CN108641103A - Phase emulsion oil-in-water and preparation method in a kind of protein stabilized height - Google Patents
Phase emulsion oil-in-water and preparation method in a kind of protein stabilized height Download PDFInfo
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- CN108641103A CN108641103A CN201810314148.0A CN201810314148A CN108641103A CN 108641103 A CN108641103 A CN 108641103A CN 201810314148 A CN201810314148 A CN 201810314148A CN 108641103 A CN108641103 A CN 108641103A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/11—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids from solid polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
- C08J3/092—Hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
- C08J3/095—Oxygen containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2389/00—Characterised by the use of proteins; Derivatives thereof
Abstract
The invention belongs to lotion preparing technical field, phase emulsion oil-in-water and preparation method in a kind of protein stabilized height are disclosed.Albumen is dispersed in water, water phase protein solution is obtained after abundant aquation, oil phase emulsification is then added, obtains phase emulsion oil-in-water in protein stabilized height.The present invention is not necessarily to any coagulator or surfactant, and phase emulsion oil-in-water viscoplasticity is good in gained height, thermostabilization and bin stability are high, has excellent protection or controlled-release effect to oil phase；Gelation is good, and plasticity is strong with remoldability, is conducive to further processing, has a good application prospect in chemical products, daily chemical product, drug, food and field of health care products.
Description
Technical field
The invention belongs to lotion preparing technical fields, and in particular in a kind of protein stabilized high phase emulsion oil-in-water and
Preparation method.
Background technology
High Internal Phase Emulsion typically refers to the lotion that dispersed phase (interior phase) percent by volume is more than 74%, in chemical products, day
Changing articles for use, drug, food and health products trade has outstanding application present situation and huge application potential.But common height
The preparation of internal phase emulsions usually requires a large amount of surfactant with stabilization, and these surfactants are usually prepared in its production
It generates in the process or itself has the factor unfavorable to health or ecological environment.Therefore, it is used in that human body is harmless, environment is friendly
Good or degradable emulsifier, which prepares High Internal Phase Emulsion, has highly important society, environment and economic benefit.In recent years, full
It is common preparing water that nano level amphipathic (the hydrophily and lipophile) albumen of sufficient requirements above has become field of food
The emulsifier of oil-in lotion, it is slow with the targeting for reaching the bin stability or realization oil-soluble bioactive substance that improve oil phase
The purpose released.And utilize phase emulsion oil-in-water in the more extensive height of the animal/vegetable protein application and preparation range of source abundance
Report is still seldom with invention.
Chinese invention patent application 2016110095755 and 201611004761X has been opened respectively utilizes wheat gliadin
The method for preparing phase emulsion oil-in-water in height with zeins.But both methods is established first by cumbersome
On the basis of chemically or physically method processing (such as anti-solvent method) prepares two kinds of protein-colloid particles, inconvenient, cost is higher.
Therefore, preparing phase emulsion oil-in-water in novel height using natural or simply dealt albumen has prior meaning.
The common nanoscale albumen with surface-active can be divided into unordered albumen and globulin.Wherein, most typical normal
The unordered albumen seen is casein sodium；And globulin can be divided into monomer (haemocyanin, ovalbumin, lysozyme etc.), two
Aggressiveness (beta lactoglobulin etc.), tripolymer (beans 7S albumen etc.), six aggressiveness (beans 11S albumen etc.) and to mix globulin (big
Beans protein isolate, whey protein isolate etc.) etc..These albumen contain part hydrophobic grouping (being usually buried in inside) and part
The polar group for carrying charge, it is excellent amphipathic to assign its, oil-water interfaces can be adsorbed on, interfacial tension is reduced, are belonged to
In ideal oil-in-water emulsifiers.But in addition to conventional surfactant, phase emulsion oil-in-water is general in currently a popular height
Inevitably gone out by modified micron-sized inorganic or organic Pickering particles or artificial synthesized stabilizing polymer, operating process
Existing more poisonous and hazardous link or product.Though and relatively large grain size improves these Pickering particles from grease
Minimum energy needed for the desorption of interface, but also weaken its corresponding emulsifying power.In relation to utilizing the emulsifier from nature
It is extremely limited to carry out the report of phase emulsion oil-in-water preparation and invention in height, it is dynamic using natural or simply dealt nanoscale
Vegetable protein prepares phase emulsion oil-in-water in novel height and the report applied and invention are even more not disclosed.To sum up, sharp
Phase emulsion oil-in-water belongs to phase oil-in-water type breast in the novel height of one kind in the height prepared with natural or simply dealt albumen
Liquid, this lotion prepare great innovative, challenge and application prospect.
