CN107298863A - The supersonically preparation method of peanut protein polysaccharide composite particle and functional food application - Google Patents
The supersonically preparation method of peanut protein polysaccharide composite particle and functional food application Download PDFInfo
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- CN107298863A CN107298863A CN201710411556.3A CN201710411556A CN107298863A CN 107298863 A CN107298863 A CN 107298863A CN 201710411556 A CN201710411556 A CN 201710411556A CN 107298863 A CN107298863 A CN 107298863A
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- Prior art keywords
- peanut protein
- carragheen
- frequency
- solution
- composite particles
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- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 111
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- 229920001282 polysaccharide Polymers 0.000 title abstract description 16
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- 239000012153 distilled water Substances 0.000 claims description 17
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- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 claims description 13
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
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- ZNOZWUKQPJXOIG-XSBHQQIPSA-L [(2r,3s,4r,5r,6s)-6-[[(1r,3s,4r,5r,8s)-3,4-dihydroxy-2,6-dioxabicyclo[3.2.1]octan-8-yl]oxy]-4-[[(1r,3r,4r,5r,8s)-8-[(2s,3r,4r,5r,6r)-3,4-dihydroxy-6-(hydroxymethyl)-5-sulfonatooxyoxan-2-yl]oxy-4-hydroxy-2,6-dioxabicyclo[3.2.1]octan-3-yl]oxy]-5-hydroxy-2-( Chemical compound O[C@@H]1[C@@H](O)[C@@H](OS([O-])(=O)=O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H]2OC[C@H]1O[C@H](O[C@H]1[C@H]([C@@H](CO)O[C@@H](O[C@@H]3[C@@H]4OC[C@H]3O[C@H](O)[C@@H]4O)[C@@H]1O)OS([O-])(=O)=O)[C@@H]2O ZNOZWUKQPJXOIG-XSBHQQIPSA-L 0.000 description 1
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Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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- A23L33/185—Vegetable proteins
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- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
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- A61K9/5052—Proteins, e.g. albumin
-
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Abstract
The invention discloses the supersonically preparation method of peanut protein polysaccharide composite particle and functional food application, it is related to functional food microcapsules technology field.It is to be prepared from by the raw material of following parts by weight：Peanut protein：1~10 part；Carragheen：1~15 part.The present invention adds carragheen into peanut protein, change the higher structure of peanut protein, open its structure, exposure active group, protein and polysaccharide form small aggregation simultaneously, so as to promote each aggregation to provide basis by hydrophobic interaction formation composite particles for embedding bioactive ingredients.The present invention is during using peanut protein carragheen composite particles embedding Tea Polyphenols, use frequency sweep ultrasonic ripple treatment technology or multi-mode ultrasonic technology, protein is promoted by the physical force of ultrasonic wave and polysaccharide is cross-linked into aggregation, so as to promote each aggregation by hydrophobic interaction formation composite particles, basis is provided for embedding bioactive ingredients.
Description
Technical field
The present invention relates to protein-polysaccharide composite particles preparing technical field, one kind is refered in particular to peanut protein and carragheen
Handled for raw material, using frequency sweep ultrasonic or multi-mode frequency ultrasonic wave treatment technology prepares composite particles and Tea Polyphenols is carried out
The method that embedding prepares functional food.
Background technology
Functional food because containing the bioactive ingredients such as vitamin, unrighted acid, polyphenol compound or probiotics,
Function with regulation human physiological functions, can delay the generation with preventing chronic disease.However, many active components are to food
Product process and storage in the factor such as temperature, oxygen, light, pH and metal ion it is sensitive, it is prone to aoxidize, isomerization, aggregation
Or degraded etc. structural change, cause bioactivity reduce or lose.Moreover, hydrophobicity and amphipathic active component dissolve in water
Degree is very low.These greatly limit application of the active component in food and medicine industry.Natural biology is big
Molecule (such as protein, polysaccharide) not only has high nutritive value, and with a variety of functional characteristics, has been widely used as bag
Bury the raw material in technology.Therefore, the composite particles system of exploitation natural macromolecular (protein and polysaccharide) is to bioactive ingredients
Embedded and protected, be the key for developing functional food and medicine.
Peanut is one of four big oil crops in the world, mainly for the production of peanut oil, and in the mistake of production peanut oil
Cheng Zhonghui produces substantial amounts of accessory substance --- peanut meal.In China, peanut meal is mainly used as producing the raw material of animal feed, should
It is relatively low with being worth.Protein content in peanut meal is about 45%-50%, is not develop and useedd sufficiently.Peanut egg
White content is the 24%-36% of total material composition in peanut, is the fifth-largest plant protein resource in the world.Peanut protein belongs to
In reserve protein, its isoelectric point, according to its dissolution degree in water, can be divided into water-solubility protein in pH4.5 or so, i.e., newborn
Albumin (content about 10%) and salting-in protein (content about 90%) two classes.Salt soluble protein is main by ground-peanut ball in peanut
Content ratio between albumen, conarachin I and conarachin II compositions, three is 73:21:6, it is peanut protein
In main protein fragments, account for the 75% of all protein.Containing abundant amino acid in peanut protein, wherein ammonia needed by human
Up to 8 kinds of base acid, not only rationally, content is also close to standard as defined in FAO for ratio.Result of study shows that peanut protein is in human body
It is interior have high digestibility, up to 90%, easily by human consumption's suctionization.Peanut protein is used as a kind of plant best in quality
Thing albumen source, with being of high nutritive value, cost is low, wide material sources the features such as, become embedding bioactive ingredients technology
In preferred feedstock.
