones is extracted in residue from seabuckthorn fruit peel is provided, this method
The value of high seabuckthorn fruit peel residue, Economic Value Added and the utilization of seabuckthorn fruit peel residue are realized, carried for the extraction of Hippophate flavone
For a new source and approach.
What embodiments of the invention were realized in：
A kind of preparation method of seabuckthorn fruit peel residue, it includes：Leftover bits and pieces after the quick-frozen pressure extracting juice of fructus hippophae is carried out
Freezing, after being dried in vacuo and crushing for the first time, seabuckthorn fruit peel residue powder is obtained, is taken off after seabuckthorn fruit peel residue powder is mixed with petroleum ether
Fat.
A kind of seabuckthorn fruit peel residue, it is being made by the preparation method of above-mentioned seabuckthorn fruit peel residue.
A kind of method that flavones is extracted in residue from seabuckthorn fruit peel, it includes：It is on the waiting list raw material：With above-mentioned seabuckthorn fruit peel residue
As raw material；Enzymolysis：Biology enzyme and buffer solution are added into seabuckthorn fruit peel residue, and adjusts pH to 4.9~5.4, is digested
Reaction, obtains suspension；Extraction：To suspension add ethanol solution to the volume fraction of the final concentration of ethanol for 60~
70%, 65~70 DEG C are heated to after mixing and carries out microwave radiation exaraction, obtains extract solution；Isolate and purify：By extract solution tree
Fat absorb-elute obtains eluent；And third time is dried in vacuo：By eluent rotary evaporation to without alcohol taste, third time is then carried out
Vacuum drying.
The beneficial effect of the embodiment of the present invention is：
The preparation method of seabuckthorn fruit peel residue provided in an embodiment of the present invention, by the way that fructus hippophae is pressed into extracting juice after quick-frozen
Leftover bits and pieces afterwards carries out deep processing, and leftover bits and pieces is carried out by the way of freezing, for the first time vacuum drying, crushing and degreasing successively
Processing, freezing can keep the composition of leftover bits and pieces not to be destroyed, and the leftover bits and pieces after freezing be carried out into first time vacuum drying, under making
Frozen Cheng Bing moisture directly distils and removed without liquid in heel.Therefore the product after freezing can not only present more
Permeability state and keep original shape, low temperature drying be also prevented from material thermal decomposition.Simultaneously because the thing dried under vacuum
Material eliminates oxidation, therefore dried product, and its physics, chemistry and biological property can be basically unchanged.Subsequent crushing
The specific surface area of seabuckthorn fruit peel residue can be improved, and then lifts the recovery rate of Hippophate flavone, degreasing is finally carried out again, enters one
Step reduces the content of the fat-soluble non-flavonoids impurity in leftover bits and pieces, further improves the recovery rate of Hippophate flavone.Pass through the party
Seabuckthorn fruit peel residue made from method, it is in powdered, its chemical sea-buckthorn Huang for being basically unchanged with biological property, greatly maintaining
The activity of ketone, while be easy to preserve and use, as raw material, the value of seabuckthorn fruit peel residue is improved, is realized husky
The Economic Value Added of spine pericarp residue and utilization.
In addition, in the residue provided in an embodiment of the present invention from seabuckthorn fruit peel extract flavones method, further refined as
What, by the technique of enzymolysis+alcohol extracting+microwave radiation exaraction, cell wall degrading enzyme is drawn using seabuckthorn fruit peel residue extraction flavones
Enter the method for extraction process, there is highly important practice significance in terms of shortening extraction time and improving extraction efficiency height, together
When Hippophate flavone recovery rate be obviously improved, while be equipped with follow-up isolate and purify so that the purity of Hippophate flavone is higher, therewith
Dry and cause Hippophate flavone utilization more easy to maintain and direct, this method can improve the value of seabuckthorn fruit peel residue, realize husky
The Economic Value Added of spine pericarp residue and utilization, a new source and approach are provided for Hippophate flavone.Seabuckthorn fruit peel is residual
Slag is the leftover bits and pieces after the quick-frozen pressure extracting juice of fructus hippophae, and flavones ingredient is extracted from sea-buckthorn leftover bits and pieces, has not only opened up activity
Effective source of composition, while improve the economic value of accessory substance.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition suggested according to normal condition or manufacturer are carried out.Agents useful for same or the unreceipted production firm person of instrument, it is
The conventional products that can be obtained by commercially available purchase.
Below to the seabuckthorn fruit peel residue of the embodiment of the present invention, its preparation method and therefrom extract flavones method enter
Row illustrates.