Invention content
In place of the above shortcoming and defect of the existing technology, the primary purpose of the present invention is that providing a kind of albumen
The preparation method of phase emulsion oil-in-water in stable height.
Another object of the present invention is to provide phase water in a kind of protein stabilized height being prepared by the above method
Oil-in lotion.
The object of the invention is achieved through the following technical solutions：
The preparation method of phase emulsion oil-in-water, specific preparation process are as follows in a kind of protein stabilized height：
Albumen is dispersed in water, water phase protein solution is obtained after abundant aquation, oil phase emulsification is then added, directly obtains
Phase emulsion oil-in-water in protein stabilized height of the oil phase volume percentage composition not less than 75%, or gone after lotion stratification
Except lower layer's water phase, phase emulsion oil-in-water in protein stabilized height of the oil phase volume percentage composition not less than 75% is obtained；
The albumen be casein sodium, haemocyanin, ovalbumin, lysozyme, beta lactoglobulin, beans 7S albumen,
At least one of beans 11S albumen, soybean protein isolate or whey protein isolate；The oil phase is n-dodecane, contains β-
In the n-dodecane of carrotene, n-hexane, lemon, Rosa Damascana, soybean oil, peanut oil, olive oil and ready-mixed oil extremely
Few one kind.
Preferably, in the protein stabilized height in phase emulsion oil-in-water oil phase volume percentage composition be 75%~
92%.More preferably 80%~92%.
Preferably, inorganic ion or polysaccharide are further added in the water phase protein solution.
Preferably, the water phase protein solution emulsifies the heat pre-treatment that takes a step forward.
Preferably, the mass concentration of albumen is 0.2%~5.0% in the water phase protein solution.
Preferably, the emulsification refers to using shearing emulsifying, ultrasonic emulsifying and high pressure microjet emulsifying
At least one of.The rotating speed of the shearing emulsifying is 2000~30000rpm, and the time is 0.5~3min；The ultrasound
The power of emulsifying is 100~900W, and the intermittent time is 1~5s, and total time is 0.5~3min；The high pressure microjet is equal
The pressure of matter emulsification is 40~100MPa, and number of processes is 1~3 time.
Phase emulsion oil-in-water in a kind of protein stabilized height, is prepared by the above method.
The present invention preparation method and obtained product has the following advantages that and advantageous effect：
(1) animal/vegetable protein used is invented to derive from a wealth of sources, produce at low cost, environmental-friendly, the degradable emulsifier of category, and
And it is harmless, or even have certain nutritive value.
(2) protein emulsifying used in the present invention is efficient, under the premise of without any coagulator or surfactant auxiliary,
Only need the albumen of low concentration (minimum reachable 0.04g/100g is in entire emulsion system) that can successfully prepare phase water in stable height
Oil-in lotion.
(3) phase emulsion oil-in-water can effectively embed the oil phase that percent by volume is more than 90% in present invention gained height.
(4) phase emulsion oil-in-water viscoplasticity is good in present invention gained height, thermostabilization and bin stability are high, has to oil phase
There are excellent protection or controlled-release effect；Gelation is good, and plasticity is strong with remoldability, is conducive to further processing.
(5) preparation method of the invention is low for equipment requirements, simple and practicable, at low cost, low energy consumption, is suitble to large-scale industry
Metaplasia is produced and processing, and phase emulsion oil-in-water is in chemical products, daily chemical product, drug, food and health products trade in gained height
With wide application space.
Description of the drawings
Fig. 1 is the emulsion oil-in-water of the different oil phase volume percentages of 1 gained of the embodiment of the present invention after being stored at room temperature 2h
Outside drawing.
Fig. 2 be 1 gained oil phase volume percentage of the embodiment of the present invention be 80% height in phase emulsion oil-in-water in room temperature
Stand the optical microscope after 2h.
Fig. 3 be 1 gained oil phase volume percentage of the embodiment of the present invention be 50% lotion after being stored at room temperature 2h, under removal
Chromatograph out phase emulsion oil-in-water optical microscope in the concentrated type height that water phase obtains.
Fig. 4 is oil phase volume percentages are 50% obtained by the shearing homogeneous of the embodiment of the present invention 3 lotion in being stored at room temperature
After 2h, except phase emulsion oil-in-water optical microscope in the concentrated type height that water phase obtains is precipitated in sub-cloud.
