CN106832350B - The preparation method of the stable Pickering lotion of starch nanometer granule - Google Patents
The preparation method of the stable Pickering lotion of starch nanometer granule Download PDFInfo
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Abstract
The present invention relates to the preparation methods of Pickering lotion, the preparation method of especially a kind of Pickering lotion stable using starch nanometer granule emulsifier, including choosing the starch that amylose content is 20-40%, it is titrated after gelatinization with dehydrated alcohol, centrifugation, precipitating freeze-drying is obtained into starch nanometer granule, starch nanometer granule is added in oil-water mixture, Pickering lotion is prepared.The preparation method of the stable Pickering lotion of starch nanometer granule of the invention, raw material is natural, and preparation condition is mild, and without using strong corrosives reagents such as sulfuric acid, preparation process is environmentally protective, nontoxic, unharmful substance discharge；The Pickering lotion of preparation, stability is good, and sensitive environmental stability is good, has preferable heat-resisting and salt tolerance；A kind of efficient, environmentally protective starch nanometer granule preparation method is provided, edible cosmetic product and field of medicaments can be widely used in.
Description
Technical field
It is especially a kind of steady using starch nanometer granule emulsifier the present invention relates to the preparation method of Pickering lotion
The preparation method of fixed Pickering lotion.
Background technique
Pickering emulsion refers to using ultrafine particle as emulsion obtained from emulsifier, also referred to as
Pickering lotion.Pickering lotion compared with the stable lotion of conventional surfactant there is strong interface stability to subtract
Few bubble problem, it is renewable, less toxic, inexpensive the advantages that, in recent years, particle emulsifying agents are in terms of food, cosmetics and pharmacy
New opplication be concerned.Such as: the particle stabilizers such as silica, aluminium oxide, wax, clay particle, titanium oxide are extensive
Applied to Pickering lotion.However, the non-biodegradable and incompatibility due to these particles exceed food safety model
It encloses, so being restricted as application of the emulsifier in food.Some food compatibility particle stabilizers have been applied to
Pickering lotion, including nano-chitosan, Cellulose nanocrystal body, adipic crystals, protein, flavone compound also by
For O/W Pickering lotion.Although peptides and polysaccharide particle emulsifying agents have in terms of the stabilizing food colloid it is very big before
On the way, but this research it is shared in terms of food ratio it is still seldom.Thus, it is based on the effective colloidal particle of food grade ingredients
Production is still a more significant challenge on a large scale on food emulsifying agent field.
Starch is that a kind of important have biodegradability, renewable, good biocompatibility natural polysaecharides high
Molecular material, abundance is cheap, so having very big demand on food and biomedicine.Exist as emulsifier
Pickering lotion field has obtained certain applications.Since starch granules usually has high hydrophily, directly starch is made
For emulsifier use, the stability of emulsion of preparation is bad, and starch granules is usually carried out chemically or physically modified enhancing, and it is dredged
It is aqueous, starch granules is improved in the affinity of oil-water interfaces, such as: granulating is prepared by OSA (octenyl succinic acid anhydride) modification
Diameter is 1-5 μm of hydrophobized starch particle, needs to use sulfuric acid in this method, can generate a large amount of acid waste liquid, and make
Standby time-consuming more, the low output of process, the stability of emulsion prepared as emulsifier and stabilizer are poor.
Summary of the invention
It is acid it is an object of the invention to overcome above-mentioned starch granules emulsifier preparation process of the existing technology to generate
Waste liquid, time-consuming, low output provide a kind of preparation side of starch granules emulsifier with the defect of this stability of emulsion difference prepared
Method, preparation process is environmentally protective, and preparation method is simple, efficient, while providing and being prepared with this starch granules emulsifier
The stability of emulsion of the method for Pickering, preparation is high.