A kind of preparation method of seabuckthorn fruit peel residue, it includes：Leftover bits and pieces after the quick-frozen pressure extracting juice of fructus hippophae is carried out
Freezing, after being dried in vacuo and crushing for the first time, seabuckthorn fruit peel residue powder is obtained, is taken off after seabuckthorn fruit peel residue powder is mixed with petroleum ether
Fat.Next, will be in case removing heel, preparing seabuckthorn fruit peel residue powder and to seabuckthorn fruit peel residue powder three steps pair of degreasing
The preparation method for the seabuckthorn fruit peel residue that the present embodiment refers to is specifically addressed.
S101. it is on the waiting list leftover bits and pieces
After the quick-frozen pressure extracting juice of fructus hippophae, remaining part is leftover bits and pieces, that is to say the pericarp residue often said, but squeeze the juice
Remaining leftover bits and pieces can not come into operation immediately, because its residue is more, easily rot, not easy to maintain, while directly utilize leftover bits and pieces
Material carries out the extraction of Hippophate flavone, extremely inefficient, therefore, in the present embodiment, will carry out further fine processing to leftover bits and pieces
And processing, the raw material that can be extracted as Hippophate flavone.
It should be noted that term " quick-frozen " refers to forming it into fructus hippophae quick freeze into minimum ice crystal, not sternly
Weight damaging cells tissue, so as to save the Normal juice of fructus hippophae and fragrance, and can preserve the long period.Quick-frozen time and temperature
It can refer to prior art progress.
S102. seabuckthorn fruit peel residue powder is prepared
The leftover bits and pieces obtained after the quick-frozen pressure extracting juice of fructus hippophae is freezed, is dried in vacuo for the first time and crushed successively
Afterwards, seabuckthorn fruit peel residue powder is obtained, wherein, freezing, for the first time vacuum drying and crushing can be according in the prior art to foods
Conventional freezing parameter, for the first time vacuum drying parameter and crush parameter selected.Obtained through inventor's creative experiments
Arrive, leftover bits and pieces is freezed under the conditions of -22 DEG C~-18 DEG C, cooling time is 20~30min, and freezing can keep getting a foothold
The composition of material is not destroyed.Then it is 0.1MPa in vacuum, drying temperature is dried to constant weight under the conditions of being 0~4 DEG C, will
Leftover bits and pieces after freezing carries out first time vacuum drying, and leftover bits and pieces is dried under cryogenic, avoids high temperature to leftover bits and pieces
The destruction of composition, greatly remain the active ingredient i.e. activity of Hippophate flavone in leftover bits and pieces.Then crushed, be crushed to
40~80 mesh obtain seabuckthorn fruit peel residue powder.The specific surface area of seabuckthorn fruit peel residue can be improved by crushing, and then lift Hippophate flavone
Recovery rate.
S103. to seabuckthorn fruit peel residue powder degreasing
Seabuckthorn fruit peel residue powder is pressed into solid-liquid ratio 1:3~1:5 mix with petroleum ether, and petroleum ether can dissolve as degreasing agent
Fat-soluble non-flavonoids impurity, 1:3~1:5 solid-liquid ratio is advantageous to petroleum ether by the fat-soluble non-Huang in seabuckthorn fruit peel residue powder
Ketone impurity fully dissolves, and improves the recovery rate of Hippophate flavone.Then after 50~70 DEG C of 1~2h of agitating and heating, 20~60 are crossed
Mesh silk, obtains filtrate.The agitating and heating under conditions of 50~70 DEG C, further lift the fat-soluble non-flavonoids of petroleum ether dissolution
The amount of impurity.Then filtrate is freezed under the conditions of -22 DEG C~-18 DEG C, then carries out second and be dried in vacuo.By filtrate
Second of vacuum drying is carried out after freezing again, in other words, first filtrate is freezed, then vacuumized, make in material it is frozen into
The moisture of ice directly distils and removed without liquid.Therefore the product after freezing not only can be presented porous state and keep
Shape originally, it is set easily to be restored to the original state after adding water, and low temperature drying is also prevented from material thermal decomposition.Simultaneously because vacuum
The material of lower drying eliminates oxidation, therefore dried product, and its physics, chemistry and biological property can be basically unchanged.
In a preferred embodiment of the invention, second vacuum drying parameter is that vacuum is 0.1MPa, drying temperature
To dry to constant weight under the conditions of 0~4 DEG C." S102. prepares seabuckthorn fruit peel residue to second of vacuum drying parameter herein with step
First time vacuum drying parameter in powder " is identical, using being dried in vacuo twice, can dramatically retain seabuckthorn fruit peel residue
The activity of middle Hippophate flavone, be advantageous to the extraction of follow-up Hippophate flavone.