Fig. 5 is that first to shear the oil phase volume percentage that prepared by ultrasonic homogeneous method after homogeneous be 50% to the embodiment of the present invention 3
Lotion, and after being stored at room temperature 2h, except phase emulsion oil-in-water optical microphotograph in the concentrated type height that water phase obtains is precipitated in sub-cloud
Mirror figure.
Fig. 6 is that the embodiment of the present invention 3 first shears the oil phase volume percentage that prepared by high pressure microjet homogeneous method after homogeneous and is
50% lotion is shown after being stored at room temperature 2h except phase emulsion oil-in-water optics in the concentrated type height that water phase obtains is precipitated in sub-cloud
Micro mirror figure.
Fig. 7 is that the oil phase volume percentage that 4 ovalbumin of the embodiment of the present invention is prepared in different proteins amount concentration is
Phase emulsion oil-in-water has the design sketch of superior moldability and remoldability in 80% gel height.
Fig. 8 be 4 ovalbumin of the embodiment of the present invention a concentration of 0.16g/100g of albumen quality (in entire emulsion system and
Speech) when the oil phase volume percentage for preparing be 80% height in phase emulsion oil-in-water heat treatment and freeze thawing treatment before and after appearance
Figure.
Fig. 9 be 4 ovalbumin of the embodiment of the present invention in albumen quality concentration down to 0.04g/100g (in entire emulsion system
For) when the oil phase volume percentage for preparing be 80% height in appearance of the phase emulsion oil-in-water before and after room temperature storage 60d
Figure, optical microscope and viscoelastic rheometry shearing frequency scanning figure.
Specific implementation mode
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) 1g casein sodium Sample Spray dries accurately are weighed, is scattered in 99g distilled water (acquiescence distilled water
Density be 1.00g/mL), and continuously stir 2h in room temperature, keep albumen fully dispersed.
(2) gained casein sodium dispersion liquid (is added into matter before standing in 4 DEG C of stand at low temperature 12h in protein dispersion
The Sodium azide for measuring a concentration of 0.02g/100g prevents the growth of microorganism), make the abundant aquation of albumen, is to obtain mass concentration
The casein sodium of 1g/100g stores liquid.
(3) before preparing lotion, 0.5h is stirred at room temperature in casein sodium storage liquid, its temperature is made to restore to room temperature, and
Albumen is promoted to be uniformly dispersed.
(4) take respectively 4.5mL, 4.0mL, 3.5mL, 3.0mL, 2.5mL, 2.0mL, 1.5mL, 1.25mL, 1.0mL,
0.5mL, 0.45mL and 0.4mL casein sodium store liquid in the sample bottle that internal diameter is 2.0cm, as lotion water phase.
(5) and then successively add respectively 0.5mL, 1.0mL, 1.5mL, 2.0mL, 2.5mL, 3.0mL, 3.5mL, 3.75mL,
4.0mL, 4.55mL and 4.6mL n-dodecane are operated in water phase top without any mixing.Grease system in each sample bottle
Total volume is 5mL.
(6) emulsification pretreatment is carried out to each oil mixing with water system.Wherein, a diameter of 1cm of shearing machine head used, shearing speed
Rate is 5000rpm, shear time 2min.For oil phase volume be more than 90% lotion shearing homogeneous use shear rate for
2800rpm, shear time 1min.
Albumen quality concentration is 1g/100g (for water phase) in casein sodium lotion manufactured in the present embodiment, is led to
Cross and embed different oil phase volumes, respectively obtain different oil phase volume percentages (10%, 20%, 30%, 40%, 50%, 60%,
70%, 80%, 90%, 91% and casein sodium emulsion oil-in-water 92%).Gained lotion is in being stored at room temperature 2h, so
It is used to observe and other tests afterwards.