Carragheen (carrageenan), is the hydrophilic polysaccharide extracted from red algae cell membrane, and different type carragheen has
Common backbone structure, respectively has feature.Skeleton structure by β-(1,3)-D- galactolipins and α-(1,4)-D- galactolipins or α-(1-4)-
3,6- inner ether-D- galactolipins are alternately connected, sulfuric acid ester sodium, potassium, calcium, the anionic linear polysaccharide of ammonium salt of composition.According to half
In lactose base whether the difference containing inner ether, the quantity of sulfate group and link position, carragheen be divided into κ-, ι-, μ-, ν-,
λ-, θ-, ε-, ω-etc. polytype, wherein ω-be a kind of new carragheen.Common carragheen be κ-, ι-and λ-type, preferable bar
Under part, in double disaccharide units that they are repeated, respectively containing one, two, three sulfate groups, it can be extrapolated and occupy quality
Than in respectively sugar unit, respectively containing one, two, three sulfate groups, it is respectively 20% that can extrapolate it to occupy mass ratio,
33% and 41%.By carragheen and the other oroteins such as compounding use such as soybean protein, casein, gelatin, with cooperative effect,
Significantly improve viscoelastic property, and adjustment and control system microstructure.
Research finds that the interphase interaction formation composite particles of protein and polysaccharide can overcome one-component pH sensitive, steady
Bioactive ingredients are played embedding and protective effect well by the low deficiency of qualitative poor, embedding efficiency.Therefore domestic and foreign scholars
The substantial amounts of preparation method about protein-polysaccharide composite particles and its research embedded to bioactive ingredients are carried out.Breast
Change method is the common method for preparing composite particles, and the deficiency of this method, which is shown, needs addition organic in the preparation process of composite particles
Solvent, surfactant, glutaraldehyde cross-linking agent etc., the residual of these reagents make composite particles have certain toxicity；Remove solvent method
The introducing of toxic cross-linking agents is directed to chemical crosslink technique；Three of the above method is not the Perfected process for preparing composite particles.From
Sub- cross-linking method and self-assembly method prepare composite particles, mild condition, it is not necessary to poisonous crosslinking agent, and chemical combination key is not generated, only according to
By non-covalent bond connection, thus it is widely used.Particularly self-assembly method, for nutrient delivery system design, security
Deng relatively more preferably.But protein and polysaccharide are two kinds of macromoleculars of different nature after all, are entered only by simple self-assembly method
Row cohesion, flocculating result is poor, and condensation product is low to the embedding efficiency of bioactive ingredients.
In order to solve this problem, the present invention introduces advanced frequency sweep type ultrasonic processing and multi-mode ultrasonication skill
Art, it is desirable to which two kinds of biological macromolecule solns of ultrasonic wave energy elicitor protein matter and polysaccharide produce what is matched with its own intrinsic frequency
Resonant frequency, produces crosslinking, obtains a kind of high embedding efficiency, pH stabilizations, the protein-polysaccharide composite particles of uniform particle diameter,
Bioactive ingredients are embedded and protected using the protein-polysaccharide composite particles of gained.
The content of the invention
To solve the above problems, the present invention adds Tea Polyphenols, profit by carrying out complex coacervation to peanut protein-carragheen
Peanut protein-carragheen composite particles are prepared with the technological means such as frequency sweep type ultrasonic and multi-mode ultrasonication, and are studied
Its embedding effect to Tea Polyphenols.
Peanut protein of the present invention-carragheen composite particles, is prepared from by the raw material of following parts by weight：
Peanut protein：1~10 part；
Carragheen：1~15 part.
It is preferred that the raw material of following parts by weight is prepared from：
Peanut protein：1 part；
Carragheen：1 part.
The preparation method of peanut protein-carragheen composite particles, is carried out as steps described below：
(1) peanut protein is dissolved into distilled water, magnetic agitation to albumen is completely dissolved；Obtaining peanut protein concentration is
(1-10) mg/mL solution；
(2) carragheen is dissolved into the aqueous solution, magnetic agitation is to being completely dissolved；Concentration is obtained for (1-15) mg/mL cards
Draw sol solution；
(3) it is 1 by volume by step (2) carrageenan solutions:1 ratio is added dropwise to step (1) peanut protein solution
In so that the mass ratio of peanut protein and carragheen is：(1~10)：(1~15), then adjusts the pH=4- of mixed solution
7。
(4) mixed solution for obtaining step (3) carries out the processing of double frequency frequency sweep ultrasonic ripple, and ultrasound condition is：Between upper and lower plates
Away from for 10cm, frequency sweep cycle 300s, intermittently than 1:1 (ultrasonic 5s, interval 5s), every piece of vibration plate power is 600W up and down.
(5) after ultrasound terminates, 1h is stood at room temperature, peanut protein-carragheen composite particles solution is produced, spray drying or
Peanut protein-carragheen complex coacervation thing is obtained after person's freeze-drying.
The pH=5 of preferred regulation mixed solution wherein in step (3).
Wherein the mass ratio of peanut protein and carragheen is preferably 1 in step (3)：1.
Double frequency combination of frequency wherein described in step (4) is：33kHz/40kHz、28kHz/33kHz、40kHz/
28kHz、28kHz/68kHz；Optimized frequency is combined as 33kHz/40kHz.