Fructus hippophae is changed into seabuckthorn fruit peel residue after above three step process, its can as extraction flavones raw material,
The value of seabuckthorn fruit peel residue is improved, realizes Economic Value Added and the utilization of seabuckthorn fruit peel residue, is the extraction of Hippophate flavone
One new source and approach are provided.
In addition, the embodiment of the present invention additionally provides a kind of obtained sea-buckthorn of the preparation method by above-mentioned seabuckthorn fruit peel residue
Pericarp residue, the seabuckthorn fruit peel residue not only can be as the raw materials of extraction Hippophate flavone isoreactivity material, while can be with
As food auxiliary material, contain substantial amounts of dietary fiber in seabuckthorn fruit peel residue, to non-biographies such as prevention cardiovascular and cerebrovascular disease, diabetes
Dye chronic disease has the effect of certain.
The present embodiment will specifically be specifically described seabuckthorn fruit peel residue and be used as the application of the raw material of extraction Hippophate flavone and specific
Extracting method, to seabuckthorn fruit peel residue as food auxiliary material, it is not specifically described here.
A kind of method that flavones is extracted in residue from seabuckthorn fruit peel, it includes：
S100. it is on the waiting list raw material
Raw material is used as using the above-mentioned seabuckthorn fruit peel residue referred to；Signified seabuckthorn fruit peel residue can be according to above-mentioned herein
Preparation method is directly prepared or is prepared as described above being commercially available by commercially available after prepared by method by other producers.
S200. digest
Biology enzyme and buffer solution are added into seabuckthorn fruit peel residue, and adjusts pH to 4.9~5.4, enzyme digestion reaction is carried out, obtains
Suspension.
Specifically, in terms of the quality of seabuckthorn fruit peel residue, the addition of biology enzyme is 0.4~1.0mg/g, and the biology enzyme can
With selected from least one of cellulase and pectase.Pectase can make intercellular pectic substance degrade, cell from group
Knit interior separation.Cellulase can degraded cellulose, it is not monomeric enzyme, but rise synergy multicomponent enzyme system, be one
Kind complex enzyme, is mainly made up of exoglucanase, endoglucanase and glucuroide etc..In the present embodiment, with fiber
At least one of plain enzyme and pectase are added in seabuckthorn fruit peel residue as biology enzyme, are advantageous to improve seabuckthorn fruit peel residue
The dissolving of cell membrane, so that the Hippophate flavone in seabuckthorn fruit peel residue is more dissolved out.Be advantageous to improve Hippophate flavone
Recovery rate.
When biology enzyme selects cellulase and pectase simultaneously, the mass ratio of cellulase and pectase is 1:1.At this
In the preferred embodiment of invention, biology enzyme is selected from one of cellulase and pectase, and is selected from cellulase, in the present invention
Most preferred embodiment in, select cellulase in endoglucanase as biology enzyme.When biology enzyme is selected from inscribe Portugal
During dextranase, the addition of biology enzyme is preferably 0.4~0.8mg/g.
Endoglucanase mainly acts on the noncrystalline domain of cellulose, random hydrolysis β-Isosorbide-5-Nitrae-glycosidic bond, by long-chain
Cellulose truncates, and the overall degraded to cellulose plays an important role.So using the method for genetic engineering, gathered by inscribe Portugal
Carbohydrase acts synergistically with the compounding of exoglucanase or the sweet enzyme of glucan, and can effectively degrade avicel cellulose.
Buffer solution can ensure the ionic environment and pH value needed for enzyme, and strong acid and strong base can make it lose activity, therefore need
Buffer solution is added, is made in certain Ph values, keeps the activity of enzyme.The suitable pH of the biology enzyme selected in the present embodiment exists
In acid range, generally 4~5.Therefore, in the present embodiment, the pH of the buffer solution of selection is also in acid range, it is preferable that
One or more of the buffer solution in acetic acid-ammonium acetate buffer, phosphate buffer and Acetic acid-sodium acetate buffer solution, more
Preferably, buffer solution is selected from Acetic acid-sodium acetate buffer solution.
In the present embodiment, the solid-liquid ratio of the addition of seabuckthorn fruit peel residue and buffer solution is 1:6~1:8；Preferably 1:7.
1 is found through the research of inventor's creative experiments:7 solid-liquid ratio can keep the activity of enzyme to greatest extent, obtain enzyme digestion reaction
To be smoothed out.