Outside drawing of the emulsion oil-in-water of gained difference oil phase volume percentage after being stored at room temperature 2h as shown in Figure 1,
When oil phase percentage is equal to or less than 70%, gained creaming of emulsion is apparent.And with the increase of oil phase volume percentage, institute
The breast analysis index for obtaining lotion continuously decreases.When oil phase volume percentage meets or exceeds 80%, gained lotion is transferred to interior
After diameter 1cm centrifuge tubes, inversion is not flowed, and the oil droplet size of lotion is smaller and uniform, and gained oil phase volume percentage is 80%
Optical microscope of the phase emulsion oil-in-water after being stored at room temperature 2h is as shown in Figure 2 in height.A certain amount of gained lotion is taken to carry out
Viscoelastic rheometry is tested, and plate diameter used is 2.783cm, and test temperature is 25 DEG C, is highly 0.1cm, strains and be
0.5%, shearing frequency ranging from 0.1Hz~10Hz (by the extra lotion wiped clean of plate edge before test).Except otherwise indicated
Outside, viscoelastic rheometry tests condition used with embodiment 1 in following embodiment.Within the scope of surveyed shearing frequency, lotion
Elasticity modulus is not influenced with viscous modulus by shearing frequency variation.When shearing frequency is 1Hz, gained oil phase volume percentage
Than being respectively 153Pa and 549Pa for the elasticity modulus of 80% and 92% lotion, viscous modulus is respectively 48Pa and 66Pa.This
Show that lotion of the gained oil phase volume percentage equal to or more than 80% has excellent viscoplasticity.
After the present embodiment stablizes low oil phase (oil phase volume percentage is less than 75%) lotion stratification, noted with band syringe needle
Emitter all extracts the water phase that bottom is precipitated, and the water phase rate of recovery is more than 92%, and remaining emulsion layer is then oil phase volume
Percentage is more than 75% emulsion oil-in-water.The lotion that gained oil phase volume percentage is 50% is after being stored at room temperature 2h, removal
It is as shown in Figure 3 that phase emulsion oil-in-water optical microscope in the concentrated type height that water phase obtains is precipitated in lower layer.Phase water in gained height
The characteristics of oil-in lotion category concentrated type High Internal Phase Emulsion equally has to be inverted and not flow, oil droplet densification and uniform particle diameter.
Embodiment 2
According to the method for embodiment 1, phase emulsion oil-in-water in the concentrated type height of bovine serum albumin stabilization is prepared.Removing protein
It changes and makees bovine serum albumin freeze-drying sample, oil phase, which changes, makees soybean oil, and emulsifying manner changes work and first shears homogeneous (shear rate is
5000rpm, shear time 2min) (ultrasonic power 285W, ultrasonic intermittent time are 3s to ultrasonic homogeneous, are ultrasonically treated total again
Time is 2min) outside, other operations are the same as embodiment 1.Contrast operation is the shearing homogeneous only with identical parameters.Wait for that lotion is stood
After layering is stablized, the water phase that bottom is precipitated all is extracted with needle applicator, the water phase rate of recovery is more than 92%, remaining
Emulsion layer then be oil phase volume percentage be more than 75% emulsion oil-in-water.Phase emulsion oil-in-water falls in gained concentrated type height
It sets and does not flow, and with than only shearing the smaller oil droplet size of concentrated type High Internal Phase Emulsion and higher springform obtained by homogeneous
Amount.
Embodiment 3
According to the method for embodiment 1, phase emulsion oil-in-water in the concentrated type height of lysozyme stabilization is prepared, removing protein changes work
Sample is lyophilized in lysozyme, and oil phase, which changes, makees peanut oil, and emulsifying manner changes work and first shears homogeneous (shear rate 5000rpm, when shearing
Between be 2min) outside, other operations are the same as embodiment 1 for high pressure microjet homogeneous (homogenization pressure 40MPa, number of processes be 1 time) again.
Contrast operation is that ultrasound is equal again for the shearing homogeneous only with identical parameters or the first shearing homogeneous according to 2 the method for embodiment
Matter.After lotion stratification stabilization, the water phase that bottom is precipitated all is extracted with needle applicator, the water phase rate of recovery
More than 92%, remaining emulsion layer is then that oil phase volume percentage is more than 75% emulsion oil-in-water.Gained oil phase volume percentage
Than the lotion for 50% after being stored at room temperature 2h, removal lower layer is precipitated phase emulsion oil-in-water in the concentrated type height that water phase obtains and falls
It sets and does not flow, and oil droplet size is nanoscale, optical microscope is as shown in Figure 6.With than only shearing homogeneous (microscope figure
See Fig. 4) or ultrasonic homogeneous (microscope figure is shown in Fig. 5) obtained by the smaller oil droplet size of concentrated type High Internal Phase Emulsion and higher elasticity
Modulus.
Embodiment 4
(1) accurate to weigh 5g ovalbumins freeze-drying sample, it is scattered in 95g distilled water, and continuously stirred in room temperature
2h keeps ovalbumin fully dispersed.