The preparation method of the composite particle-loaded Tea Polyphenols of peanut protein-carragheen, is carried out as steps described below：
(1) peanut protein is dissolved into distilled water, magnetic agitation to albumen is completely dissolved；Obtaining peanut protein concentration is
(1-10) mg/mL solution；
(2) carragheen is dissolved into the aqueous solution, magnetic agitation is to being completely dissolved；Concentration is obtained for (1-15) mg/mL cards
Draw sol solution；
(3) it is 1 by volume by step (2) carrageenan solutions:1 ratio is added dropwise to step (1) peanut protein solution
In so that the mass ratio of peanut protein and carragheen is：(1~10)：(1~15), then adjusts the pH=4- of mixed solution
7。
(4) Tea Polyphenols of certain mass is added in peanut protein and carragheen composite particles solution prepared by step (3),
So that the mass ratio of peanut protein and Tea Polyphenols is 1：(1~5)；
(5) mixed solution for obtaining step (4) carries out the processing of double frequency frequency sweep ultrasonic ripple, and ultrasound condition is：Between upper and lower plates
Away from for 10cm, frequency sweep cycle 300s, intermittently than 1:1 (ultrasonic 5s, interval 5s), every piece of vibration plate power is 600W up and down.
(6) after ultrasound terminates, 1h is stood at room temperature, and the peanut protein-carragheen composite particles for producing loading tea polyphenol are molten
Peanut protein-carragheen composite particles of loading tea polyphenol are obtained after liquid, spray drying or freeze-drying.
The pH=5 of preferred regulation mixed solution wherein in step (3).
Wherein the mass ratio of peanut protein and carragheen is preferably 1 in step (3)：2.
Wherein the mass ratio of peanut protein and Tea Polyphenols is preferably 1 in step (4)：2.
Double frequency combination of frequency wherein described in step (5) is：33kHz/40kHz、28kHz/33kHz、40kHz/
28kHz、28kHz/68kHz；Optimized frequency is combined as 33kHz/40kHz.
The preparation method of peanut protein-carragheen composite particles, is carried out as steps described below：
(1) peanut protein is dissolved into distilled water, magnetic agitation to albumen is completely dissolved；Obtaining peanut protein concentration is
(1-10) mg/mL solution；
(2) carragheen is dissolved into the aqueous solution, magnetic agitation is to being completely dissolved；Concentration is obtained for (1-15) mg/mL cards
Draw sol solution；
(3) it is 1 by volume by step (2) carrageenan solutions:1 ratio is added dropwise to step (1) peanut protein solution
In so that the mass ratio of peanut protein and carragheen is：(1~10)：(1~15), then adjusts the pH=4- of mixed solution
7。
(4) multifrequency mode ultrasound processing is carried out to the mixed solution of step (3), wherein described multiple frequency ultrasonic tupe
For：Three frequency synchronizing ultrasounds are handled or double-frequency synchronous is ultrasonically treated or single-frequency is ultrasonically treated, and ultrasonic power density 100~
150W/L；Ultrasonic pulse working time 10s；Interpulse period 5s, sonication treatment time is 40min.
(5) after ultrasound terminates, 1h is stood at room temperature, peanut protein-carragheen composite particles solution is produced, spray drying or
Peanut protein-carragheen complex coacervation thing is obtained after person's freeze-drying.
The pH=5 of preferred regulation mixed solution wherein in step (3).
Wherein the mass ratio of peanut protein and carragheen is preferably 1 in step (3)：1.
Three frequency synchronizing ultrasounds processing or that double-frequency synchronous is ultrasonically treated or single-frequency is ultrasonically treated is super wherein in step (4)
Frequency of sound wave is combined as：22kHz, 28kHz, 22/40kHz or 28/22/40kHz, preferably 28/22/40kHz.
The preparation method of the composite particle-loaded Tea Polyphenols of peanut protein-carragheen, is carried out as steps described below：
(1) peanut protein is dissolved into distilled water, magnetic agitation to albumen is completely dissolved；Obtaining peanut protein concentration is
(1-10) mg/mL solution；
(2) carragheen is dissolved into the aqueous solution, magnetic agitation is to being completely dissolved；Concentration is obtained for (1-15) mg/mL cards
Draw sol solution；
(3) it is 1 by volume by step (2) carrageenan solutions:1 ratio is added dropwise to step (1) peanut protein solution
In so that the mass ratio of peanut protein and carragheen is：(1~10)：(1~15), then adjusts the pH=4- of mixed solution
7。
(4) Tea Polyphenols of certain mass is added in peanut protein and carragheen composite particles solution prepared by step (3),
So that the mass ratio of peanut protein and Tea Polyphenols is 1：(1~5)；
(5) multifrequency mode ultrasound processing is carried out to the mixed solution of step (4), wherein described multiple frequency ultrasonic tupe
For：Three frequency synchronizing ultrasounds are handled or double-frequency synchronous is ultrasonically treated or single-frequency is ultrasonically treated, and ultrasonic power density 100~
150W/L；Ultrasonic pulse working time 10s；Interpulse period 5s, sonication treatment time is 40min.
(6) after ultrasound terminates, 1h is stood at room temperature, and the peanut protein-carragheen composite particles for producing loading tea polyphenol are molten
Peanut protein-carragheen composite particles of loading tea polyphenol are obtained after liquid, spray drying or freeze-drying.