The parameter of enzymolysis includes：Hydrolysis temperature is 40~45 DEG C, and enzymolysis time is 30~60min.Inventor is through creativeness
The above-mentioned enzymolysis parameter that work is chosen is advantageous to keep the activity of biology enzyme, while is advantageous to the efficiency of lifting enzymolysis.
S300. extract
Ethanol solution is added in the suspension obtained into step " S200. enzymolysis " to the volume of the final concentration of ethanol
Fraction is 60~70%, and 65~70 DEG C are heated to after mixing and carries out microwave radiation exaraction, obtains extract solution.
It in power is 200~270W that microwave radiation exaraction, which is, processing time be 15~20min under conditions of carry out.
In the present embodiment, extracted by the way of " enzymolysis+alcohol extracting+microwave radiation exaraction ", will first with biology enzyme
The cell wall degradation of seabuckthorn fruit peel residue, be advantageous to be lifted the dissolution rate of the active ingredient of seabuckthorn fruit peel residue, then utilize nothing
Hydrous ethanol solution is extracted, and assisted microwave synthesis extracts, and is had compared to single alcohol extracting or microwave radiation exaraction and is significantly improved
The effect of Hippophate flavone output capacity.
S400. isolate and purify
Extract solution progress adsorption and desorption by resin is obtained into eluent.
Specifically, first extract solution is filtered through filter paper, is then then added to X-5 type resin columns, utilize 10~15 times of cylinders
The ethanol solution that long-pending volume fraction is 95% elutes, and collects eluent.
S500. third time is dried in vacuo
By eluent rotary evaporation to without alcohol taste, third time vacuum drying is then carried out.
Specifically, eluent is in 45~50 DEG C of water-baths, and 80~100 turns/min, vacuum is under the conditions of 0.07~0.09MPa
Then rotary evaporation carries out third time vacuum drying under 0.08~0.1MPa of vacuum, temperature 50 C and produced to without alcohol taste
Product, gained powder are Hippophate flavone.
With reference to embodiment, the present invention is described in further detail, but is not restricted to present disclosure.
Embodiment 1
A kind of preparation method of seabuckthorn fruit peel residue, it includes：By the leftover bits and pieces after the quick-frozen pressure extracting juice of fructus hippophae in -22
DEG C freezed；Then first time vacuum drying is carried out, vacuum drying parameter is for the first time：Vacuum is 0.08MPa, is dried
Temperature is 4 DEG C and dried to constant weight, then takes the dried leftover bits and pieces of 1000g to be crushed to 40 mesh and obtains seabuckthorn fruit peel residue powder, standby
With.Then 5000ml petroleum ethers are added in first seabuckthorn fruit peel residue powder and are mixed, after 60 DEG C of agitating and heating 1h, cross 20 mesh thin,tough silk
Cloth, gained filtrate are freezed at -20 DEG C, then carry out depressurizing second of vacuum drying.The ginseng that second of reduced vacuum is dried
Number is：Vacuum：0.08MPa, 4 DEG C of drying temperature, dry to constant weight and terminate.Gained solid is seabuckthorn fruit peel residue.
Embodiment 2
A kind of preparation method of seabuckthorn fruit peel residue, it includes：By the leftover bits and pieces after the quick-frozen pressure extracting juice of fructus hippophae in -20
DEG C freezed；Then first time vacuum drying is carried out, vacuum drying parameter is for the first time：Vacuum is 0.1MPa, is dried
Temperature is 2 DEG C and dried to constant weight, then takes the dried leftover bits and pieces of 1000g to be crushed to 80 mesh and obtains seabuckthorn fruit peel residue powder, standby
With.Then 4000ml petroleum ethers are added in first seabuckthorn fruit peel residue powder and are mixed, after 60 DEG C of agitating and heating 1h, cross 40 mesh thin,tough silk
Cloth, gained filtrate are freezed at -20 DEG C, are then carried out second and are dried in vacuo.The parameter that second reduced vacuum is dried is：
Vacuum：0.1MPa, 2 DEG C of drying temperature, dry to constant weight and terminate.Gained solid is seabuckthorn fruit peel residue.
