CN107674247A - A kind of short amylose protein nano particle and its preparation method and application - Google Patents
A kind of short amylose protein nano particle and its preparation method and application Download PDFInfo
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- CN107674247A CN107674247A CN201710819045.5A CN201710819045A CN107674247A CN 107674247 A CN107674247 A CN 107674247A CN 201710819045 A CN201710819045 A CN 201710819045A CN 107674247 A CN107674247 A CN 107674247A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
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- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/275—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of animal origin, e.g. chitin
- A23L29/281—Proteins, e.g. gelatin or collagen
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- A—HUMAN NECESSITIES
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- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
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Abstract
The present invention relates to have technical field of nano material, there is provided a kind of short amylose protein nano particle and its preparation method and application.The present invention mixes short amylose solution and albumen, at 4 DEG C after 8~12h of retrogradation processing, centrifuges, freeze-drying, obtains short amylose protein nano particle；Wherein, the mass ratio of the short amylose butt and the albumen is 10:1~10:7.5.With the change of protein classes and ratio different patterns is presented, stability is good, gel structure enhancing, available for dietary gel modifying agent in the short amylose protein nano particle being prepared.
Description
Technical field
The present invention relates to technical field of nano material, specifically a kind of heterozygosis prepared using starch and albumen as raw material
Nano particle.
Background technology
Dietary gel modifying agent can improve the stickiness of food, improve dietary gel, so as to change the physical of food
Shape, assign the glutinous profit of food, suitable mouthfeel.The thickener kind that China ratifies to use at present has 39 kinds, is mostly some edible glues,
Price is of a relatively high.
For starch as cheap, wide material sources natural materials, stickiness is higher after gelatinization, is improving dietary gel
In terms of matter, there is huge market potential.However, starch gel has the shortcomings that not resistant to shearing, easy to aging, significantly limit
Application of the starch in terms of gel modifying agent.
The methods of by pre-gelatinized, damp and hot, xeothermic modification, chemical graft, the gel characteristic of starch can be improved, but it is general
The effect that logical physical method improves gel is not notable, and the method for chemical graft has potential safety hazard again.
The content of the invention
Present invention aims at provide a kind of nanometer of green safe, inexpensive short amylose and proteins Hybrid preparation
Particle and preparation method thereof, the nano particle of preparation can significantly improve starch gel structure and property, available for dietary gel
Modifying agent.
In order to solve the above-mentioned technical problem, technical scheme is as follows：
The invention provides a kind of preparation method of short amylose-protein nano particle, comprise the following steps：
The pH value for adjusting short amylose solution is 7.0~11.0；
The short amylose solution and albumen are mixed, 8~12h of retrogradation processing, centrifugation, will be centrifuged at 4~25 DEG C
Obtained sediment freeze-drying, obtains short amylose-protein nano particle；
Wherein, for the short amylose solution in terms of starch on dry basis, the mass ratio with the albumen is 10:1~10:7.5.
Preferably, the mass-volume concentration of the short amylose solution is 10~25%.
Preferably, after the short amylose solution is gelatinized by starch milk, it is prepared through digesting de- branch.
Mixed it is furthermore preferred that the starch milk is sodium dihydrogen phosphate-citrate buffer solution that starch is 4.0~5.5 with pH value
Conjunction is prepared.
It is furthermore preferred that the mass-volume concentration of the starch milk is 10~25%.
Preferably, the enzymolysis it is de- to draw enzyme be Pullulanase, the enzyme dosage is 5~15NPUN/g starch on dry basis；
The temperature of the de- branch of enzymolysis is 50~65 DEG C, and the time for digesting de- branch is 6~12h.
Preferably, the step of also including enzyme deactivation after the de- branch of the enzymolysis.
In the present invention, the albumen is the one or more in soybean protein isolate, rice protein and whey protein isolate.
Another object of the present invention is to provide short amylose-protein nano particle that the above method is prepared.
Another object of the present invention is to provide above-mentioned short amylose-protein nano particle in gel modifying agent
Using.
Compared with prior art, the present invention has advantages below：
Method provided by the invention prepares heterozygosis nano particle, system to short amylose nano particle situ addition albumen
Different patterns is presented with the change of protein classes and ratio in standby nano particle.Nano particle size and pattern and gel
Structure has direct relation.Nano level particle is easily fitted in the network structure of gel, forms the shape similar to gel node
State, so as to strengthen the intensity of gel.In terms of pattern, the structure unfolded is as flower-shaped structure, the spherical shape nanometer for the closure that compares
For particle, it is more beneficial for being wound in gel structure, strengthens the stability of gel structure.Short straight chain prepared by the present invention forms sediment
Powder-protein nano particle has higher heat endurance, suitable for food processing process.And the present invention is in short amylose nanometer
After particle situ addition native protein, had a better role for the gel structure tool of starch gelatinization liquid, main performance
In the elasticity enhancing of gel.The preparation condition of the present invention is gentle, and preparation process is green safe, and cost is low, is advantageous to industrial metaplasia
Production.