The pH=5 of preferred regulation mixed solution wherein in step (3).
Wherein the mass ratio of peanut protein and carragheen is preferably 1 in step (3)：1.
Wherein the mass ratio of peanut protein and Tea Polyphenols is preferably 1 in step (4)：2.
Three frequency synchronizing ultrasounds processing or that double-frequency synchronous is ultrasonically treated or single-frequency is ultrasonically treated is super wherein in step (5)
Frequency of sound wave is combined as：22kHz, 28kHz, 22/40kHz or 28/22/40kHz, preferably 28/22/40kHz.
The peanut protein of loading tea polyphenol-carragheen composite particles, with stability is good, good biocompatibility, sustained release when
Between it is long, contain the advantages of rate is high, can be applied to make health food, food or medicine.
The beneficial effects of the present invention are：
(1) present invention adds carragheen into peanut protein, changes the higher structure of peanut protein, opens its structure,
Exposure active group, while protein and polysaccharide form small aggregation, so as to promote each aggregation to pass through hydrophobic interaction
Form composite particles and provide basis for embedding bioactive ingredients.
(2) present invention uses frequency sweep ultrasonic during using peanut protein-carragheen composite particles embedding Tea Polyphenols
Ripple treatment technology or multi-mode ultrasonic technology, promote protein by the physical force of ultrasonic wave and polysaccharide are cross-linked into aggregation
Body, so as to promote each aggregation by hydrophobic interaction formation composite particles, basis is provided for embedding bioactive ingredients.
(3) preparation method of peanut protein-carragheen composite particles of Tea Polyphenols, technological operation letter are embedded in the present invention
It is single, organic reagent, suitable industrialized production, and peanut protein are not directed in preparation process and carragheen cost of material is cheap, system
Standby technique is simple.
(4) peanut protein-carragheen composite particles of embedding Tea Polyphenols of the invention have that stability is good, biocompatibility
Good, slow-release time length, the advantages of rate is high is contained, can be applied to the multiple fields such as food, health products, medicine and cosmetics.
Brief description of the drawings
Fig. 1 is the multi-mode ultrasonic wave biological processing equipment structure chart of the present invention, wherein 1,2,3 be ultrasonic vibrating plate, 4 be Sheng
Liquid device, 5 be water-bath, and 6 be temp probe, and 7 be circulating pump, and 8 be Computerized controller, and 9,10,11 be ultrasonic controller.
Fig. 2 is the equipment drawing of frequency sweep double-frequency ultrasound pretreatment unit, 1- ultrasounds pond, 2- thermometers, 3- thermostatted water bathing pools, 4-
Vibration plate under vibration plate on ultrasonic wave, 5- ultrasonic waves, 6- sample treatments region, 7- computer controllers, 8- supersonic generators.
Embodiment
Used term, unless otherwise indicated, can typically be understood by those of ordinary skill in the art in the present invention.
The present invention is described in further detail with reference to specific embodiment, and with reference to data.Illustrate hereby：These embodiments are
In order to demonstrate the invention, rather than in any way the scope of the present invention is limited.
Fig. 1 is multi-mode ultrasonic wave biological processing equipment of the invention, and the equipment is furnished with a Computerized controller 8,
Ultrasound works parameter (ultrasonic power density, frequency, pulse working time, intermittent time and processing total time) can be set to control respectively
Three ultrasonic controllers 9,10,11 are made, the ultrasonic vibrating plate 1,2,3 of three different frequencies is connected respectively, single-frequency/two can be achieved
Individual frequency/tri- frequency ultrasonic wave processing；Solution input to be processed will be needed to contain single-frequency/double frequency/multiple frequency ultrasonic is carried out in liquid device 4
Processing, starts circulating pump 7 and solution is circulated.Automatically controlling for solution temperature is realized by water-bath 5 and temp probe 6.
The equipment drawing for the frequency sweep double-frequency ultrasound pretreatment unit that Fig. 2 uses for the present invention, is Jiangsu University's independent development.It is super
Acoustic generator 8 can send the ultrasonic wave for determining frequency and frequency sweep both of which, and separate unit supersonic generator power is 600W.In ultrasonic pond
Placement ultrasonic wave vibration plate upper plate 4 symmetrical above and below and ultrasonic wave lower plate 5, are controlled on ultrasonic wave vibration plate by supersonic generator 8 in 1
Plate 4 and ultrasonic wave lower plate 5；After the setting each parameter of ultrasonic wave of computer controller 7, supersonic generator 8 is controlled, sends and meets the requirements
Ultrasonic wave；3 be the thermostatted water bathing pool of equipment in the present invention, passes through the monitoring temperature, and being adjusted according to need of work in real time of thermometer 2
Save medium temperature；Need to liquid raw material to be processed be placed in sample sack to be placed in treatment fluid region 6 and carry out ultrasonication.
Peanut protein in the present invention is commercially available prod, and food grade products, lipidated protein is more than 90%.
Carragheen in the present invention is κ-type carragheen, ι-type carragheen and λ-type carragheen, commercially available prod, food-grade production
Product.
Tea polyphenol raw materials in the present invention are commercially available prod, and food grade products, purity is more than 90%.