Embodiment 3
A kind of preparation method of seabuckthorn fruit peel residue, it includes：By the leftover bits and pieces after the quick-frozen pressure extracting juice of fructus hippophae in -18
DEG C freezed；Then first time vacuum drying is carried out, vacuum drying parameter is for the first time：Vacuum is 0.1MPa, is dried
Temperature is 0 DEG C and dried to constant weight, then takes the dried leftover bits and pieces of 1000g to be crushed to 60 mesh and obtains seabuckthorn fruit peel residue powder, standby
With.Then 3000ml petroleum ethers are added in first seabuckthorn fruit peel residue powder and are mixed, after 60 DEG C of agitating and heating 1h, cross 60 mesh thin,tough silk
Cloth, gained filtrate are freezed at -18 DEG C, are then carried out second and are dried in vacuo.Vacuum drying parameter is for the second time：Vacuum
Degree：0.1MPa, 0 DEG C of drying temperature, dry to constant weight and terminate.Gained solid is seabuckthorn fruit peel residue.
Embodiment 4~6
Embodiment 4 provides a kind of seabuckthorn fruit peel residue, and it is the preparation side of the seabuckthorn fruit peel residue provided by embodiment 1
Method is prepared；Embodiment 5 provides a kind of seabuckthorn fruit peel residue, and it is the system of the seabuckthorn fruit peel residue provided by embodiment 2
Preparation Method is prepared；Embodiment 6 provides a kind of seabuckthorn fruit peel residue, and it is the seabuckthorn fruit peel residue provided by embodiment 3
Preparation method be prepared.
Embodiment 7
A kind of method that flavones is extracted in residue from seabuckthorn fruit peel, it includes：The seabuckthorn fruit peel residue provided with embodiment 4
As raw material, 0.7g cellulases are added into 1000g seabuckthorn fruit peel residues, add Acetic acid-sodium acetate buffer solution adjust pH to
5.0, hydrolysis temperature is 42 DEG C, enzymolysis time 40min, carries out enzyme digestion reaction, obtains suspension；Added into suspension
2300mL ethanol solutions cause final concentration of 60% (volume fraction) of ethanol, are heated to 65 DEG C after well mixed and carry out
Microwave radiation exaraction, obtain extract solution.The condition of microwave radiation exaraction is：Power 270W, processing time be：18min；Will extraction
Liquid filters, and filtrate crosses X-5 type resin columns, is eluted using the ethanol solution of 1000mL 95% (volume fraction), collects eluent；
By eluent in 45 DEG C of water-baths, 100 turns/min, rotary evaporation is extremely without alcohol taste under the conditions of vacuum is 0.07MPa, then in vacuum
0.08MPa is spent, third time vacuum drying is carried out under temperature 50 C and obtains the general flavone 8.90g of seabuckthorn fruit peel residue, in general flavone
The content of anthocyanidin is 50.2%.
Embodiment 8
A kind of method that flavones is extracted in residue from seabuckthorn fruit peel, it includes：The seabuckthorn fruit peel residue provided with embodiment 5
As raw material, 0.4g endoglucanases are added into 1000g seabuckthorn fruit peel residues, add the regulation of Acetic acid-sodium acetate buffer solution
PH to 5.4, hydrolysis temperature are 45 DEG C, enzymolysis time 30min, carry out enzyme digestion reaction, obtain suspension；Added into suspension
2350mL ethanol solutions cause final concentration of 70% (volume fraction) of ethanol, are heated to 70 DEG C after well mixed and carry out
Microwave radiation exaraction, obtain extract solution.The condition of microwave radiation exaraction is：Power 250W, processing time be：15min；Will extraction
Liquid filters, and filtrate crosses X-5 type resin columns, is eluted using the ethanol solution of 1000mL 95% (volume fraction), collects eluent；
By eluent in 48 DEG C of water-baths, 100 turns/min, rotary evaporation is extremely without alcohol taste under the conditions of vacuum is 0.08MPa, then in vacuum
0.1MPa is spent, third time vacuum drying is carried out under temperature 50 C and obtains the general flavone 9.10g in seabuckthorn fruit peel residue, in general flavone
Anthocyanidin content is 50.5%.
Embodiment 9
A kind of method that flavones is extracted in residue from seabuckthorn fruit peel, it includes：The seabuckthorn fruit peel residue provided with embodiment 5
As raw material, 1.0g endoglucanases are added into 1000g seabuckthorn fruit peel residues, add the regulation of Acetic acid-sodium acetate buffer solution
PH to 5.4, hydrolysis temperature are 40 DEG C, enzymolysis time 60min, carry out enzyme digestion reaction, obtain suspension；Added into suspension
2350mL ethanol solutions, now, the volume fraction of the final concentration of ethanol for 70% it is well mixed after carry out Microwave-assisted Extraction
Take, obtain extract solution.The condition of microwave radiation exaraction is：Power 200W, processing time be：20min；Extract solution is filtered, filtered
Liquid crosses X-5 type resin columns, is eluted using the ethanol solution of 1000mL 95% (volume fraction), collects eluent；By eluent
In 50 DEG C of water-baths, 100 turns/min, rotary evaporation is extremely without alcohol taste under the conditions of vacuum is 0.09MPa, then in vacuum
0.1MPa, third time vacuum drying is carried out under temperature 50 C and obtains the general flavone 9.15g in seabuckthorn fruit peel residue, the flower of general flavone
Blue or green cellulose content is 51.5%.