Brief description of the drawings
Fig. 1 is the transmission plot of the short amylose of different proportion-soybean protein isolate nano particle, wherein, formed sediment by short straight chain
The mass ratio meter of powder and soybean protein isolate, A.10:1, B.10:2.5, C.10:5, D.10:7.5；
Fig. 2 is the transmission plot of the short amylose of different proportion-rice protein protein nano particle, wherein, formed sediment by short straight chain
The mass ratio meter of powder and soybean protein isolate, A.10:1, B.10:2.5, C.10:5, D.10:7.5；
Fig. 3 is the transmission plot of the short amylose of different proportion-whey protein isolate nano particle, wherein, formed sediment by short straight chain
The mass ratio meter of powder and soybean protein isolate, A.10:1, B.10:2.5, C.10:5, D.10:7.5；
Fig. 4 is different short amylose-soybean protein isolate nano particles in angular frequency range 0.1-100rad/s, right
The influence of corn starch pasting liquid storage modulus (G')；
Fig. 5 is different short amylose-soybean protein isolate nano particles in angular frequency range 0.1-100rad/s, right
The influence of corn starch pasting liquid loss angle tangent (tan δ)；
Fig. 6 is different short amylose-rice protein nano particles in angular frequency range 0.1-100rad/s, to corn
The influence of starch gelatinization liquid storage modulus (G')；
Fig. 7 is different short amylose-rice protein nano particles in angular frequency range 0.1-100rad/s, to corn
The influence of starch gelatinization liquid loss angle tangent (tan δ)；
Fig. 8 is different short amylose-whey protein isolate nano particles in angular frequency range 0.1-100rad/s, right
The influence of corn starch pasting liquid storage modulus (G')；
Fig. 9 is different short amylose-whey protein isolate nano particles in angular frequency range 0.1-100rad/s, right
The influence of corn starch pasting liquid loss angle tangent (tan δ).
Embodiment
The invention provides a kind of preparation method of short amylose-protein nano particle, the nano particle of preparation can
Significantly improve starch gel structure and property.
Short amylose-protein nano preparation method of granules of the present invention comprises the following steps：
The pH value for adjusting short amylose solution is 7.0~11.0；
The short amylose solution and albumen are mixed, 8~12h of retrogradation processing at 4 DEG C, centrifugation, will be obtained after centrifugation
The sediment freeze-drying arrived, obtains short amylose-protein nano particle.
In the present invention, the mass-volume concentration of preferably described short amylose solution for 10~25%, more preferably 11~
15%.Under this concentration, the concentration of short amylose exceedes the critical point concentration (10%) of short amylose, but will not under this concentration
Form substantial amounts of aggregate and precipitate.Short amylose can either be dispersed in water well, while and can is enough self-assembled into starch and received
Rice grain, when adding a certain amount of albumen, heterozygosis nano particle can be self-assembled into.
Short amylose used in the present invention can use commercially available prod, by the short amylose short straight chain of formation soluble in water
Starch solution, for preparing short amylose-protein nano particle.
The short amylose of the present invention can also be prepared voluntarily.In an embodiment of the present invention, it is preferred to use enzymolysis
Method directly prepares short amylose solution.
As a preferred embodiment, after the short amylose solution of the present invention is gelatinized by starch milk, through digesting de- branch
It is prepared.
In the present invention, starch milk is to be mixed with to form with sodium dihydrogen phosphate-citrate buffer solution by starch.The present invention is right
The species of starch is not particularly limited, in the specific embodiment of the invention, it is preferred to use cornstarch (CS).The phosphoric acid of the present invention
Sodium dihydrogen-citric acid solution is used to maintain the constant of pH value of starch milk, prevents enzyme pH value in processing procedure from changing
Cause the reduction of enzymolysis efficiency.In the present invention, the pH value of the sodium dihydrogen phosphate-citrate buffer solution is preferably 4.0~5.5,
More preferably 4.6~5.0.Buffer solution under this pH value state is advantageous to keep the greater activity of enzyme, and it is de- to improve starch milk enzymolysis
Branch efficiency.In the present invention, the starch milk mass-volume concentration being preferably prepared is 10~25%, more preferably 15~20%,
In favor of digesting the progress of de- branch.
Starch milk is gelatinized.The present invention is not particularly limited to the method for starch milk gelatinization, using in this area
Conventional gelatinizing method.In the present invention, it is preferred to it is gelatinized using water-bath.The starch milk is subjected to water-bath, makes starch complete
Gelatinization.In the present invention, the temperature of water-bath is preferably 80~100 DEG C, more preferably 85~95 DEG C；Water-bath gelatinization time be preferably
30~60min, more preferably 40~50min.After gelatinization, starch granules swell, disintegration in starch milk, starch chain are unfolded,
Starch debranching enzymes could be in starch chain bifurcation cutoff process.
After the gelatinization, obtained gelatinized starch breast is preferably cooled to 55~60 DEG C by the present invention, to prevent the paste of high temperature
Changing starch reduces starch debranching enzymatic activity.