Embodiment 1-6 (is not added with ultrasound)
The preparation method of the composite particle-loaded Tea Polyphenols of peanut protein-carragheen, is carried out as steps described below：
(1) peanut protein is dissolved into distilled water, magnetic agitation to albumen is completely dissolved；Obtaining peanut protein concentration is
(1-10) mg/mL solution；
(2) kappa-carrageenan is dissolved into the aqueous solution, magnetic agitation is to being completely dissolved；Concentration is obtained for (1-15) mg/mL
Carrageenan solutions；
(3) it is 1 by volume by step (2) carrageenan solutions:1 ratio is added dropwise to step (1) peanut protein solution
In so that then the mass ratio of peanut protein and carragheen adjusts the pH=5 of mixed solution to be shown in Table 1.
(4) Tea Polyphenols of certain mass is added in peanut protein and carragheen composite particles solution prepared by step (3),
So that the mass ratio of peanut protein and Tea Polyphenols is 1：2；
(5) 1h is stood at room temperature, produces peanut protein-carragheen composite particles solution, spray drying or freeze-drying
Peanut protein-carragheen complex coacervation thing is obtained afterwards.
(6) measure of Tea Polyphenols envelop rate and load factor
Peanut protein-carragheen composite particles solution of loading tea polyphenol is taken, is centrifuged using high speed freezing centrifuge
The measure of Tea Polyphenols mainly uses tartaric acid iron colorimetric method for determining in (10000rpm, 4 DEG C) 30min, supernatant, specific as follows：
Supernatant after high speed centrifugation is transferred in 50mL volumetric flasks, distilled water is added to scale.Prepare liquid 5mL is drawn, is placed in
In 25mL volumetric flasks, plus ferrous sulfate aqueous solution 5mL, fully mix, then add the phosphoric acid hydrogen two that pH7.5, concentration are 1/15mol/L
Sodium-potassium phosphate buffer is to scale.10mm cuvettes are used, at wavelength 540nm, reference is made with blank reagent solution, are surveyed
Determine absorbance (OD).A certain amount of Tea Polyphenols sample is accurately weighed according to same method to be dissolved in distilled water, is settled to 50mL
Afterwards, it is diluted to after various concentrations, makes the standard curve of Tea Polyphenols.According to the Tea Polyphenols dissociated in regression equation calculation prepare liquid
Content.
The envelop rate and load factor of Tea Polyphenols are calculated according to following formula：
The envelop rate (%) of the Tea Polyphenols=total matter of Tea Polyphenols of (Tea Polyphenols gross mass-supernatant Tea Polyphenols quality) × 100/
Amount；
The load factor (%) of the Tea Polyphenols=total matter of composite particles of (Tea Polyphenols gross mass-clear liquid Tea Polyphenols quality) × 100/
Amount.
Embodiment 1-6 preparation process is identical, and simply peanut protein/carragheen mass ratio is different, is specifically shown in Table 1 different quality
Influence of the peanut protein/carragheen of ratio to Tea Polyphenols envelop rate and load factor.
By comparative example 1-6 different qualities in table 1 than peanut protein/carragheen to Tea Polyphenols envelop rate and load
The influence of rate can be seen that (is not added with carragheen, i.e. embodiment 6) compared with the control, and addition carragheen can significantly improve peanut
Albumen embeds the envelop rate of Tea Polyphenols；Peanut protein/carragheen mass ratio is 1:When 5 the envelop rate of Tea Polyphenols can improve
37.5%, peanut protein/carragheen mass ratio is 1:The envelop rate of Tea Polyphenols is then set to improve 75.0% when 1.
Different peanut protein/influences of the carragheen mass ratio to Tea Polyphenols envelop rate and load factor of table 1
Embodiment 7-10 (processing of frequency sweep dual-frequency ultrasonic wave)
Peanut protein：10 parts；
Carragheen：15 parts.
The preparation method of the composite particle-loaded Tea Polyphenols of peanut protein-carragheen, is carried out as steps described below：
(1) peanut protein is dissolved into distilled water, magnetic agitation to albumen is completely dissolved；Obtaining peanut protein concentration is
10mg/mL solution；
(2) ι-type carragheen is dissolved into the aqueous solution, magnetic agitation is to being completely dissolved；Concentration is obtained for 15mg/mL cards
Draw sol solution；
(3) it is 1 by volume by step (2) carrageenan solutions:1 ratio is added dropwise to step (1) peanut protein solution
In so that the mass ratio of peanut protein and carragheen is 10:15, then adjust the pH=5 of mixed solution.
(4) Tea Polyphenols of certain mass is added in peanut protein and carragheen composite particles solution prepared by step (3),
So that the mass ratio of peanut protein and Tea Polyphenols is 1：2；
(5) mixed solution for obtaining step (4) carries out the processing of double frequency frequency sweep ultrasonic ripple, and ultrasound condition is：Between upper and lower plates
Away from for 10cm, frequency sweep cycle 300s, intermittently than 1:1 (ultrasonic 5s, interval 5s), every piece of vibration plate power is 600W up and down.
(6) after ultrasound terminates, 1h is stood at room temperature, peanut protein-carragheen composite particles solution is produced, spray drying or
Peanut protein-carragheen complex coacervation thing is obtained after person's freeze-drying.