Embodiment 10
The present embodiment and the method that flavones is extracted from seabuckthorn fruit peel residue that embodiment 9 provides are essentially identical, distinctive points
It is：In embodiment 9, biology enzyme selects endoglucanase；Buffer solution is selected from Acetic acid-sodium acetate buffer solution.And the present embodiment
In, biology enzyme is 1 from mass ratio:1 cellulase and pectase, buffer solution are selected from acetic acid-ammonium acetate buffer, phosphoric acid
Salt buffer and Acetic acid-sodium acetate buffer solution.
Embodiment 11
The present embodiment and the method that flavones is extracted from seabuckthorn fruit peel residue that embodiment 9 provides are essentially identical, distinctive points
It is：In embodiment 9, biology enzyme selects endoglucanase；Buffer solution is selected from Acetic acid-sodium acetate buffer solution.And the present embodiment
In, biology enzyme selects pectase, and buffer solution is selected from acetic acid-ammonium acetate buffer and phosphate buffer.
Comparative example
Firstth, the selection that obtains seabuckthorn fruit peel residue is handled leftover bits and pieces with Different treatments
Seabuckthorn fruit peel residue is handled using six kinds of different processing modes, the fructus hippophae then obtained with Different treatments
Skin residue is respectively as raw material, and the extracting mode provided with embodiment 7 is extracted, and finally calculates Different treatments and obtains
Seabuckthorn fruit peel residue extract in the same manner after the extraction yield of flavones and the content of anthocyanidin.
Wherein, six kinds of different processing mode difference are as follows：
Comparative example 1：Leftover bits and pieces after fructus hippophae is squeezed the juice under normal temperature is directly as raw material；
Comparative example 2：By the leftover bits and pieces after the quick-frozen pressure extracting juice of fructus hippophae directly as raw material；
Comparative example 3：Using fructus hippophae it is quick-frozen pressure extracting juice after leftover bits and pieces drying after as raw material；
Comparative example 4：Leftover bits and pieces after the quick-frozen extracting juice of fructus hippophae is vacuum dried rear as raw material；
Comparative example 5：Using the leftover bits and pieces after the quick-frozen extracting juice of fructus hippophae it is chilled, vacuum drying after as raw material；
Test example 1：By the leftover bits and pieces after the quick-frozen extracting juice of fructus hippophae it is chilled, vacuum drying, crush and degreasing after, as
Raw material.
Obtained seabuckthorn fruit peel residue after the processing mode processing different using above-mentioned six kinds is as raw material with identical side
Method is extracted, and the extracting flavonoids yield of acquisition and the result of anthocyanidin recovery rate refer to table 1.
Influence of the seabuckthorn fruit peel residue that the Different treatments of table 1. obtain to yield
Conclusion：From comparative example 1 and comparative example 2 as can be seen that leftover bits and pieces squeezes fruit compared to normal temperature after quick-frozen squeezing juice
The activity for remaining active ingredient flavones of leftover bits and pieces after juice, be advantageous to improve extraction efficiency and anthocyanidin and the extraction of flavones
Yield.The form that high temperature is dried it can be seen from comparative example 3 and comparative example 4, which is dried, greatly to be destroyed in leftover bits and pieces
The activity of active ingredient flavones, and be dried in vacuo leftover bits and pieces is dried under cryogenic, avoid high temperature to leftover bits and pieces into
The destruction divided, causes the extracting flavonoids yield of comparative example 3 and comparative example 4 and the extraction efficiency of anthocyanidin to have marked difference.This
Outside, the specific surface area of seabuckthorn fruit peel residue can be improved by being crushed it can be seen from comparative example 5 and test example 1, so as to lift flavones
With the extraction efficiency of anthocyanidin.
