CN106832350A - The preparation method of the Pickering emulsions of starch nanometer granule stabilization - Google Patents
The preparation method of the Pickering emulsions of starch nanometer granule stabilization Download PDFInfo
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Abstract
The present invention relates to the preparation method of Pickering emulsions, a kind of especially preparation method of the Pickering emulsions of use starch nanometer granule emulsifying agent stabilization, including choosing the starch that amylose content is 20 40%, titrated with absolute ethyl alcohol after gelatinization, centrifugation, precipitation is freezed and obtains starch nanometer granule, starch nanometer granule is added in oil-water mixture, prepare Pickering emulsions.The preparation method of the Pickering emulsions of starch nanometer granule stabilization of the invention, raw material is natural, and preparation condition is gentle, and the severe corrosive reagent such as sulfuric acid is not used, preparation process environmental protection, nontoxic, unharmful substance discharge；The Pickering emulsions of preparation, good stability, sensitive environment good stability, with preferable heat-resisting and salt tolerance；There is provided a kind of starch nanometer granule preparation method of efficient, environmental protection, 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 emulsifying agent the present invention relates to the preparation method of Pickering emulsions
The preparation method of fixed Pickering emulsions.
Background technology
Pickering emulsion refers to the emulsion using obtained from ultrafine particle as emulsifying agent, also referred to as
Pickering emulsions.Pickering emulsions subtract compared with the emulsion of conventional surfactant stabilization with strong interface stability
The advantages of few bubble problem, renewable, low toxicity, low cost, in recent years, particle emulsifying agents are in terms of food, cosmetics and pharmacy
New opplication receive much concern.For example：The particle stabilizers such as silica, aluminum oxide, wax, clay particle, titanium oxide are extensive
It is applied to Pickering emulsions.However, because the non-biodegradable and incompatibility of these particles exceed food security model
Enclose, application as emulsifying agent in food be restricted.Some food compatibility particle stabilizers have been applied to
Pickering emulsions, including nano-chitosan, Cellulose nanocrystal body, adipic crystals, protein, flavone compound also by
For O/W Pickering emulsions.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 shared in terms of food ratio of research is still little.Thus, based on the effective colloidal particle of food grade ingredients
Large-scale making is still a more significant challenge on food emulsifying agent field.
Starch is important high with biodegradability, renewable, good biocompatibility natural polysaecharides of a class
Molecular material, abundance is cheap, so having very big demand on food and biomedicine.Exist as emulsifying agent
Pickering emulsions field has obtained certain applications.Because starch granules generally has hydrophily high, directly starch is made
For emulsifying agent is used, the stability of emulsion of preparation is bad, typically by starch granules chemically or physically be modified enhancing its dredge
It is aqueous, affinity of the starch granules in oil-water interfaces is improved, for example：Granulating is prepared by the way that OSA (octenyl succinic acid anhydride) is modified
Footpath is 1-5 μm of hydrophobized starch particle, needs to use sulfuric acid in this method, can produce substantial amounts of acid waste liquid, and make
Standby process is time-consuming more, yields poorly, and the stability of emulsion prepared as emulsifying agent and stabilizer is poor.
The content of the invention
Above-mentioned starch granules emulsifier preparation process it is an object of the invention to overcome prior art to exist produces acid
Waste liquid, take, yield poorly, with the defect of this stability of emulsion difference for preparing, there is provided a kind of preparation side of starch granules emulsifier
Method, preparation process environmental protection, preparation method is simple, efficient, while provide being prepared with this starch granules emulsifier
The method of Pickering, the stability of emulsion of preparation is high.
The present invention is realized using following technical scheme：
A kind of preparation method of the Pickering emulsions of starch nanometer granule stabilization, comprises the following steps：
(1) preparation of starch nanometer granule emulsifying agent：It is the starch of 20-40% to choose amylose content, and add water gelatinization, by nothing
Water-ethanol is dropwise added drop-wise in dextrin, is stirred when being added dropwise, and controls mixer rotating speed 500-1500rpm, and titration terminates follow-up
Continuous stirring 1-5h, suspension is centrifuged, and precipitation is freezed and obtains starch nanometer granule emulsifying agent；
(2) preparation of Pickering emulsions：Starch nanometer granule emulsifying agent is 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 emulsions is obtained.