After obtaining gelatinized starch breast, the present invention carries out the gelatinized starch breast to digest de- branch, obtains short amylose.This
In invention, the enzymolysis is de-, and to draw enzyme be starch debranching enzymes, and the starch debranching enzymes are preferably Pullulanase.In the present invention, institute
The enzyme dosage for stating Pullulanase is 5~15NPUN/g starch on dry basis, more preferably 7~13NPUN/g starch on dry basis.
In the present invention, the temperature of the de- branch of enzymolysis is preferably 50~65 DEG C, more preferably 55~60 DEG C；The de- branch of enzymolysis
Time is preferably 6~12h, more preferably 7~9h.
Digest containing the different amylose of molecular weight, the present invention that obtained enzymolysis liquid is low while hot in obtained enzymolysis liquid
Speed centrifugation removes long linear starch, obtains short amylose.In the present invention, the rotating speed of low-speed centrifugal is preferably 2000~3000r/
Min, more preferably 2300~2800r/min；Centrifugation time is preferably 3~5min.After low-speed centrifugal, long linear starch is because of it
Molecular weight is larger, can precipitate, and short amylose molecule chain is short, and molecular weight is small, can be dispersed in supernatant.
After the low-speed centrifugal, obtained supernatant is preferably carried out enzyme deactivation by the present invention, obtains short amylose.The present invention
The method of enzyme deactivation is not particularly limited, it is preferred to use high temperature enzyme deactivation method is by starch debranching enzyme denaturation.Specifically, heat on described
Clear liquid is incubated 10~20min, enzyme is thoroughly lost activity to 90~100 DEG C.
After the enzyme deactivation, the present invention preferably sloughs obtained enzyme deactivation supernatant low-speed centrifugal the enzyme of denaturation, obtains short straight
Chain starch solution.In the present invention, the rotating speed of low-speed centrifugal is preferably 2000~3000r/min, more preferably 2300~2800r/
min；Centrifugation time is preferably 2~5min.The short amylose being prepared is scattered in supernatant.
The pH value of short amylose solution is adjusted to 7~11, so that the pH value of solution adapts to the needs of different protein dissolutions,
It is completely dissolved albumen.Such as when the protein is preferably soybean protein isolate, the pH value of corresponding short amylose solution
Preferably 10.0~11.0；When the protein is preferably rice protein, the pH value of corresponding short amylose solution is preferred
For 8.5~9.5；When the protein is preferably whey protein isolate, the pH value of corresponding short amylose solution is preferably
7.0~7.5.
The present invention is not particularly limited to the mode for adjusting the pH value of short amylose solution, can play the short straight chain of adjustment
The method of starch solution pH value is within protection scope of the present invention.Such as it is adjusted with sodium hydroxide, potassium hydroxide alkali.
The present invention is not particularly limited to the existence form of alkali, the alkali of solid or solution form.Such as it is adjusted using aqueous slkali,
It is preferred that the concentration of aqueous slkali is 0.01~1mol/L, more preferably 0.1~0.5mol/L.
Short amylose solution after adjustment pH value is mixed with albumen and carries out retrogradation processing.In processing procedure of bringing back to life,
The self assembly that short amylose and protein molecular carry out nano particle can occur, obtain heterozygosis nano particle.
In the present invention, the albumen includes but is not limited to soybean protein isolate (SPI), rice protein (RP) separates with whey
One or more in albumen (WPI).
In the present invention, the mass ratio of the short amylose butt and the albumen is 10:1~10:7.5, more preferably
10:1.5~10:5, further, the mass ratio of the short amylose butt and the albumen can independently be 10:1、
10:1.5、10:2、10:2.5、10:3、10:3.5、10:4、10:4.2、10:4.5、10:5、10:5.5、10:6、10:6.5、10:
7、10:7.5.With the further increase of protein ratio, the clustering phenomena increase of heterozygosis nano particle, the enhancing of gel structure is made
With more notable.
Protein and the pattern with the ratio regular meeting influence heterozygosis nano particle of short amylose.Such as soybean protein and short straight chain
Starch is compounded to form spherical nano particle, and ratio is less than 10:There is portion cavity structure in nano particle when 5, when ratio is more than
10:When 5, formation is solid nanosphere.Rice protein and short amylose are less than 10 in ratio:Formed when 2.5 spherical
Nano particle, and higher than 10:When 2.5, formation is flower-shaped nanostructured.Lactalbumin and short amylose are compound, are formed
Be stack lamellar structure, ratio be higher than 10:What is formed when 5 is irregular spherical nanoparticle.
In the present invention, the temperature of the retrogradation processing is preferably 4~25 DEG C, more preferably 4~10 DEG C.Retrogradation processing when
Between be preferably 8~12h, more preferably 9~11h.
After retrogradation processing, the present invention retrogradation is handled after solution centrifugal, after obtained sediment freeze-drying, obtain
To the solution containing short amylose-protein nano particle.
In the present invention, the rotating speed of the centrifugation is preferably 4000~6000r/min, more preferably 4500~5500r/min.