(7) measure of Tea Polyphenols envelop rate and load factor
Peanut protein-carragheen composite particles solution of loading tea polyphenol is taken, is centrifuged using high speed freezing centrifuge
The measure of Tea Polyphenols mainly uses tartaric acid iron colorimetric method for determining in (10000rpm, 4 DEG C) 30min, supernatant, specific as follows：
Supernatant after high speed centrifugation is transferred in 50mL volumetric flasks, distilled water is added to scale.Prepare liquid 5mL is drawn, is placed in
In 25mL volumetric flasks, plus ferrous sulfate aqueous solution 5mL, fully mix, then add the phosphoric acid hydrogen two that pH7.5, concentration are 1/15mol/L
Sodium-potassium phosphate buffer is to scale.10mm cuvettes are used, at wavelength 540nm, reference is made with blank reagent solution, are surveyed
Determine absorbance (OD).A certain amount of Tea Polyphenols sample is accurately weighed according to same method to be dissolved in distilled water, is settled to 50mL
Afterwards, it is diluted to after various concentrations, makes the standard curve of Tea Polyphenols.According to the Tea Polyphenols dissociated in regression equation calculation prepare liquid
Content.
The envelop rate and load factor of Tea Polyphenols are calculated according to following formula：
The envelop rate (%) of the Tea Polyphenols=total matter of Tea Polyphenols of (Tea Polyphenols gross mass-supernatant Tea Polyphenols quality) × 100/
Amount；
The load factor (%) of the Tea Polyphenols=total matter of composite particles of (Tea Polyphenols gross mass-clear liquid Tea Polyphenols quality) × 100/
Amount.
Embodiment 7-10 preparation process is identical, and simply ultrasound parameter is slightly changed, and the different ultrasound modes of table 2 are to Tea Polyphenols
The influence of envelop rate and load factor.
Influence of the different ultrasound modes of table 2 to Tea Polyphenols envelop rate and load factor
| Embodiment | Supersonic frequency or pattern | Envelop rate % | Load factor % |
| Comparative example (i.e. embodiment 4) | It is not ultrasonic | 40.1 | 5.1 |
| Embodiment 7 | 33kHz/40kHz | 64.9 | 6.2 |
| Embodiment 8 | 28kHz/33kHz | 53.8 | 5.2 |
| Embodiment 9 | 40kHz/28kHz | 55.9 | 5.6 |
| Embodiment 10 | 28kHz/68kHz | 58.7 | 5.9 |
The frequency sweep ultrasonic ripple combined by comparative example 7-10 different frequencies in table 2 is to Tea Polyphenols envelop rate and load factor
Influence, it can be found that the processing of frequency sweep ultrasonic ripple can significantly improve peanut protein-carragheen composite particles embedding Tea Polyphenols
Envelop rate, compared with the control (not ultrasonic), double frequency frequency sweep ultrasonic ripple processing can make Tea Polyphenols envelop rate improve 34.2%~
61.8%, and the processing of 33kHz/40kHz double frequency frequency sweep ultrasonic ripple then makes the envelop rate of Tea Polyphenols improve 61.8%.
Embodiment 11-14 (processing of multi-mode frequency ultrasonic wave)
Peanut protein：10 parts；
Carragheen：15 parts.
The preparation method of the composite particle-loaded Tea Polyphenols of peanut protein-carragheen, is carried out as steps described below：
(1) peanut protein is dissolved into distilled water, magnetic agitation to albumen is completely dissolved；Obtaining peanut protein concentration is
10mg/mL solution；
(2) λ-type carragheen is dissolved into the aqueous solution, magnetic agitation is to being completely dissolved；Concentration is obtained for 15mg/mL cards
Draw sol solution；
(3) it is 1 by volume by step (2) carrageenan solutions:1 ratio is added dropwise to step (1) peanut protein solution
In so that the mass ratio of peanut protein and carragheen is 10:15, then adjust the pH=5 of mixed solution.
(4) Tea Polyphenols of certain mass is added in peanut protein and carragheen composite particles solution prepared by step (3),
So that the mass ratio of peanut protein and Tea Polyphenols is 1：2；
(5) multifrequency mode ultrasound processing is carried out to the mixed solution of step (4), wherein described multiple frequency ultrasonic tupe
For：Three frequency synchronizing ultrasounds are handled or double-frequency synchronous is ultrasonically treated or single-frequency is ultrasonically treated, ultrasonic power density 100W/L；It is super
Ping working time 10s；Interpulse period 5s, sonication treatment time is 40min.
(6) after ultrasound terminates, 1h is stood at room temperature, peanut protein-carragheen composite particles solution is produced, spray drying or
Peanut protein-carragheen complex coacervation thing is obtained after person's freeze-drying.
(7) measure of Tea Polyphenols envelop rate and load factor
Peanut protein-carragheen composite particles solution of loading tea polyphenol is taken, is centrifuged using high speed freezing centrifuge
The measure of Tea Polyphenols mainly uses tartaric acid iron colorimetric method for determining in (10000rpm, 4 DEG C) 30min, supernatant, specific as follows：
Supernatant after high speed centrifugation is transferred in 50mL volumetric flasks, distilled water is added to scale.Prepare liquid 5mL is drawn, is placed in
In 25mL volumetric flasks, plus ferrous sulfate aqueous solution 5mL, fully mix, then add the phosphoric acid hydrogen two that pH7.5, concentration are 1/15mol/L
Sodium-potassium phosphate buffer is to scale.10mm cuvettes are used, at wavelength 540nm, reference is made with blank reagent solution, are surveyed
Determine absorbance (OD).A certain amount of Tea Polyphenols sample is accurately weighed according to same method to be dissolved in distilled water, is settled to 50mL
Afterwards, it is diluted to after various concentrations, makes the standard curve of Tea Polyphenols.According to the Tea Polyphenols dissociated in regression equation calculation prepare liquid
Content.