(2) gained ovalbumin dispersion liquid (is added before standing in ovalbumin dispersion liquid in 4 DEG C of stand at low temperature 12h
Mass concentration is the Sodium azide of 0.02g/100g, prevents the growth of microorganism), make the abundant aquation of ovalbumin, with gained quality
The ovalbumin of a concentration of 5g/100g stores liquid.
(3) before preparing lotion, 0.5h is stirred at room temperature in ovalbumin storage liquid, so that its temperature is restored to room temperature, and promote
It is uniformly dispersed into protein body.
(4) ovalbumin storage liquid is diluted with distilled water respectively, is respectively 0.2g/100g to obtain mass concentration
The ovalbumin solution of~5.0g/100g.
(5) take the ovalbumin solution of 1.0mL different quality concentration in sample bottle or plastics note that internal diameter is 2.0cm respectively
Emitter (ensures injection orifice sealing) when homogeneous, then addition 4.0mL olive oil is not necessarily in ovalbumin solution top respectively successively
Any mixing operation.Grease system total volume in each sample bottle is 5mL.
(6) emulsification pretreatment is carried out to each grease system.For a concentration of 0.2g/100g of ovalbumin quality in water phase
Lotion shearing homogeneous uses shear rate for 2 800rpm, shear time 0.5min.
Phase emulsion oil-in-water contained oil phase volume fraction is 80% in height manufactured in the present embodiment, respectively obtains difference
(0.04g/100g~1g/100g is in entire emulsion system for ovalbumin quality concentration.Unless otherwise indicated, following embodiment is high
Albumen quality concentration is for for entire emulsion system in internal phase emulsions) stabilization gel height in phase oil-in-water type breast
Liquid.Gained lotion is subsequently used for observation and other tests in being stored at room temperature 2h.
Observation indicate that in a concentration of 0.04g/100g~1g/100g of albumen quality, gained lotion can be inverted not
Flowing.Phase water packet in the gel height that the oil phase volume percentage that ovalbumin is prepared in different proteins amount concentration is 80%
Water emulsion has superior moldability and the design sketch of remoldability as shown in fig. 7, gained High Internal Phase Emulsion is in apparent gel, i.e.,
From syringe be transferred to desktop after lotion remain on lotion in complete cylindric or shearing homogenizing process directly with cylinder
Shape form is adhered to shearing machine head.And this gel High Internal Phase Emulsion has certain plasticity (with internal diameter 0.3cm's
Suction pipe can draw the small cylinder for being transferred out of a diameter of 0.3cm form stables from obtained emulsion system, and cross-lap exists
Small cylinder together cannot merge) and the remoldability (plastic injector for sealing the gel-like emulsion separated in injection orifice
In compression is pushed out together with air, you can complete the fusion again of gel-like emulsion), be suitable for following process.Visco elastic fluids
Become test result and again shows that gained lotion has stronger gel strength.When shearing frequency is 1Hz, the bullet of gained lotion
Property modulus first by 822Pa (a concentration of 0.04g/100g of ovalbumin quality), increasing to 1205Pa, (ovalbumin quality is a concentration of
0.32g/100g), then it is down to 932Pa (a concentration of 0.38g/100g of ovalbumin quality), finally increases to 1400Pa (ovalbumins
Mass concentration is 0.4g/100g).
The oil phase body that ovalbumin is prepared at a concentration of 0.16g/100g of albumen quality (for entire emulsion system)
Product percentage is outside drawing before and after the heat treatment of phase emulsion oil-in-water in 80% height and freeze thawing treatment as shown in figure 8, gained
The freeze-thaw stability that lotion has excellent thermal stability and is worth utilizing.By gained lotion (sample bottle strictly seals) boiling water bath
15min, ice bath 5min, makes its temperature be cooled to room temperature immediately after.The result shows that the emulsion gel intensity after heating obviously increases
Add.When shearing frequency is 1Hz, albumen quality concentration be respectively 0.04g/100g, 0.16g/100g, 0.28g/100g with
The elasticity modulus after lotion heating when 0.4g/100g is increased to by 760Pa, 1001Pa, 1311Pa and 1119Pa respectively successively
946Pa, 2013Pa, 4267Pa and 4410Pa.This illustrates that phase oil-in-water type is newborn in the novel protein stabilized gel height of gained
Liquid has the ability of the even thermotropic enhancing gel strength of excellent thermal stability.Gained lotion is freezed for 24 hours, so in -20 DEG C
Restore afterwards to room temperature in 25 DEG C of defrosting 4h to its temperature.Observation demulsification situation.Freeze thawing the result shows that, gained lotion is after freeze thawing one
It is secondary to be substantially completely demulsified.Therefore, phase emulsion oil-in-water can be used as inflammable and explosive or have in the protein stabilized gel height of gained
The storage of malicious organic liquid and transport agent, and when the organic liquid that is embedded is required, primary simple freeze thawing treatment
Regain organic liquid.And by first boiling water bath (15min), (ovalbumin is dense for ice bath (5min) treated high protein concentration afterwards
Degree is more than 0.6g/100) gel High Internal Phase Emulsion carry out identical freeze thawing treatment after, lotion keeps original appearance substantially
It with microscopic pattern, is not demulsified, freeze-thaw stability is good.