The present invention, which is that the following technical solution is employed, to be realized:
A kind of preparation method for the Pickering lotion that starch nanometer granule is stable, comprising the following steps:
(1) preparation of starch nanometer granule emulsifier: the starch that amylose content is 20-40% is chosen, adds water to be gelatinized, by nothing
Water-ethanol is added drop-wise in dextrin dropwise, while be added dropwise while stir, control blender revolving speed 500-1500rpm, after titration after
Continuous stirring 1-5h, suspension is centrifuged, and precipitating freeze-drying is obtained starch nanometer granule emulsifier；
(2) preparation of Pickering lotion: starch nanometer granule emulsifier being added in oil-water mixture and is mixed, control
The concentration of starch nanometer granule processed is 0.25-2wt%, and mixed liquor is used high-shear homogenizer extremely by 15-35 DEG C of the temperature of mixed liquor
It is uniformly distributed, Pickering lotion is made.
Above-mentioned technical proposal, further, the process of step (1) starch gelatinization are that starch is added water, starch concentration 3-
10wt%, boiling water water-bath are gelatinized 20-60min.
Above-mentioned technical proposal, further, the volume ratio of dextrin and dehydrated alcohol are 1:(1-5).
Above-mentioned technical proposal, further, the grease volume ratio of step (2) oil-water mixture are (1:3)-(3:1).
Above-mentioned technical proposal, further, the oil are mutually vegetable oil.
Above-mentioned technical proposal, further, the vegetable oil are selected from soybean oil, peanut oil, corn oil, sunflower oil, castor
One of sesame oil.
Above-mentioned technical proposal, it is further, mixed liquor is equal with the revolving speed of 10000-30000rmp using high-shear homogenizer
Matter 2-4 minutes.
Above-mentioned technical proposal, further, the average grain diameter of starch nanometer granule emulsifier made from step (1) is
50nm-700nm。
Above-mentioned technical proposal, further, the average grain diameter of starch nanometer granule emulsifier made from step (1) is
180nm-350nm。
Above-mentioned technical proposal, further, the starch are selected from cornstarch, sweet potato starch and tapioca.
The preparation method of the stable Pickering lotion of starch nanometer granule disclosed by the invention is prepared using alcohol method
The starch nanometer granule emulsifier of variety classes and different-grain diameter, raw material is natural, and preparation condition is mild, strong rotten without using sulfuric acid etc.
Corrosion reagent, preparation process is environmentally protective, nontoxic, unharmful substance discharge；The Pickering lotion of preparation, stability is good,
Sensitive environmental stability is good, has preferable heat-resisting and salt tolerance；Provide a kind of efficient, environmentally protective starch nanometer granule
Preparation method can be widely used in edible cosmetic product and field of medicaments.
Detailed description of the invention
Fig. 1 a is the transmission electron microscope picture of the different starch nanometer granules of embodiment 1；
Fig. 1 b is the grain size distribution of the different starch nanometer granules of embodiment 1；
Fig. 1 c is the three-phase contact angle figure of the different starch nanometer granules of embodiment 1；
Fig. 2 a is that the Pickering emulsion intercalation method of 2 variety classes starch nanometer granule of embodiment preparation observes figure；
Fig. 2 b is the microscope figure of the Pickering lotion of 2 variety classes starch nanometer granule of embodiment preparation；
Fig. 2 c is the laser co-focusing figure of the Pickering lotion of 2 variety classes starch nanometer granule of embodiment preparation；
Fig. 3 a is the starch nanometer granule grain size distribution of the different mixing speed preparations of embodiment 3；
Fig. 3 b is the three-phase contact angle figure of 3 sweet potato starch nano particle of embodiment；
Fig. 3 c is the three-phase contact angle figure of 3 cornstarch nano particle of embodiment；
Fig. 4 a is the Pickering emulsion intercalation method observation that 4 sweet potato starch nano particle of embodiment is emulsifier preparation
Figure；
Fig. 4 b is the Pickering emulsion intercalation method observation that 4 cornstarch nano particle of embodiment is emulsifier preparation
Figure；
Fig. 4 c is the microscope figure for the Pickering lotion that 4 sweet potato starch nano particle of embodiment is emulsifier preparation；
Fig. 4 d is the microscope figure for the Pickering lotion that 4 cornstarch nano particle of embodiment is emulsifier preparation；
Fig. 5 a is that the Pickering emulsion intercalation method of 5 sweet potato starch concentrations of nanoparticles of embodiment preparation observes figure；
Fig. 5 b is that the Pickering emulsion intercalation method of 5 cornstarch concentrations of nanoparticles of embodiment preparation observes figure；
Fig. 6 a is that the Pickering emulsion intercalation method of the different oil-water ratios of embodiment 6 observes figure；
Fig. 6 b is the microscope figure of the Pickering lotion of the different oil-water ratios of embodiment 6；
Fig. 7 a is influence of 7 different temperatures of embodiment to the size droplet diameter of Pickering lotion；
Fig. 7 b is Pickering emulsion intercalation method observation figure under 7 different temperatures of embodiment；
Fig. 7 c is influence of the different salt ionic concentrations of embodiment 7 to Pickering stability of emulsion；
Fig. 7 d is the micro- sem observation figure of Pickering lotion under the different salt ionic concentrations of embodiment 7.