The envelop rate and load factor of Tea Polyphenols are calculated according to following formula：
The envelop rate (%) of the Tea Polyphenols=total matter of Tea Polyphenols of (Tea Polyphenols gross mass-supernatant Tea Polyphenols quality) × 100/
Amount；
The load factor (%) of the Tea Polyphenols=total matter of composite particles of (Tea Polyphenols gross mass-clear liquid Tea Polyphenols quality) × 100/
Amount.
Embodiment 11-14 preparation process is identical, and simply ultrasound parameter is slightly changed, and the different ultrasound modes of table 3 are more to tea
The influence of phenol envelop rate and load factor.
Influence of the different ultrasound modes of table 3 to Tea Polyphenols envelop rate and load factor
The ultrasonic wave combined by comparative example 11-14 different modes multi-frequency in table 3 is to Tea Polyphenols envelop rate and bears
The influence of load rate, it can be found that the processing of multi-mode frequency ultrasonic wave can significantly improve peanut protein-carragheen composite particles bag
The envelop rate of Tea Polyphenols is buried, compared with the control (not ultrasonic), the processing of double frequency frequency sweep ultrasonic ripple can carry the envelop rate of Tea Polyphenols
It is high by 29.4%~58.6%, and the processing of 28kHz/22kHz/40kHz three frequently combined ultrasonic ripples then carries the envelop rate of Tea Polyphenols
It is high by 58.6%.
Claims (10)
1. peanut protein-carragheen composite particles, it is characterised in that be prepared from by the raw material of following parts by weight：
Peanut protein：1~10 part；
Carragheen：1~15 part.
2. peanut protein according to claim 1-carragheen composite particles, it is characterised in that the raw material system of following parts by weight
It is standby to form：
Peanut protein：1 part；
Carragheen：1 part.
3. the preparation method of peanut protein according to claim 1 or 2-carragheen composite particles, it is characterised in that according to
Following step is carried out：
（1）Peanut protein is dissolved into distilled water, magnetic agitation to albumen is completely dissolved；Obtaining peanut protein concentration is（1-
10）Mg/mL solution；
（2）Carragheen is dissolved into the aqueous solution, magnetic agitation is to being completely dissolved；Obtaining concentration is（1-15）Mg/mL carragheens
Solution；
（3）By step（2）Carrageenan solutions are 1 by volume:1 ratio is added dropwise to step（1）In peanut protein solution, make
The mass ratio of peanut protein and carragheen is：（1~10）：（1~15）, then adjust pH=4-7 of mixed solution；
（4）By step（3）Obtained mixed solution carries out the processing of double frequency frequency sweep ultrasonic ripple, and ultrasound condition is：Upper and lower plates spacing is
10cm, frequency sweep cycle 300s, intermittently than 1:1（Ultrasonic 5s, interval 5s）, every piece of vibration plate power is 600W up and down；
（5）After ultrasound terminates, 1h is stood at room temperature, produces peanut protein-carragheen composite particles solution, spray drying or cold
It is lyophilized it is dry after peanut protein-carragheen complex coacervation thing.
4. the preparation method of peanut protein according to claim 3-carragheen composite particles, it is characterised in that wherein step
（3）In preferred regulation mixed solution pH=5；
Wherein step（3）The mass ratio of middle peanut protein and carragheen is preferably 1：1；
Wherein step（4）Described in double frequency combination of frequency be：33 kHz/ 40kHz、28kHz/33kHz、40 kHz/28
kHz、28 kHz/68 kHz；Optimized frequency is combined as 33kHz/40 kHz.
5. the preparation method of the composite particle-loaded Tea Polyphenols of peanut protein-carragheen, it is characterised in that carry out as steps described below：
（1）Peanut protein is dissolved into distilled water, magnetic agitation to albumen is completely dissolved；Obtaining peanut protein concentration is（1-
10）Mg/mL solution；
（2）Carragheen is dissolved into the aqueous solution, magnetic agitation is to being completely dissolved；Obtaining concentration is（1-15）Mg/mL carragheens
Solution；
（3）By step（2）Carrageenan solutions are 1 by volume:1 ratio is added dropwise to step（1）In peanut protein solution, make
The mass ratio of peanut protein and carragheen is：（1~10）：（1~15）, then adjust pH=4-7 of mixed solution；
（4）The Tea Polyphenols of certain mass is added into step（3）In the peanut protein and carragheen composite particles solution of preparation so that
The mass ratio of peanut protein and Tea Polyphenols is 1：（1~5）；
（5）By step（4）Obtained mixed solution carries out the processing of double frequency frequency sweep ultrasonic ripple, and ultrasound condition is：Upper and lower plates spacing is
10cm, frequency sweep cycle 300s, intermittently than 1:1（Ultrasonic 5s, interval 5s）, every piece of vibration plate power is 600W up and down；
（6）After ultrasound terminates, 1h is stood at room temperature, peanut protein-carragheen composite particles solution of loading tea polyphenol is produced, and is sprayed
Peanut protein-carragheen composite particles of loading tea polyphenol are dried or obtained after being freeze-dried to mist.