In addition, what ovalbumin was prepared when albumen quality concentration is down to 0.04g/100g (for entire emulsion system)
Outside drawing, light microscope of the phase emulsion oil-in-water before and after room temperature storage 60d in the height that oil phase volume percentage is 80%
Figure with viscoelastic rheometry shearing frequency scanning figure as shown in figure 9, in albumen quality concentration down to 0.04g/100g, when prepare
High Internal Phase Emulsion is after storing 60d, and appearance still keeps stable with microstructure, and gel strength is almost unchanged, this illustrates gained
Lotion has excellent bin stability.
Embodiment 5
According to the method for embodiment 4, prepare oil phase volume score be 80% protein stabilized height in phase oil-in-water type
Lotion.The difference is that albumen changes and makees casein sodium, haemocyanin, ovalbumin, lysozyme, beta lactoglobulin, beans 7S eggs
In vain, the freeze-drying sample or Sample Spray dry of beans 11S albumen, soybean protein isolate or whey protein isolate, albumen in lotion
Mass concentration is respectively 0.16g/100g, 0.28g/100g and 0.4g/100g, and oil phase is that (mass concentration is containing beta carotene
0.00 3g/100g) n-dodecane solution.By lotion (sample bottle strictly seal) of the gained containing beta carotene in dark place 95
DEG C water bath with thermostatic control 5h, to promote the oxidation and degradation of beta carotene.Lotion after heat treatment immediately ice bath make its temperature restore to
Room temperature, then freeze thawing treatment, draws the oil phase containing beta carotene from demulsification system.Using Their Determination by Spectrophotometry β-Hu
The Retention of radish element.
The result shows that after 95 DEG C of sealings are protected from light heat treatment 5h, it is embedded in the beta carotene loss pole in all gained lotions
Low, Retention is held in 98% or more；And the beta carotene loss not embedded by lotion equally handled is significantly higher, deposits
It is about 85.7% to stay rate.Therefore, in conjunction with the digestibility of animal/vegetable protein, phase oil-in-water in this novel protein stabilized height
Type lotion can be used as easily slow with air catalytic oxidation or the easily embedding of photodegradative oil-soluble bioactive substance and oral delivery
Carrier (oil phase must be changed to harmless organic solvent) is released, the storage that can significantly improve the bioactive substance that is embedded is stablized
Property, and realize and continue slow release in its human body.
Embodiment 6
According to the method for embodiment 4, prepare oil phase volume score be 80% protein stabilized height in phase oil-in-water type
Lotion.The difference is that albumen changes and makees casein sodium, haemocyanin, ovalbumin, lysozyme, beta lactoglobulin, beans 7S eggs
In vain, the freeze-drying sample or Sample Spray dry of beans 11S albumen, soybean protein isolate or whey protein isolate, albumen in lotion
Mass concentration is respectively 0.16g/100g, 0.28g/100g and 0.4g/100g, and oil phase is n-hexane.Gained lotion is placed in logical
In wind cupboard (sample bottle is open), in being stored at room temperature 2h, n-hexane is enable to volatilize.Then freeze thawing demulsification processing is carried out to lotion,
By the Retention for calculating n-hexane before homogeneous with emulsion system altitude difference method after demulsification.