Specific embodiment
In order to which the above objects, features and advantages of the present invention is more clearly understood, with reference to the accompanying drawing and implement
The present invention will be further described for example.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, still, the present invention may be used also
To be implemented using other modes described herein are different from, therefore, the present invention is not limited to following public specific embodiments.
Embodiment 1
Alcohol method prepares starch nanometer granule emulsifier: choosing cassava, sweet potato and cornstarch, respectively weighs 5g, divide respectively
It is scattered in 100ml water (starch concentration 5%), is then gelatinized 30min in boiling water water-bath, corn starch pasting liquid, sweet is made
Sweet potato starch dextrin and tapioca are gelatinized liquid.100ml dehydrated alcohol is taken respectively, is added drop-wise in above-mentioned three kinds of dextrins dropwise
(volume ratio of every kind of dextrin and dehydrated alcohol is 1:1) stirs when being added dropwise, and the revolving speed for controlling magnetic stirring apparatus is
1500rpm continues to stir 2h after titration, then suspension is centrifuged, and precipitating freeze-drying is obtained starch nanometer granule powder.Figure
1a is the transmission electron microscope picture of different starch nanometer granules, is corresponding in turn to tapioca nano particle from left to right, sweet potato starch is received
Rice grain and cornstarch nanometer.Fig. 1 b is the grain size distribution of different starch nanometer granules, is corresponding in turn to cassava from left to right
Starch nanometer granule, sweet potato starch nano particle and cornstarch nanometer.Fig. 1 c is in contact for the three of different starch nanometer granules
Angle figure is corresponding in turn to tapioca nano particle, sweet potato starch nano particle and cornstarch nano particle from left to right.It is different
The partial size of starch nanometer granule is shown in Table 1.
Fig. 1 a, 1b, 1c and table 1 illustrate that the cassava of the present embodiment, sweet potato, cornstarch nano particle, what is all had divides
Property is dissipated, and the three-phase contact angle of nano particle is all near 90 °.
Embodiment 2
What it is by soybean oil and water is that 1:1 is mixed with oil-water mixture according to volume ratio, takes three parts of oil-water mixtures respectively,
Every part is 100mL.Corn nano particle, sweet potato nano particle and tapioca nano particle prepared by example 1 will be applied and respectively take 1g,
Be added separately in the oil-water mixture of above-mentioned preparation, control mixed liquor temperature be 25 DEG C, using high-shear homogenizer with
Pickering lotion is made in the speed homogeneous of 10000rmp 2 minutes.Fig. 2 a is the preparation of variety classes starch nanometer granule
Pickering emulsion intercalation method observation figure is corresponding in turn to the stability sight for placing 0h, 1h, 3h, 1day and 7day from left to right
Examine figure；Fig. 2 b is the microscope figure of the Pickering lotion of variety classes starch nanometer granule preparation, is corresponding in turn to from left to right
The lotion of sweet potato starch nano particle, tapioca nano particle and cornstarch nanoparticles stable；Fig. 2 c is variety classes
The laser co-focusing figure of the Pickering lotion of starch nanometer granule preparation, is corresponding in turn to tapioca nanometer from left to right
Grain, sweet potato starch nano particle and cornstarch nano particle, the part indicated in figure between two arrows is starch nanometer granule
Thickness around emulsion droplets, it can be seen that starch nanometer granule is uniformly dispersed in around emulsion droplets, the stabilization formed
Property.It is herein including SPSNPs expression sweet potato starch nano particle in attached drawing, TSNPs expression tapioca nano particle, CSNPs
Indicate cornstarch nano particle.