6. the preparation method of the composite particle-loaded Tea Polyphenols of peanut protein-carragheen according to claim 5, its feature exists
In wherein step（3）In preferred regulation mixed solution pH=5；
Wherein step（3）The mass ratio of middle peanut protein and carragheen is preferably 1：2；
Wherein step（4）The mass ratio of middle peanut protein and Tea Polyphenols is preferably 1：2；
Wherein step（5）Described in double frequency combination of frequency be： 33 kHz/ 40kHz、28kHz/33kHz、40 kHz/28
kHz、28 kHz/68 kHz；Optimized frequency is combined as 33kHz/40 kHz.
7. the preparation method of peanut protein according to claim 1 or 2-carragheen composite particles, it is characterised in that or
Carry out as steps described below：
（1）Peanut protein is dissolved into distilled water, magnetic agitation to albumen is completely dissolved；Obtaining peanut protein concentration is（1-
10）Mg/mL solution；
（2）Carragheen is dissolved into the aqueous solution, magnetic agitation is to being completely dissolved；Obtaining concentration is（1-15）Mg/mL carragheens
Solution；
（3）By step（2）Carrageenan solutions are 1 by volume:1 ratio is added dropwise to step（1）In peanut protein solution, make
The mass ratio of peanut protein and carragheen is：（1~10）：（1~15）, then adjust pH=4-7 of mixed solution；
（4）To step（3）Mixed solution carry out multifrequency mode ultrasound processing, wherein described multiple frequency ultrasonic tupe is：
Three frequency synchronizing ultrasounds are handled or double-frequency synchronous is ultrasonically treated or single-frequency is ultrasonically treated, the W/L of ultrasonic power density 100 ~ 150；
The s of ultrasonic pulse working time 10；The s of interpulse period 5, sonication treatment time is 40min；
（5）After ultrasound terminates, 1h is stood at room temperature, produces peanut protein-carragheen composite particles solution, spray drying or cold
It is lyophilized it is dry after peanut protein-carragheen complex coacervation thing.
8. the preparation method of peanut protein according to claim 7-carragheen composite particles, it is characterised in that wherein step
（3）In preferred regulation mixed solution pH=5；
Wherein step（3）The mass ratio of middle peanut protein and carragheen is preferably 1：1；
Wherein step（4）In the processing of three frequency synchronizing ultrasounds or double-frequency synchronous is ultrasonically treated or single-frequency is ultrasonically treated ultrasonic wave
Combination of frequency is：22kHz, 28kHz, 22/40 kHz or 28/22/40 kHz, preferably 28/22/40 kHz.
9. the preparation method of the composite particle-loaded Tea Polyphenols of peanut protein-carragheen, it is characterised in that or as steps described below
Carry out：
（1）Peanut protein is dissolved into distilled water, magnetic agitation to albumen is completely dissolved；Obtaining peanut protein concentration is（1-
10）Mg/mL solution；
（2）Carragheen is dissolved into the aqueous solution, magnetic agitation is to being completely dissolved；Obtaining concentration is（1-15）Mg/mL carragheens
Solution；
（3）By step（2）Carrageenan solutions are 1 by volume:1 ratio is added dropwise to step（1）In peanut protein solution, make
The mass ratio of peanut protein and carragheen is：（1~10）：（1~15）, then adjust pH=4-7 of mixed solution；
（4）The Tea Polyphenols of certain mass is added into step（3）In the peanut protein and carragheen composite particles solution of preparation so that
The mass ratio of peanut protein and Tea Polyphenols is 1：（1~5）；
（5）To step（4）Mixed solution carry out multifrequency mode ultrasound processing, wherein described multiple frequency ultrasonic tupe is：
Three frequency synchronizing ultrasounds are handled or double-frequency synchronous is ultrasonically treated or single-frequency is ultrasonically treated, the W/L of ultrasonic power density 100 ~ 150；
The s of ultrasonic pulse working time 10；The s of interpulse period 5, sonication treatment time is 40min；
（6）After ultrasound terminates, 1h is stood at room temperature, peanut protein-carragheen composite particles solution of loading tea polyphenol is produced, and is sprayed
Peanut protein-carragheen composite particles of loading tea polyphenol are dried or obtained after being freeze-dried to mist；
Wherein step（3）In preferred regulation mixed solution pH=5；
Wherein step（3）The mass ratio of middle peanut protein and carragheen is preferably 1：1；
Wherein step（4）The mass ratio of middle peanut protein and Tea Polyphenols is preferably 1：2；
Wherein step（5）In the processing of three frequency synchronizing ultrasounds or double-frequency synchronous is ultrasonically treated or single-frequency is ultrasonically treated ultrasonic wave
Combination of frequency is：22kHz, 28kHz, 22/40 kHz or 28/22/40 kHz, preferably 28/22/40 kHz.
10. the purposes of the peanut protein of loading tea polyphenol-carragheen composite particles, it is characterised in that for make health food,
Food or medicine.
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| CN113230234A (en) * | 2021-04-27 | 2021-08-10 | 江苏大学 | Ultrasonic preparation method of bioactive ingredient-loaded protein peptide-polysaccharide nanoparticles |
| CN113289559A (en) * | 2021-06-04 | 2021-08-24 | 中国农业大学 | Nano microcapsule embedding hydrophilic compound and preparation method and application thereof |
| CN113289559B (en) * | 2021-06-04 | 2022-03-25 | 中国农业大学 | Nano microcapsule embedding hydrophilic compound and preparation method and application thereof |
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