Secondth, the selection of different extracting modes
The extracting mode of Fructus Hippophae polysaccharide have it is a variety of, such as：In alcohol extracting, ultrasonic wave extraction, Microwave Extraction, and the present embodiment
" enzymolysis+alcohol extracting+microwave radiation exaraction " provided, in the contrast experiment, the seabuckthorn fruit peel residue that is provided from embodiment 2
Seabuckthorn fruit peel residue made from preparation method is extracted, in the raw material according to above-mentioned four kinds of extracting methods respectively as raw material
The content of Fructus Hippophae polysaccharide is 11.5mg/g, and the recovery rate of Hippophate flavone is calculated according to below equation：
Hippophate flavone content in recovery rate=extracted amount/seabuckthorn fruit peel residue.
It should be noted that in following extraction processes, NM part, prior art can refer to.
Ethanol extracts：Seabuckthorn fruit peel residue addition ethanol is extracted, shaker water bath extraction 2h, to the filtrate after extraction
It is freeze-dried to obtain Hippophate flavone.
Ultrasonic wave extraction：By seabuckthorn fruit peel residue, after addition ethanol stirs, it is placed in ultrasonic wave and extracts 6min, shake
Bed water-bath extracts 2h, freeze-dried to the filtrate after extraction to obtain Hippophate flavone.
Microwave Extraction：After seabuckthorn fruit peel residue addition ethanol is stirred, it is placed in microwave and extracts 6min, shaker water bath
2h is extracted, it is freeze-dried to the filtrate after extraction to obtain Hippophate flavone.
Enzymolysis+alcohol extracting+microwave radiation exaraction：Extracted respectively in a manner of 7~embodiment of embodiment 9 provides.
Experimental result is with reference to table 2 below：
The influence of the extracting flavonoids rate of 2. different extracting modes of table
| Extracting method | Raw material dosage (g) | Extracting flavonoids amount (mg) | Extracting flavonoids rate (%) |
| Ethanol extracts | 1000 | 5.18 | 45.0 |
| Ultrasonic wave extraction | 1000 | 4.15 | 36.1 |
| Microwave Extraction | 1000 | 5.36 | 46.6 |
| Embodiment 7 | 1000 | 8.90 | 77.4 |
| Embodiment 8 | 1000 | 9.10 | 79.1 |
| Embodiment 9 | 1000 | 9.15 | 79.6 |
It can be seen from comparative example, using the extraction process of seeweed polyphenol provided in an embodiment of the present invention, sand can be significantly improved
The recovery rate of spine flavones.
In summary, the preparation method of seabuckthorn fruit peel residue provided in an embodiment of the present invention, by by fructus hippophae through quick-frozen
Afterwards press extracting juice after leftover bits and pieces carry out deep processing, successively using freezing, for the first time vacuum drying, crushing and degreasing by the way of pair
Leftover bits and pieces is handled, and freezing can keep the composition of leftover bits and pieces not to be destroyed, and the leftover bits and pieces after freezing is carried out true for the first time
Sky is dried, and the moisture of frozen Cheng Bing in leftover bits and pieces is directly distilled and is removed without liquid.Therefore the product after freezing is not
But porous state can be presented and keep original shape, low temperature drying is also prevented from material thermal decomposition.It is simultaneously because true
The lower dry material of sky eliminates oxidation, therefore dried product, and its physics, chemistry and biological property can substantially not
Become.Subsequent crushing can improve the specific surface area of seabuckthorn fruit peel residue, and then lift the recovery rate of Hippophate flavone, again finally
Degreasing is carried out, the content of the fat-soluble non-flavonoids impurity in leftover bits and pieces is further reduced, further improves carrying for Hippophate flavone
Take rate.By seabuckthorn fruit peel residue made from this method, it is in powdered, and its chemistry and biological property are basically unchanged, greatly
The activity of the Hippophate flavone maintained, while be easy to preserve and use, as raw material, improve the profit of seabuckthorn fruit peel residue
With value, Economic Value Added and the utilization of seabuckthorn fruit peel residue are realized.
In addition, in the residue provided in an embodiment of the present invention from seabuckthorn fruit peel extract flavones method, further refined as
What, by the technique of enzymolysis+alcohol extracting+microwave radiation exaraction, cell wall degrading enzyme is drawn using seabuckthorn fruit peel residue extraction flavones
Enter the method for extraction process, there is highly important practice significance in terms of shortening extraction time and improving extraction efficiency height, together
When Hippophate flavone recovery rate be obviously improved, while be equipped with follow-up isolate and purify so that the purity of Hippophate flavone is higher, therewith
Dry and cause Hippophate flavone utilization more easy to maintain and direct, this method can improve the value of seabuckthorn fruit peel residue, realize husky
The Economic Value Added of spine pericarp residue and utilization, a new source and approach are provided for Hippophate flavone.Seabuckthorn fruit peel is residual
Slag is the leftover bits and pieces after the quick-frozen pressure extracting juice of fructus hippophae, and flavones ingredient is extracted from sea-buckthorn leftover bits and pieces, has not only opened up activity
Effective source of composition, while improve the economic value of accessory substance.