Fig. 2 a, 2b, 2c and the explanation of table 1, the emulsification having been had using the lotion that these nano particles are prepared as emulsifier
Property, emulsification sex index is 18-22%.Microscope figure and laser co-focusing chart are bright, and nano particle can be uniformly dispersed in oil
The surface of drop forms lesser emulsion droplets.
Embodiment 3
By controlling blender revolving speed, the starch nanometer granule of different-grain diameter is prepared.Concrete operation method reference implementation example
1: it chooses sweet potato starch or cornstarch → being gelatinized respectively → and is added dropwise dehydrated alcohol, control blender revolving speed is respectively 300,
500,1000,1500 and 2000rpm → centrifugation → freeze-drying.Fig. 3 a is the starch nanometer granule partial size point of different mixing speeds preparation
Butut is corresponding in turn to sweet potato starch nano particle, cornstarch nano particle from left to right；Fig. 3 b is sweet potato starch nano particle
Three-phase contact angle figure, be corresponding in turn to from left to right blender revolving speed be 300,500,1000,1500 and 2000rpm under the conditions of make
Standby sweet potato starch nano particle；Fig. 3 c is the three-phase contact angle figure of cornstarch nano particle, is corresponding in turn to stirs from left to right
Mix the cornstarch nano particle prepared under the conditions of machine revolving speed is 300,500,1000,1500 and 2000rpm.Different mixing speeds
The cornstarch nano particle of lower preparation and the partial size of sweet potato starch nano particle are as shown in table 2.
The starch nanometer granule of different-grain diameter can be prepared by different rotating speeds, revolving speed is increased to by 300rmp
2000rmp, the dispersibility that obtained nano particle diameter is reduced to 50nm by 700, and has had.
Embodiment 4
The starch nanometer granule of different-grain diameter prepared by embodiment 3 is prepared into Pickering lotion, concrete operations side respectively
Method reference implementation example 2.Fig. 4 a is the Pickering emulsion intercalation method observation that sweet potato starch nano particle is emulsifier preparation
Figure；Fig. 4 b is the Pickering emulsion intercalation method observation figure that cornstarch nano particle is emulsifier preparation；Fig. 4 c is sweet potato
Starch nanometer granule is the microscope figure of the Pickering lotion of emulsifier preparation；Fig. 4 d is that cornstarch nano particle is cream
The microscope figure of the Pickering lotion of agent preparation.In above each figure, the corresponding emulsifier particle of label A, B, C, D and E
Diameter is successively about 710,340,220,180 and 50nm；A, the corresponding emulsifier grain diameter of b, c, d and e successively be about 680,
320,220,190 and 60nm.
With the increase of partial size, the contact angle of nano particle is gradually increased, and partial size is the starch nanometer granule of 100-200nm
Contact angle near 90 °.By measurement and the micro- sem observation of stability of emulsion it is found that partial size is the starch of 100-200nm
The emulsibility that the Pickering of nanoparticles stable has had.The oil droplet of formation is smaller.So the partial size of nano particle will affect
Emulsion intercalation method.
Embodiment 5
The method of reference implementation example 2 prepares oil water mixture, and sweet potato starch nano particle is added in oil water mixture,
The concentration for controlling sweet potato starch nano particle is respectively 0,0.25%, 0.5%, 1% and 2%, prepares Pickering lotion.Figure
5a is that the Pickering emulsion intercalation method of sweet potato starch concentrations of nanoparticles preparation observes figure, in figure 0h, 1h, 1day and
7day represents the resting period；Fig. 5 b is that the Pickering emulsion intercalation method of cornstarch concentrations of nanoparticles preparation observes figure.