Above-mentioned technical proposal, further, the process of step (1) starch gelatinization is that starch adds water, and starch concentration is 3-
10wt%, boiling water water-bath gelatinization 20-60min.
Above-mentioned technical proposal, further, dextrin is 1 with the volume ratio of absolute ethyl alcohol：(1-5).
Above-mentioned technical proposal, further, the profit volume ratio of step (2) oil-water mixture is (1:3)-(3:1).
Above-mentioned technical proposal, further, the oil phase is vegetable oil.
Above-mentioned technical proposal, further, the vegetable oil is selected from soybean oil, peanut oil, corn oil, sunflower oil, castor
One kind in sesame oil.
Above-mentioned technical proposal, it is further, mixed liquor is equal with the rotating 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 emulsifying agent is obtained in step (1)
50nm-700nm。
Above-mentioned technical proposal, further, the average grain diameter of starch nanometer granule emulsifying agent is obtained in step (1)
180nm-350nm。
Above-mentioned technical proposal, further, the starch is selected from cornstarch, sweet potato starch and tapioca.
The preparation method of the Pickering emulsions of starch nanometer granule stabilization disclosed by the invention, is prepared using alcohol method
The starch nanometer granule emulsifying agent of variety classes and different-grain diameter, raw material is natural, and preparation condition is gentle, does not use sulfuric acid etc. strong rotten
Corrosion reagent, preparation process environmental protection, nontoxic, unharmful substance discharge；The Pickering emulsions of preparation, good stability,
Sensitive environment good stability, with preferable heat-resisting and salt tolerance；There is provided a kind of starch nanometer granule of efficient, environmental protection
Preparation method, can be widely used in edible cosmetic product and field of medicaments.
Brief description of the drawings
Fig. 1 a are the transmission electron microscope picture of the different starch nanometer granules of embodiment 1；
Fig. 1 b are the grain size distribution of the different starch nanometer granules of embodiment 1；
Fig. 1 c are the three-phase contact angle figure of the different starch nanometer granules of embodiment 1；
Fig. 2 a are Pickering emulsion intercalation methods observation figure prepared by the variety classes starch nanometer granule of embodiment 2；
Fig. 2 b are the microscope figure of Pickering emulsions prepared by the variety classes starch nanometer granule of embodiment 2；
Fig. 2 c are the laser co-focusing figure of Pickering emulsions prepared by the variety classes starch nanometer granule of embodiment 2；
Fig. 3 a are starch nanometer granule grain size distribution prepared by the different mixing speeds of embodiment 3；
Fig. 3 b are the three-phase contact angle figure of the sweet potato starch nano particle of embodiment 3；
Fig. 3 c are the three-phase contact angle figure of the cornstarch nano particle of embodiment 3；
Fig. 4 a are that the sweet potato starch nano particle of embodiment 4 is that Pickering emulsion intercalation methods prepared by emulsifying agent are observed
Figure；
Fig. 4 b are that the cornstarch nano particle of embodiment 4 is that Pickering emulsion intercalation methods prepared by emulsifying agent are observed
Figure；
Fig. 4 c are the microscope figure that the sweet potato starch nano particle of embodiment 4 is Pickering emulsions prepared by emulsifying agent；
Fig. 4 d are the microscope figure that the cornstarch nano particle of embodiment 4 is Pickering emulsions prepared by emulsifying agent；
Fig. 5 a are Pickering emulsion intercalation methods observation figure prepared by the sweet potato starch concentrations of nanoparticles of embodiment 5；
Fig. 5 b are Pickering emulsion intercalation methods observation figure prepared by the cornstarch concentrations of nanoparticles of embodiment 5；
Fig. 6 a are the Pickering emulsion intercalation methods observation figure of the different oil-water ratios of embodiment 6；
Fig. 6 b are the microscope figure of the Pickering emulsions of the different oil-water ratios of embodiment 6；
Fig. 7 a are influence of the different temperatures of embodiment 7 to the size droplet diameter of Pickering emulsions；
Fig. 7 b are Pickering emulsion intercalation methods observation figure under the different temperatures of embodiment 7；
Fig. 7 c are influence of the different salt ionic concentrations of embodiment 7 to Pickering stability of emulsion；
Fig. 7 d are the micro- sem observation figure of Pickering emulsions under the different salt ionic concentrations of embodiment 7.