The present invention is preferably washed while centrifugation, to remove the impurity such as cushioning liquid or alkali.Specially will centrifugation solution and water
Mixing is centrifuged, and removes the supernatant of centrifugation.The present invention is not particularly limited to the volume of mixing water, is closed according to centrifugation situation
Reason sets washing water consumption.In the present invention, preferably washing is to centrifuge 1~3 times of liquor capacity with water volume.It is excellent in the present invention
It is 4~5 times to select washing times, and washing time is 10~20min/ times.
In the present invention, freeze-drying is preferably vacuum freeze drying.The temperature of the vacuum freeze drying is -86~-70
DEG C, more preferably -86 DEG C；The pressure of vacuum freeze drying is 0.1~1MPa, more preferably 0.1MPa；Vacuum freeze drying
Time is 48~72h, more preferably 72h.
After freeze-drying, short amylose-protein nano particle is obtained.The nano particle of preparation is with protein classes and ratio
The change of example, is presented different patterns, has higher heat endurance and stronger gel structure, can be used in gel improvement
Agent, such as the modifying agent of dietary gel.
For the object, technical solutions and advantages of the present invention are more clearly understood, the present invention is entered with reference to embodiment
Row detailed description, but they can not be interpreted as limiting the scope of the present invention.
Material therefor, reagent and instrument, the source of equipment, model and producer are as follows in the embodiment of the present invention：
Waxy corn starch：Heilongjiang Academy of Agricultural Sciences provides；
Pullulanase：Letter (China) Investment Co., Ltd of Novi provides；
Citric acid：Analyze pure；
Disodium hydrogen phosphate：Analyze pure；
Arabic gum：Tianjin Kai Xin chemical industry Co., Ltd；
Alpha-amylase：Sigma-Aldrich (Shanghai) trade Co., Ltd；
Soybean protein isolate, rice protein, whey protein isolate：Shandong Tianshen Bioprotein Co., Ltd.；
1 percent electronic balances (SPS401F)：Beijing Sai Duolisi instrument systems Co., Ltd；
Low speed large capacity centrifuge (DL-5-B)：Town in Shanghai booth instrument and equipment factory；
Ultrasonic cleaner (KQ-500B)：Kunshan Ultrasonic Instruments Co., Ltd.；
Vacuum freeze drier (ZDG-0.25)：Yantai Moon Co., Ltd.；
Transmission electron microscope (HT7700)：FDAC；
Ultraviolet specrophotometer (TU1810)：Beijing Puxi General Instrument Co., Ltd；
Differential scanning calorimeter (DSC1)：Mei Teletuo benefits International Trading Company Ltd of the U.S.；
Haier's refrigerator (BCD-215KS)：Qingdao HaiEr Co., Ltd；
Accurate pH meter：Shanghai Lei Ci instrument plants；
Embodiment 1
(1) cushioning liquid is prepared：Accurately weigh 3.27g disodium hydrogen phosphates and 2.24g citric acids are dissolved in 200mL distilled water
In, stirring makes it fully dissolve, stand-by；Prepare sodium dihydrogen phosphate-citrate buffer solution that pH is 4.8.
(2) general Shandong indigo plant enzyme pretreatment：Accurate to weigh 1350NPUN/mL, the general Shandong indigo plant enzymes of 1mL are instilled in 10mL distilled water, stirred
Mix and be allowed to be sufficiently mixed, it is stand-by；
(3) starch milk is prepared：Weigh 15g waxy corn starch to add in 100mL steps (1) cushioning liquid, be made 15%
Starch emulsion；
(4) it is gelatinized：By 95 DEG C of water-bath 50min of starch milk of preparation, starch is gelatinized completely, be then cooled to 50 DEG C.
(5) digest：The general Shandong indigo plant enzyme liquid that step (2) is handled well, enzyme liquid and starch are added into the colloidal solution after gelatinization
Ratio be 0.1mL/g starch on dry basis, 58 DEG C of enzymolysis 12h；
(6) low-speed centrifugal：Obtained enzymolysis liquid is centrifuged into 3min with 3000r/min rotating speed while hot, to remove long linear
Starch, obtain supernatant；
(7) enzyme deactivation：Continue the supernatant that heating stepses (6) obtain, elevate the temperature to 95 DEG C, keep 15min, make enzyme thorough
Bottom loses activity；Obtained feed liquid is centrifuged into 2min under 3000r/min after insulation, low-speed centrifugal sloughs the enzyme of denaturation, is made
Short amylose solution.
(8) pH is adjusted：The pH that short amylose solution is adjusted with 0.5mol/L sodium hydroxide solution is 11.0.
(9) self assembly prepares heterozygosis nano particle：Respectively according to 10:1、10:2.5、10:5、10:7.5 mass ratio (phase
For short amylose quality) soybean protein isolate is added in the short amylose solution that is obtained to step (8), in 4 DEG C next time
Raw processing 8h, obtains the solution containing heterozygosis nano particle；
(10) washing, vacuum freeze drying：The solution containing heterozygosis nano particle that step (9) is obtained is in 6000r/
Centrifugation washing 4-5 times, each 10min/ times under min.Sediment fraction vacuum freeze drying is obtained into short amylose-protein nano
Particle.