The above two width figure label 0,0.25%, 0.5%, 1% and 2%, respectively indicates the concentration of starch nanometer granule.With nanometer
Grain concentration increases to 2% from 0, and emulsion intercalation method dramatically increases.
Embodiment 6
It is respectively 1:3,2:3,1:1 that the method for reference implementation example 2, which prepares grease volume ratio, the oil water mixture of 3:2,3:1,
Sweet potato starch nano particle is added in above-mentioned oil water mixture, the concentration of control sweet potato starch nano particle is 1%, respectively
Prepare Pickering lotion.Fig. 6 a is that the Pickering emulsion intercalation method observation of different oil-water ratios is schemed, digital 0.75 in figure,
0.6,0.5,0.4,0.25 oil number is respectively indicated.Fig. 6 b is the microscope figure of the Pickering lotion of different oil-water ratios, from a left side
The mixture grease volume ratio being corresponding in turn to the right side is respectively 1:3,2:3,1:1,3:2,3:1.When the concentration of starch nanometer granule
When being 1%, oil-water ratio increases to 3:1 from 1:3, and emulsibility first increases to be reduced afterwards, and when oil-water ratio is 1:1, emulsibility is most strong.
Embodiment 7
The sensitive environment (salt ion, temperature etc.) of the stable Pickering lotion of starch nanometer granule is tested.
1. freshly prepared sweet potato starch concentrations of nanoparticles is 1% by the preparation method of reference implementation example 5
Pickering lotion is respectively put into 25,40,60 and 90 DEG C of water-bath and heats 30min, places into the environment of room temperature and stores up
It deposits, the influence by bottle or microscope observation analysis temperature to stability of emulsion.Fig. 7 a is different temperatures to Pickering cream
The influence of the size droplet diameter of liquid, abscissa are heating time (min), and ordinate is the partial size (μm) of emulsion droplets.Fig. 7 b is difference
At a temperature of Pickering emulsion intercalation method observation figure.The temperature of lotion increases to 90 DEG C by 25 DEG C, and emulsion droplets become larger, but does not have
It is destroyed.
2. the preparation method of reference implementation example 6 weighs the mixed liquor of a certain amount of starch nanometer granule from different oil-water ratios
In, preparing grease volume ratio is respectively 1:3,2:3,1:1, and the oil water mixture of 3:2,3:1 weigh a certain amount of sweet potato starch and receives
Rice grain is added to above-mentioned oil mixing with water species, and the concentration of control sweet potato starch nano particle is 1%, meanwhile, respectively to mixing
Sodium chloride is added in liquid, control salt ionic concentration is 0,10,30,60 and 90mM, and mixed liquor is used high-shear homogenizer
10000rmp homogeneous 2 minutes, can obtain Pickering lotion.Fig. 7 c is that different salt ionic concentrations are steady to Pickering lotion
It qualitatively influences, Fig. 7 d is the micro- sem observation figure of Pickering lotion under different salt ionic concentrations, is corresponding in turn to from left to right
Salt ionic concentration be 0,10,30,60 and 90mM.In the range of salt ionic concentration is 10-90mM, emulsion intercalation method does not have
It is significant to change.
It is above-mentioned experiments have shown that illustrating the heat-resisting and salt tolerance that the stable lotion of such starch nanometer granule has had.
Table 1
Table 2
PDI indicates polymer dispersity index in above-mentioned table, and PDI is bigger, indicates that molecular weight distribution is wider；PDI is smaller, table
Show that molecular weight distribution is more uniform.
CI indicates that emulsification sex index is the ratio of bottom whey height and lotion total height, and CI is smaller, indicates that emulsibility is got over
It is good.
Embodiment described above is only that preferred embodiments of the present invention will be described, not to the scope of the present invention
It is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical solution of the present invention
The various changes and improvements made should all be fallen into the protection scope that claims of the present invention determines.