Specific embodiment
In order to be more clearly understood from the above objects, features and advantages of the present invention, below in conjunction with the accompanying drawings and implement
The present invention will be further described for example.
Many details are elaborated in the following description in order to fully understand the present invention, but, the present invention may be used also
To be implemented using other modes described here are different from, therefore, the present invention is not limited to following public specific embodiment.
Embodiment 1
Alcohol method prepares starch nanometer granule emulsifying agent：Cassava, sweet potato, and cornstarch are chosen, 5g is respectively weighed, divided respectively
It is scattered in 100ml water (starch concentration is 5%), then be gelatinized 30min in boiling water water-bath, corn starch pasting liquid, sweet is obtained
Sweet potato starch dextrin and tapioca dextrin.100ml absolute ethyl alcohols are taken respectively, are dropwise added drop-wise in above-mentioned three kinds of dextrins
(every kind of dextrin is 1 with the volume ratio of absolute ethyl alcohol:1), stirred when being added dropwise, the rotating speed for controlling magnetic stirring apparatus is
1500rpm, titration continues to stir 2h after terminating, then suspension is centrifuged, and precipitation is freezed and obtains starch nanometer granule powder.Figure
1a is the transmission electron microscope picture of different starch nanometer granules, tapioca nano particle, sweet potato starch is corresponding in turn to from left to right and is received
Rice grain and cornstarch nanometer.Fig. 1 b are the grain size distribution of different starch nanometer granules, and cassava is corresponding in turn to from left to right
Starch nanometer granule, sweet potato starch nano particle and cornstarch nanometer.Fig. 1 c are the three of different starch nanometer granules to be in contact
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 particle diameter 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 all divide with good
Dissipate property, and nano particle three-phase contact angle all near 90 °.
Embodiment 2
According to volume ratio it is 1 by soybean oil and water:1 is mixed with oil-water mixture, and three parts of oil-water mixtures are taken 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 takes 1g,
Be added separately in the oil-water mixture of above-mentioned preparation, control the temperature of mixed liquor for 25 DEG C, using high-shear homogenizer with
The speed homogeneous of 10000rmp 2 minutes, is obtained Pickering emulsions.Fig. 2 a are prepared by variety classes starch nanometer granule
Pickering emulsion intercalation methods 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 are the microscope figure of Pickering emulsions prepared by variety classes starch nanometer granule, are corresponding in turn to from left to right
The emulsion of sweet potato starch nano particle, tapioca nano particle and cornstarch nanoparticles stable；Fig. 2 c are variety classes
The laser co-focusing figure of Pickering emulsions prepared by starch nanometer granule, is corresponding in turn to tapioca nanometer from left to right
Grain, sweet potato starch nano particle and cornstarch nano particle, the part indicated between two arrows in figure are starch nanometer granule
Thickness around emulsion droplets, it can be seen that starch nanometer granule is uniformly dispersed in around emulsion droplets, the stabilization for having been formed
Property.SPSNPs represents sweet potato starch nano particle in including accompanying drawing herein, and TSNPs represents tapioca nano particle, CSNPs
Represent cornstarch nano particle.
Fig. 2 a, 2b, 2c and table 1 illustrate, the emulsification having been had as emulsion prepared by emulsifying agent using these nano particles
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 less emulsion droplets.