Embodiment 2
(1) cushioning liquid is prepared：Accurately weigh 3.27g disodium hydrogen phosphates and 2.24g citric acids are dissolved in 200mL distilled water
In, stirring makes it fully dissolve, stand-by；Prepare sodium dihydrogen phosphate-citrate buffer solution that pH is 5.0.
(2) general Shandong indigo plant enzyme pretreatment：Accurate to weigh 1350NPUN/mL, the general Shandong indigo plant enzymes of 1mL are instilled in 15mL distilled water, stirred
Mix and be allowed to be sufficiently mixed, it is stand-by；
(3) starch milk is prepared：Weigh 20g waxy corn starch to add in 100mL steps (1) cushioning liquid, be made 20%
Starch emulsion；
(4) it is gelatinized：By 80 DEG C of water-bath 60min of starch milk of preparation, starch is gelatinized completely, be then cooled to 57 DEG C
(5) digest：The general Shandong indigo plant enzyme liquid that step (2) is handled well, enzyme liquid and starch are added into the colloidal solution after gelatinization
Ratio be 0.2mL/g starch on dry basis, digest 8h at 60 DEG C；
(6) low-speed centrifugal：Obtained enzymolysis liquid is centrifuged into 3min with 2000r/min rotating speed while hot, to remove long linear
Starch, obtain supernatant；
(7) enzyme deactivation：Continue the supernatant that heating stepses (6) obtain, elevate the temperature to 100 DEG C, keep 10min, make enzyme
Thoroughly lose activity；Obtained feed liquid is centrifuged into 3min under 2000r/min after insulation, low-speed centrifugal sloughs the enzyme of denaturation, system
Obtain short amylose solution.
(8) pH is adjusted：The pH that short amylose solution is adjusted with 1mol/L sodium hydroxide solution is 9.0.
(9) self assembly prepares heterozygosis nano particle：Respectively according to 10:1、10:2.5、10:5、10:7.5 mass ratio (phase
For short amylose quality) rice protein is added in the short amylose solution that is obtained to step (8), at 4 DEG C at retrogradation
9h is managed, obtains the solution containing heterozygosis nano particle；
(10) washing, vacuum freeze drying：The solution containing heterozygosis nano particle that step (9) is obtained is in 5000r/
Centrifugation washing 4-5 times, each 20min under min.Sediment fraction vacuum freeze drying is obtained into short amylose-protein nano
Grain.
Embodiment 3
(1) cushioning liquid is prepared：Accurately weigh 3.27g disodium hydrogen phosphates and 2.24g citric acids are dissolved in 200mL distilled water
In, stirring makes it fully dissolve, stand-by；Prepare sodium dihydrogen phosphate-citrate buffer solution that pH is 4.5.
(2) general Shandong indigo plant enzyme pretreatment：Accurate to weigh 1350NPUN/mL, the general Shandong indigo plant enzymes of 1mL are instilled in 12mL distilled water, stirred
Mix and be allowed to be sufficiently mixed, it is stand-by；
(3) starch milk is prepared：Weigh 10g waxy corn starch to add in 100mL steps (1) cushioning liquid, be made 10%
Starch emulsion；
(4) it is gelatinized：By 90 DEG C of water-bath 40min of starch milk of preparation, starch is gelatinized completely, be then cooled to 55 DEG C.
(5) digest：The general Shandong indigo plant enzyme liquid that step (2) is handled well, enzyme liquid and starch are added into the colloidal solution after gelatinization
Ratio be 0.2mL/g starch on dry basis, 55 DEG C of enzymolysis 8h；
(6) low-speed centrifugal：Obtained enzymolysis liquid is centrifuged into 5min with 2000r/min rotating speed while hot, to remove long linear
Starch, obtain supernatant；
(7) enzyme deactivation：Continue the supernatant that heating stepses (6) obtain, elevate the temperature to 90 DEG C, keep 20min, make enzyme thorough
Bottom loses activity；Obtained feed liquid is centrifuged into 5min under 3000r/min after insulation, low-speed centrifugal sloughs the enzyme of denaturation, is made
Short amylose solution.
(8) pH is adjusted：The pH that short amylose solution is adjusted with 0.2mol/L sodium hydroxide solution is 7.0.
(9) self assembly prepares heterozygosis nano particle：Respectively according to 10:1、10:2.5、10:5、10:7.5 mass ratio (phase
For short amylose quality) whey protein isolate is added in the short amylose solution that is obtained to step (8), in 4 DEG C next time
Raw processing 8h, obtains the solution containing heterozygosis nano particle；
(10) washing, vacuum freeze drying：The solution containing heterozygosis nano particle that step (9) is obtained is in 6000r/
Centrifugation washing 4-5 times, each 20min under min.Sediment fraction vacuum freeze drying is obtained into short amylose-protein nano
Grain.
Embodiment 4
(1) cushioning liquid is prepared：Accurately weigh 3.27g disodium hydrogen phosphates and 2.24g citric acids are dissolved in 200mL distilled water
In, stirring makes it fully dissolve, stand-by；It is sodium dihydrogen phosphate-citrate buffer solution between 5.3 to prepare pH.