Claims (10)
1. a kind of preparation method for the Pickering lotion that starch nanometer granule is stable, which comprises the following steps:
(1) preparation of starch nanometer granule emulsifier: the starch that amylose content is 20-40% is chosen, adds water to be gelatinized, by anhydrous second
Alcohol is added drop-wise in dextrin dropwise, is stirred when being added dropwise, and is controlled blender revolving speed 500-1500rpm, is continued to stir after titration
1-5h is mixed, suspension is centrifuged, precipitating freeze-drying obtains starch nanometer granule emulsifier；
(2) preparation of Pickering lotion: starch nanometer granule emulsifier being added in oil-water mixture and is mixed, and control is formed sediment
The concentration of powder nano particle is 0.25-2wt%, and mixed liquor is used high-shear homogenizer homogeneous by 15-35 DEG C of the temperature of mixed liquor,
Pickering lotion is made.
2. the preparation method of the stable Pickering lotion of starch nanometer granule according to claim 1, feature exist
In the process of step (1) starch gelatinization is that starch is added to water, and starch concentration 1-5wt%, boiling water water-bath is gelatinized 20-60min.
3. the preparation method of the stable Pickering lotion of starch nanometer granule according to claim 2, feature exist
In the volume ratio of dextrin and dehydrated alcohol is 1:(1-5).
4. the preparation method of the stable Pickering lotion of starch nanometer granule according to claim 3, feature exist
In the grease volume ratio of step (2) oil-water mixture is (1:3)-(3:1).
5. the preparation method of the stable Pickering lotion of starch nanometer granule according to claim 4, feature exist
In the oil in the oil-water mixture is mutually vegetable oil.
6. the preparation method of the stable Pickering lotion of starch nanometer granule according to claim 5, feature exist
In the vegetable oil is selected from one of soybean oil, peanut oil, corn oil, sunflower oil, castor oil.
7. the preparation method of the stable Pickering lotion of starch nanometer granule according to claim 6, feature exist
In, by mixed liquor using high-shear homogenizer with the revolving speed of 10000-30000rpm, homogeneous 2-4 minutes.
8. the preparation method of the stable Pickering lotion of starch nanometer granule according to claim 1-7,
It is characterized in that, the average grain diameter of starch nanometer granule emulsifier made from step (1) is 50nm-700nm.
9. the preparation method of the stable Pickering lotion of starch nanometer granule according to claim 8, feature exist
In the average grain diameter of starch nanometer granule emulsifier made from step (1) is 180nm-350nm.
10. the preparation method of the stable Pickering lotion of starch nanometer granule according to claim 1-7,
It is characterized in that, the starch is selected from cornstarch, sweet potato starch and tapioca.
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| CN108434010B (en) * | 2018-06-06 | 2020-10-20 | 西南交通大学 | Pickering emulsion type cosmetic with stable SOD enzyme particles and preparation process thereof |
| CN110003498B (en) * | 2019-03-21 | 2020-07-07 | 江南大学 | Edible pickering emulsion and preparation method thereof |
| CN109938327B (en) * | 2019-04-03 | 2022-04-29 | 东北农业大学 | Method for preparing fat substitute by regulating and controlling aggregation of oil drops in emulsion through cassava starch |
| CN109938328B (en) * | 2019-04-03 | 2022-04-29 | 东北农业大学 | Method for preparing fat substitute by regulating and controlling oil drop aggregation in emulsion through flaxseed gum |
| CN110506930B (en) * | 2019-07-17 | 2022-06-14 | 华南理工大学 | Starch-based high-stability Pickering emulsion and preparation method thereof |
| CN111000799B (en) * | 2019-12-31 | 2021-11-30 | 青岛农业大学 | Curcumin Pickering emulsion with colon-targeted delivery function and preparation method and application thereof |
| CN111116941B (en) * | 2019-12-31 | 2022-07-01 | 镇江市智农食品有限公司 | Preparation method of nano-starch-based Pickering emulsion |
| CN111905642B (en) * | 2020-09-14 | 2021-08-31 | 山东大学 | Pickering emulsion based on mung bean extracted particles and preparation method and application thereof |
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