The result shows that volatilization experiment after, n-hexane ovalbumin quality concentration be respectively 0.04g/100g,
The Retention in lotion when 0.16g/100g, 0.28g/100g and 0.4g/100g respectively may be about 95.3% successively, 96.2%,
97.6% and 98.6%；And the n-hexane in the oil water mixture without any emulsifier equally handled then volatilize it is more serious,
Its Retention is only about 56.2%.Therefore, in this novel protein stabilized high phase emulsion oil-in-water can be used as it is volatile
The occlusion vehicle of organic liquid can effectively inhibit its volatilization in conjunction with other seal approach, be conducive to its long-term storage and transport.
Embodiment 7
According to the method for embodiment 4, prepare oil phase volume score be 80% protein stabilized height in phase oil-in-water type
Lotion.The difference is that albumen changes and makees casein sodium, haemocyanin, ovalbumin, lysozyme, beta lactoglobulin, beans 7S eggs
In vain, the freeze-drying sample or Sample Spray dry of beans 11S albumen, soybean protein isolate or whey protein isolate, albumen in lotion
Mass concentration is respectively 0.16g/100g, 0.28g/100g and 0.4g/100g, and oil phase is lemon or Rosa Damascana.By institute
Lotion in 45 DEG C of constant temperature blast drying ovens plus promoting lemon volatilization (sample bottle open), stand the 14d times.In preceding 7d,
Lotion, which is taken out, every 12h carries out smell identification；Afterwards in 7d, then smell identification is carried out every taking-up lotion for 24 hours.
The result shows that in 14d, at 40 DEG C plus under the premise of promoting volatilization, lemon or Rosa Damascana are in gained lotion
It obtains slowly constantly discharging, each smell identification can smell apparent lemon smell or rose scent.And do not embed
Lemon or Rosa Damascana then volatilize comparatively fast, are almost smelt after 12d less than any smell, essential oil volume substantially reduces.Therefore, this
Phase emulsion oil-in-water can be used as embedding and the slow-released carrier of essential oil in kind novel protein stabilized height, realize essential oil it is long when
Between slow sustained release.
Embodiment 8
According to the method for embodiment 4, prepare oil phase volume score be 80% protein stabilized height in phase oil-in-water type
Lotion, unlike, albumen, which changes, makees soybean 7S globulin freeze-drying sample, kidney bean 7S albumen freeze-drying sample, soybean 11S albumen freeze-drying sample
Sample or whey protein isolate Sample Spray dry is lyophilized in product, soybean protein isolate, and albumen quality concentration is fixed as in lotion
0.2g/100g, and as in the protein solution of water phase respectively contain 0mmol/L, 50mmol/L, 100mmol/L, 200mmol/L
With the sodium chloride of 300mmol/L, oil phase is ready-mixed oil.
The result shows that after room temperature is protected from light and stands 2h, it can all be inverted and not flow.In all gel height of gained lotion
Phase emulsion.According to 4 the method for embodiment, the plasticity and remoldability of gained lotion are measured, the results showed that gained lotion has
There are good plasticity and remoldability, is suitable for following process.Viscoelastic rheometry test result shows with chlorination in water phase
Na concn (ionic strength) gradually increases, and the elasticity modulus of gained lotion first significantly rises rear slowly decline.The chlorination in water phase
Na concn is the elasticity modulus highest of lotion prepared by 50mmol/L or 100mmol/L, i.e. gel strength highest.According to embodiment
4 the methods measure the thermal stability of gained lotion, the results showed that gained lotion all has good thermal stability and coagulated with thermotropic
The strengthened characteristic of glue.According to 4 the method for embodiment, the freeze-thaw stability of gained lotion is measured.The result shows that in water phase
The lotion prepared when containing sodium chloride not less than 100mmol/L, regardless of whether carrying out first boiling water bath according to embodiment 4
(15min) ice bath (5min) is handled afterwards, and lotion all has good freeze-thaw stability, the appearance and microscopic pattern of lotion after freeze thawing
It is basically unchanged.Therefore, the solidifying of phase emulsion oil-in-water in this novel protein stabilized height can be improved in suitable ionic strength
Glue characteristic, machinability and freeze-thaw stability.In addition, gained lotion all has excellent bin stability, after storing 60d
Appearance still keeps stable with microstructure, and gel strength is almost unchanged.