(2) general Shandong indigo plant enzyme pretreatment：Accurate to weigh 1350NPUN/mL, the general Shandong indigo plant enzymes of 1mL are instilled in 20mL distilled water, stirred
Mix and be allowed to be sufficiently mixed, it is stand-by；
(3) starch milk is prepared：Weigh 10g waxy corn starch to add in 100mL steps (1) cushioning liquid, be made 25%
Starch emulsion；
(4) it is gelatinized：By 100 DEG C of water-bath 30min of starch milk of preparation, starch is gelatinized completely, be then cooled to 65 DEG C；
(5) digest：The general Shandong indigo plant enzyme liquid that step (2) is handled well, enzyme liquid and starch are added into the colloidal solution after gelatinization
Ratio be 0.3mL/g starch on dry basis, 65 DEG C of enzymolysis 6h；
(6) low-speed centrifugal：Obtained enzymolysis liquid is centrifuged into 5min with 3000r/min rotating speed while hot, to remove long linear
Starch, obtain supernatant；
(7) enzyme deactivation：Continue the supernatant that heating stepses (6) obtain, elevate the temperature to 90 DEG C, keep 20min, make enzyme thorough
Bottom loses activity；Obtained feed liquid is centrifuged into 4min under 2000r/min after insulation, low-speed centrifugal sloughs the enzyme of denaturation, is made
Short amylose solution；
(8) pH is adjusted：The pH value that short amylose solution is adjusted with 0.5mol/L sodium hydroxide solution is 7.0.
(9) self assembly prepares heterozygosis nano particle：Respectively according to 10:1、10:2.5、10:5、10:7.5 mass ratio (phase
For short amylose quality) whey protein isolate is added in the short amylose solution that is obtained to step (8), in 4 DEG C next time
Raw processing 10h, obtains the solution containing heterozygosis nano particle；
(10) washing, vacuum freeze drying：The solution containing heterozygosis nano particle that step (9) is obtained is in 5000r/
Centrifugation washing 4-5 times, each 15min under min.Sediment fraction vacuum freeze drying is obtained into short amylose-protein nano
Grain.
Embodiment 5
The short amylose that embodiment 1~3 is prepared-protein nano particle 0.01g is scattered in 10ml ultra-pure waters,
Make its it is fully dispersed uniformly after, drop 0.1ml and siphons away unnecessary solution with filter paper on the copper mesh for supporting film with carbon, then
To the common drying of copper mesh, dried sample is put into transmission electron microscope system, vacuumizes 5min, accelerate electricity in 2kv
Pressure observation, takes pictures.As a result Fig. 1~3 are seen respectively.
Fig. 1 is the transmission plot of the short amylose of the different proportion of embodiment 1-soybean protein isolate nano particle.Can be with by Fig. 1
Find out, the mass ratio of the short straight chain of starch and soybean protein isolate is 10:When 1, heterozygosis nano particle is in have portion cavity not
Regular spherical, for particle diameter between 60-90nm, and with the increase of soybean protein isolate ratio, particle diameter has obvious reduction trend,
Particularly to 10:When 5, nano particle is between 10-20nm, although nano particle has certain clustering phenomena, between particle
It is not adhered phenomenon, favorable dispersibility significantly.In addition when ratio increases to 10:When 7.5, nano particle is in solid ball
Shape, and clustering phenomena is obvious.
Fig. 2 is the transmission plot of the short amylose of different proportion-rice protein nano particle in embodiment 2.It can be seen by Fig. 2
Go out, the mass ratio of the short straight chain of starch and rice protein is 10:When 1, the presentation of heterozygosis nano particle is irregular spherical, with albumen
The further increase of ratio, heterozygosis nanoparticle aggregate is into leaf shape, or even flower-shape.The flower it can be seen from enlarged drawing in Fig. 2 C
The nanostructured of shape is formed by many heterozygosis nano-particles self assembles.
Fig. 3 is the transmission plot of the short amylose of different proportion-whey protein isolate nano particle in embodiment 3.Can by Fig. 3
To find out, the mass ratio of the short straight chain of starch and rice protein is 10:1-10:When 5, the lamella knot stacked is presented in heterozygosis nano particle
Structure, there is the spheroid of many regular shapes in the lamellar structure of stacking it can be seen from enlarged drawing in Fig. 3 A, the piece that this explanation stacks
Rotating fields are the formation of heterozygosis nano-particles self assemble.When ratio increases to 10 it can be seen from Fig. 3 D:When 7.5, nano particle
Structure present irregular, aggregation is obvious spherical, and particle diameter is between 50-100nm.