Embodiment 3
By controlling mixer rotating speed, the starch nanometer granule of different-grain diameter is prepared.Concrete operation method reference implementation example
1：Choose sweet potato starch or cornstarch → be gelatinized respectively → be added dropwise absolute ethyl alcohol, control mixer rotating speed is respectively 300,
500th, 1000,1500 and 2000rpm → centrifugation → lyophilized.Fig. 3 a are starch nanometer granule particle diameter point prepared by different mixing speeds
Butut, is corresponding in turn to sweet potato starch nano particle, cornstarch nano particle from left to right；Fig. 3 b are sweet potato starch nano particle
Three-phase contact angle figure, mixer rotating speed is corresponding in turn to from left to right to make under the conditions of 300,500,1000,1500 and 2000rpm
Standby sweet potato starch nano particle；Fig. 3 c are the three-phase contact angle figure of cornstarch nano particle, be corresponding in turn to stir from left to right
The machine rotating speed of mixing is the cornstarch nano particle of preparation under the conditions of 300,500,1000,1500 and 2000rpm.Different mixing speeds
The cornstarch nano particle of lower preparation and the particle diameter 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, rotating speed is increased to by 300rmp
2000rmp, the nano particle diameter for obtaining is reduced to 50nm by 700, and with good dispersiveness.
Embodiment 4
The starch nanometer granule of different-grain diameter prepared by embodiment 3 prepares Pickering emulsions, concrete operations side respectively
Method reference implementation example 2.Fig. 4 a are that sweet potato starch nano particle is that Pickering emulsion intercalation methods prepared by emulsifying agent are observed
Figure；Fig. 4 b are that cornstarch nano particle is that Pickering emulsion intercalation methods observation prepared by emulsifying agent is schemed；Fig. 4 c are sweet potato
Starch nanometer granule is the microscope figure of Pickering emulsions prepared by emulsifying agent；Fig. 4 d are that cornstarch nano particle is breast
The microscope figure of Pickering emulsions prepared by agent.Above in each figure, the corresponding emulsifying agent particle of label A, B, C, D and E
Footpath is about 710,340,220,180 and 50nm successively；The corresponding emulsifying agent grain diameter of a, b, c, d and e successively about 680,
320th, 220,190 and 60nm.
With the increase of particle diameter, the contact angle of nano particle gradually increases, and particle diameter is the starch nanometer granule of 100-200nm
Contact angle near 90 °.By the measure and micro- sem observation of stability of emulsion, particle diameter 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 particle diameter of nano particle can influence
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,
Control the concentration of sweet potato starch nano particle to be respectively 0,0.25%, 0.5%, 1% and 2%, prepare Pickering emulsions.Figure
5a be sweet potato starch concentrations of nanoparticles prepare Pickering emulsion intercalation methods observation figure, in figure 0h, 1h, 1day and
7day represents the resting period；Fig. 5 b are Pickering emulsion intercalation methods observation figure prepared by cornstarch concentrations of nanoparticles.
Label 0,0.25%, 0.5%, 1% and 2% in the width figure of the above two, represents the concentration of starch nanometer granule respectively.With nanometer
Grain concentration increases to 2% from 0, and emulsion intercalation method is dramatically increased.
Embodiment 6
The method of reference implementation example 2 prepares profit volume ratio and is respectively 1:3,2:3,1:1,3:2,3:1 oil water mixture,
Sweet potato starch nano particle is added in above-mentioned oil water mixture, it is 1% to control the concentration of sweet potato starch nano particle, respectively
Prepare Pickering emulsions.Fig. 6 a are the Pickering emulsion intercalation method observation figures of different oil-water ratios, digital 0.75 in figure,
0.6th, 0.5,0.4,0.25 oil number is represented respectively.Fig. 6 b are the microscope figure of the Pickering emulsions of different oil-water ratios, from a left side
1 is respectively to the right mixture profit volume ratio being corresponding in turn to:3,2:3,1:1,3:2,3:1.When the concentration of starch nanometer granule
For 1% when, oil-water ratio is from 1:3 increase to 3:1, emulsibility first increases to be reduced afterwards, is 1 in oil-water ratio:Emulsibility is most strong when 1.