Embodiment 9
According to the method for embodiment 4, prepare oil phase volume score be 80% protein stabilized height in phase oil-in-water type
Lotion, unlike, protein solution changes soybean 11S albumen (freeze-drying sample) solution, the beta lactoglobulin crossed as the pre-heat treatment and (freezes
Dry-eye disease) and soybean 11S albumen (freeze-drying sample) mixed solution (mass ratio 1:1) or xanthans (is lyophilized with soybean 11S albumen
Sample) mixed solution (mass ratio 1:19).Wherein, the pre-heat treatment of soybean 11S protein solutions, which operates, is：It is by mass concentration
The soybean 11S protein storage liquid boiling water bath 15min of 5g/100g, ice bath 5min, makes its temperature be cooled to room temperature immediately after.
The result shows that after room temperature is protected from light and stands 2h, it can all be inverted and not flow.In all gel height of gained lotion
Phase emulsion.According to 4 the method for embodiment, gained lotion correlation properties are measured, the results showed that gained lotion all has good
Gelation, plasticity and remoldability are suitable for following process；It is strong with heat-induced gel that gained lotion all has good thermal stability
Spend the characteristic of enhancing；When albumen quality concentration is more than 0.6g/100g, treated for ice bath (5min) afterwards for elder generation's boiling water bath (15min)
Lotion all has good freeze-thaw stability, and the freeze-thaw stability of gained lotion can be improved in the introducing (xanthans) of polysaccharide.In addition,
Gained lotion all has excellent bin stability, stores the appearance after 60d and still keeps stable, gel strength with microstructure
It is almost unchanged.Therefore the animals and plants in the protein stabilized height of this novel characteristic good in the water phase of phase emulsion oil-in-water
Whether albumen is not limited to simple the pre-heat treatment, it is not limited to the type of albumen, whether being not limited to the introducing of polysaccharide.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (9)
1. the preparation method of phase emulsion oil-in-water in a kind of protein stabilized height, it is characterised in that specific preparation process is as follows：
Albumen is dispersed in water, water phase protein solution is obtained after abundant aquation, oil phase emulsification is then added, directly obtains oil phase
Phase emulsion oil-in-water in protein stabilized height of the volumn concentration not less than 75%, or after lotion stratification under removal
Layer water phase obtains phase emulsion oil-in-water in protein stabilized height of the oil phase volume percentage composition not less than 75%；
The albumen is casein sodium, haemocyanin, ovalbumin, lysozyme, beta lactoglobulin, beans 7S albumen, beans
At least one of 11S albumen, soybean protein isolate or whey protein isolate；The oil phase is n-dodecane, contains β-carrot
At least one in the n-dodecane of element, n-hexane, lemon, Rosa Damascana, soybean oil, peanut oil, olive oil and ready-mixed oil
Kind.
2. the preparation method of phase emulsion oil-in-water, feature exist in a kind of protein stabilized height according to claim 1
In：Oil phase volume percentage composition is 75%~92% in phase emulsion oil-in-water in the protein stabilized height.
3. the preparation method of phase emulsion oil-in-water, feature exist in a kind of protein stabilized height according to claim 1
In：Oil phase volume percentage composition is 80%~92% in phase emulsion oil-in-water in the protein stabilized height.
4. according to the preparation method of phase emulsion oil-in-water in a kind of protein stabilized height of claims 1 to 3 any one of them,
It is characterized in that：Inorganic ion or polysaccharide are further added in the water phase protein solution.
5. according to the preparation method of phase emulsion oil-in-water in a kind of protein stabilized height of claims 1 to 3 any one of them,
It is characterized in that：The water phase protein solution emulsifies the heat pre-treatment that takes a step forward.
6. according to the preparation method of phase emulsion oil-in-water in a kind of protein stabilized height of claims 1 to 3 any one of them,
It is characterized in that：The mass concentration of albumen is 0.2%~5.0% in the water phase protein solution.
7. according to the preparation method of phase emulsion oil-in-water in a kind of protein stabilized height of claims 1 to 3 any one of them,
It is characterized in that：The emulsification refers to using in shearing emulsifying, ultrasonic emulsifying and high pressure microjet emulsifying
It is at least one.
8. the preparation method of phase emulsion oil-in-water, feature exist in a kind of protein stabilized height according to claim 7
In：The rotating speed of the shearing emulsifying is 2000~30000rpm, and the time is 0.5~3min；The ultrasound emulsifying
Power is 100~900W, and the intermittent time is 1~5s, and total time is 0.5~3min；The pressure of the high pressure microjet emulsifying
Power is 40~100MPa, and number of processes is 1~3 time.
9. phase emulsion oil-in-water in a kind of protein stabilized height, it is characterised in that：Described in any one of claim 1~8
Method be prepared.
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