Embodiment 6
Short amylose-influence of the protein nano particle to cornstarch rheological property
Cornstarch is gelatinized in water, prepares the corn starch pasting liquid that mass-volume concentration is 12%；
Starch nanometer granule (spheric granules for the 70-120nm that short amylose is self-assembly of) is mixed with water, prepared
Mass-volume concentration is 4% starch nanometer granule suspension；
Short amylose-protein nano particle that embodiment 1~3 is prepared mixes with water, and it is dense to prepare quality volume
Spend short amylose-protein nano particle suspension for 4%；
Above-mentioned corn starch pasting liquid is well mixed with starch nanometer granule suspension in 50 DEG C of volumetrics, what is obtained is mixed
Liquid is closed as a control group, by above-mentioned corn starch pasting liquid and short amylose-protein nano particle suspension in 50 DEG C of inferior bodies
Product is well mixed, and obtained mixed liquor is as test group.By above-mentioned mixed liquor at 25 DEG C, 0.5% (linear-viscoelastic of fixed strain
In area), perform a scan in angular frequency range 0.1-100rad/s.Obtain storage modulus (G') and loss angle tangent (tan δ
=G "/G') function as angular frequency.As a result as shown in Fig. 4~9：
Fig. 4~5 are the heterozygosis that in embodiment 1 prepared by different short amyloses (SLG), soybean protein isolate (SPI) ratio
Influence of the nano particle to cornstarch (CS) dextrin gelling properties.As seen from Figure 4, the storage of pure corn starch pasting liquid
For energy modulus between 30-40Pa, the storage modulus that with the addition of the corn starch pasting liquid of starch nanometer granule brings up to 47-60Pa
Between.And it with the addition of the dextrin storage modulus for the heterozygosis nano particle that the short amylose of the present invention is prepared with soybean protein isolate
Improve to 100-250Pa, it can be seen that the heterozygosis nano particle of the present invention has for corn starch pasting lyogel structure
Significant humidification, and as the increase of protein ratio, the heterozygosis nano particle of preparation are got over to the humidification of gel structure
Significantly.Similarly, as seen from Figure 5, as the increase of heterozygosis nano particle, the shearing loss angle of dextrin become in reduction
Gesture, it was demonstrated that its gel structure significantly increases.
Fig. 6~7 are the heterozygosis nanometer that in embodiment 2 prepared by different short amyloses (SLG), rice protein (RP) ratio
Influence of the grain to corn starch pasting lyogel property.As seen from Figure 6, the storage modulus of pure corn starch pasting liquid exists
Between 30-40Pa, the storage modulus that with the addition of the corn starch pasting liquid of starch nanometer granule is brought up between 47-60Pa.And
The dextrin storage modulus that with the addition of the heterozygosis nano particle that short amylose is prepared with rice protein is improved to 70-250Pa, by
This can be seen that the heterozygosis nano particle of the present invention has a significant humidification for corn starch pasting lyogel structure, and with
The increase of protein ratio, the heterozygosis nano particle of preparation is more notable to the humidification of gel structure.Similarly, can by Fig. 7
To find out, with the increase of heterozygosis nano particle, the shearing loss angle of dextrin is in reduction trend, it was demonstrated that its gel structure is notable
Enhancing.
Fig. 8~9 are the heterozygosis that in embodiment 3 prepared by different short amyloses (SLG), whey protein isolate (WPI) ratio
Influence of the nano particle to corn starch pasting lyogel property.As seen from Figure 8, the energy storage mould of pure corn starch pasting liquid
Amount between 30-40Pa, with the addition of the corn starch pasting liquid of starch nanometer granule storage modulus bring up to 47-60Pa it
Between.And the dextrin storage modulus that with the addition of the heterozygosis nano particle that short amylose is prepared with lactalbumin is improved to 80-
200Pa, it can be seen that heterozygosis nano particle of the present invention has significant enhancing to make for corn starch pasting lyogel structure
With, and as the increase of protein ratio, the heterozygosis nano particle of preparation are more notable to the humidification of gel structure.Similarly,
As seen from Figure 9, with the increase of heterozygosis nano particle, the shearing loss angle of dextrin is in reduction trend, it was demonstrated that its gel
Structure significantly increases.
Embodiment 7
Short amylose-protein nano particle thermal characteristics measure
Heterozygosis nanoparticle sample and the distilled water of the preparation of 9 ± 1mg embodiments 1~3 are weighed using mass ratio as 1：2 ratio
It is well mixed, well mixed sample is placed in aluminium crucible and balances 30min, is then risen with 10 DEG C/min speed
Temperature, temperature range are 25~120 DEG C, determine its T respectivelyo(initial temperature), Tp(peak temperature), Tc(final temperature) and enthalpy
The situation of change of (△ H).
The thermal characteristics of heterozygosis nano particle prepared by different short amyloses, soybean protein isolate ratio is shown in Table 1.By table 1
It can be seen that the gelatinization peak temperature of starch nanometer granule is at 89.92 DEG C, enthalpy 12.40J/g.And the short straight chain/soybean of starch
The peak value gelatinization point and enthalpy of protein isolate heterozygosis nano particle significantly improve, and with the increase of protein ratio, gelatinization temperature
Degree and enthalpy further improve.Especially when the ratio of the short straight chain of starch and soybean protein isolate is 10:When 5, nano particle
Peak value gelatinization point reaches 102.19 DEG C, and enthalpy also reaches and is up to 17.83J/g.And when ratio is further improved to 10:7.5
When, the heat endurance of heterozygosis nano particle has the trend of reduction.