Embodiments described above is part of the embodiment of the present invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of preparation method of seabuckthorn fruit peel residue, it is characterised in that it includes：Under after the quick-frozen pressure extracting juice of fructus hippophae
Heel is freezed, first time is dried in vacuo and after crushing, seabuckthorn fruit peel residue powder is obtained, by the seabuckthorn fruit peel residue powder and stone
Degreasing after oily ether mixing.
2. the preparation method of seabuckthorn fruit peel residue according to claim 1, it is characterised in that freeze the leftover bits and pieces bag
Include：The leftover bits and pieces is freezed under the conditions of -22 DEG C~-18 DEG C, cooling time is 20~30min.
3. the preparation method of seabuckthorn fruit peel residue according to claim 1, it is characterised in that for the first time described in vacuum drying
Leftover bits and pieces includes：In vacuum it is 0.08~0.1MPa by the leftover bits and pieces after cooling, under the conditions of drying temperature is 0~4 DEG C
It is dried to constant weight.
4. the preparation method of seabuckthorn fruit peel residue according to claim 1, it is characterised in that seabuckthorn fruit peel is residual described in degreasing
Ground-slag includes：The seabuckthorn fruit peel residue powder is pressed into solid-liquid ratio 1:3~1:5 mix with the petroleum ether, in 50~70 DEG C of stirrings
After heating 1~2h, 20~60 mesh silks are crossed, filtrate is obtained, the filtrate is freezed under the conditions of -22 DEG C~-18 DEG C, so
Second it is dried in vacuo afterwards, wherein, second of vacuum drying parameter is that vacuum is 0.08~0.1MPa, drying temperature 0
Dried under the conditions of~4 DEG C to constant weight.
5. a kind of seabuckthorn fruit peel residue, it is characterised in that it is residual as the seabuckthorn fruit peel as described in any one of Claims 1 to 4
The preparation method of slag is made.
6. the method for flavones is extracted in a kind of residue from seabuckthorn fruit peel, it is characterised in that it includes：
It is on the waiting list raw material：Raw material is used as using the seabuckthorn fruit peel residue described in claim 5；
Enzymolysis：Biology enzyme and buffer solution are added into the seabuckthorn fruit peel residue, and adjusts pH to 4.9~5.4, digest instead
Should, obtain suspension；
Extraction：The volume fraction that ethanol solution to the final concentration of ethanol are added to the suspension is 60~70%, is mixed
After be heated to 65~70 DEG C and carry out microwave radiation exaraction, obtain extract solution；
Isolate and purify：Extract solution progress adsorption and desorption by resin is obtained into eluent；And
Third time is dried in vacuo：By the eluent rotary evaporation to without alcohol taste, third time vacuum drying is then carried out.
7. the method for flavones is extracted in the residue according to claim 6 from seabuckthorn fruit peel, it is characterised in that digest the sand
The hydrolysis temperature of spine pericarp residue is 40~45 DEG C, and enzymolysis time is 30~60min.
8. the method for flavones is extracted in the residue according to claim 6 from seabuckthorn fruit peel, it is characterised in that with the sea-buckthorn
The quality meter of pericarp residue, the addition of the biology enzyme is 0.4~1.0mg/g, and the biology enzyme is selected from cellulase and fruit
At least one of glue enzyme, it is preferable that the biology enzyme is selected from cellulase, it is highly preferred that the biology enzyme is selected from inscribe Portugal
Dextranase.
9. the method for flavones is extracted in the residue according to claim 6 from seabuckthorn fruit peel, it is characterised in that the fructus hippophae
Skin residue and the solid-liquid ratio of the addition of the buffer solution are 1:6~1:8；Preferably, the buffer solution is selected from acetic acid-acetic acid
One or more in ammonium buffer solution, phosphate buffer and Acetic acid-sodium acetate buffer solution, it is highly preferred that the buffer solution selects
From Acetic acid-sodium acetate buffer solution.
10. the method for flavones is extracted in the residue according to claim 6 from seabuckthorn fruit peel, it is characterised in that microwave radiation technology
It in power is 200~270W that extraction, which is, processing time be 15~20min under conditions of carry out.
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