The thermal characteristics of heterozygosis nano particle prepared by the different short amyloses of table 1, soybean protein isolate ratio
The thermal characteristics of heterozygosis nano particle prepared by different short amyloses, rice protein ratio is shown in Table 2.Can be with by table 2
Find out that the peak value gelatinization point of the short straight chain of starch-rice protein heterozygosis nano particle is less than pure starch nanometer granule, and with egg
The increase of white ratio, it is more obvious to reduce trend.This be probably due to the denaturation temperature of rice protein it is relatively low caused by.It is but miscellaneous
For the purer starch nanometer granule of enthalpy for closing nano particle, trend is significantly increased.But with increasing for protein ratio, its enthalpy
It is smaller to be worth value added.
The thermal characteristics of heterozygosis nano particle prepared by the different short amyloses of table 2, rice protein ratio
The thermal characteristics of heterozygosis nano particle prepared by different short amyloses, whey protein isolate ratio is shown in Table 3.By table 3
It can be seen that the peak value gelatinization point and enthalpy of the short straight chain of starch-whey protein isolate heterozygosis nano particle significantly improve, and with
The increase of protein ratio, gelatinization point and enthalpy further improve.Especially when the short straight chain of starch and whey protein isolate
Ratio is 10:When 5, the peak value gelatinization point of nano particle reaches 112.49 DEG C, and enthalpy also reaches and is up to 18.23J/g.And work as
Ratio is further improved to 10:When 7.5, the heat endurance of heterozygosis nano particle has the trend of reduction.
The thermal characteristics of heterozygosis nano particle prepared by the different short amyloses of table 3, whey protein isolate ratio
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of short amylose-protein nano particle, it is characterised in that comprise the following steps：
The pH value for adjusting short amylose solution is 7.0~11.0；
The short amylose solution and albumen are mixed, 8~12h of retrogradation processing, centrifugation, by the centrifugation at 4~25 DEG C
Obtained sediment freeze-drying, obtains short amylose-protein nano particle；
Wherein, for the short amylose solution in terms of starch on dry basis, the mass ratio with the albumen is 10:1~10:7.5.
2. preparation method according to claim 1, it is characterised in that the mass-volume concentration of the short amylose solution
For 10~25%.
3. preparation method according to claim 1, it is characterised in that the short amylose solution is gelatinized by starch milk
Afterwards, it is prepared through digesting de- branch.
4. preparation method according to claim 3, it is characterised in that the starch milk is starch and pH value is 4.0~5.5
Sodium dihydrogen phosphate-citrate buffer solution be mixed with and form.
5. the method according to claim 3 or 4, it is characterised in that the mass-volume concentration of the starch milk be 10~
25%.
6. the preparation method according to claim 3 or 4, it is characterised in that the enzymolysis is de-, and to draw enzyme be Pullulanase, institute
It is 5~15NPUN/g starch on dry basis to state enzyme dosage；The temperature of the de- branch of enzymolysis is 50~65 DEG C, and the time for digesting de- branch is
6~12h.
7. preparation method according to claim 3, it is characterised in that also include after the de- branch of enzymolysis：By the enzymolysis
The feed liquid enzyme deactivation that de- branch obtains.
8. preparation method according to claim 1, it is characterised in that the albumen is soybean protein isolate, rice protein
With the one or more in whey protein isolate.
9. short amylose-protein nano particle that claim 1~8 any one methods described is prepared.
10. short amylose described in claim 9-application of the protein nano particle in gel modifying agent.
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Cited By (3)
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| CN110606961A (en) * | 2019-07-15 | 2019-12-24 | 华南理工大学 | Starch nano particle with amphipathy and preparation method thereof |
| WO2021077380A1 (en) * | 2019-10-25 | 2021-04-29 | 合肥工业大学 | Bifunctional starch-based composite nanoparticle, preparation method therefor and use thereof |
| CN115777914A (en) * | 2022-09-30 | 2023-03-14 | 上海交通大学 | Slow release delivery carrier based on nutritional functional components embedded in debranched starch-zein composite particles and preparation method thereof |
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| CN106883463A (en) * | 2017-02-23 | 2017-06-23 | 青岛农业大学 | A kind of preparation method of pattern and size tunable type starch nanometer granule |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110606961A (en) * | 2019-07-15 | 2019-12-24 | 华南理工大学 | Starch nano particle with amphipathy and preparation method thereof |
| WO2021008171A1 (en) * | 2019-07-15 | 2021-01-21 | 华南理工大学 | Amphiphilic starch nanoparticles and preparation method therefor |
| CN110606961B (en) * | 2019-07-15 | 2022-03-29 | 华南理工大学 | Starch nano particle with amphipathy and preparation method thereof |
| WO2021077380A1 (en) * | 2019-10-25 | 2021-04-29 | 合肥工业大学 | Bifunctional starch-based composite nanoparticle, preparation method therefor and use thereof |
| CN115777914A (en) * | 2022-09-30 | 2023-03-14 | 上海交通大学 | Slow release delivery carrier based on nutritional functional components embedded in debranched starch-zein composite particles and preparation method thereof |
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