Embodiment 7
Sensitive environment (the salt ion, temperature etc.) experiment of the Pickering emulsions of starch nanometer granule stabilization.
1. the preparation method of reference implementation example 5, is 1% by freshly prepared sweet potato starch concentrations of nanoparticles
Pickering emulsions, are respectively put into 25,40,60 and 90 DEG C of water-bath and heat 30min, place into and store up in the environment of room temperature
Deposit, the influence by bottle or microscope observation analysis temperature to stability of emulsion.Fig. 7 a are different temperatures to Pickering breasts
The influence of the size droplet diameter of liquid, abscissa is the heat time (min), and ordinate is the particle diameter (μm) of emulsion droplets.Fig. 7 b are difference
At a temperature of Pickering emulsion intercalation methods observation figure.The temperature of emulsion increases to 90 DEG C by 25 DEG C, and emulsion droplets become big, but do not have
Have destroyed.
2. the preparation method of reference implementation example 6, weighs the mixed liquor of a certain amount of starch nanometer granule and different oil-water ratios
In, prepare profit volume ratio and be respectively 1:3,2:3,1:1,3:2,3:1 oil water mixture, weighs a certain amount of sweet potato starch and receives
Rice grain is added to above-mentioned oil mixing with water species, and it is 1% to control the concentration of sweet potato starch nano particle, meanwhile, respectively to mixing
Sodium chloride is added in liquid, controls salt ionic concentration for 0,10,30,60 and 90mM, mixed liquor is used into high-shear homogenizer
10000rmp, homogeneous 2 minutes, you can obtain Pickering emulsions.Fig. 7 c are that different salt ionic concentrations are steady to Pickering emulsions
Qualitatively influence, Fig. 7 d are the micro- sem observation figure of Pickering emulsions under different salt ionic concentrations, are corresponding in turn to from left to right
Salt ionic concentration be 0,10,30,60 and 90mM.It is there be not emulsion intercalation method in the range of 10-90mM in salt ionic concentration
It is significant to change.
Above-mentioned experiment shows to illustrate the heat-resisting and salt tolerance that the emulsion of this kind of starch nanometer granule stabilization has had.
Table 1
Table 2
PDI represents polymer dispersity index in above-mentioned table, and PDI is bigger, represents that molecular weight distribution is wider；PDI is smaller, table
Show that molecular weight distribution is more uniform.
CI represents the ratio that emulsification sex index is bottom whey height and emulsion total height, and CI is smaller, represents that emulsibility is got over
It is good.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the scope of the present invention
It is defined, on the premise of design spirit of the present invention is not departed from, those of ordinary skill in the art are to technical scheme
The various modifications made and improvement, all should fall into the protection domain of claims of the present invention determination.
Claims (10)
1. the preparation method of the Pickering emulsions of a kind of starch nanometer granule stabilization, it is characterised in that comprise the following steps：
(1) preparation of starch nanometer granule emulsifying agent：It is the starch of 20-40% to choose amylose content, and add water gelatinization, by anhydrous second
Alcohol is dropwise added drop-wise in dextrin, is stirred when being added dropwise, and controls mixer rotating speed 500-1500rpm, titration to continue to stir after terminating
1-5h is mixed, suspension is centrifuged, precipitation is lyophilized to obtain starch nanometer granule emulsifying agent；
(2) preparation of Pickering emulsions：Starch nanometer granule emulsifying agent is added in oil-water mixture and is mixed, 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 emulsions are obtained.
2. the preparation method of the Pickering emulsions of starch nanometer granule according to claim 1 stabilization, its feature exists
In the process of step (1) starch gelatinization is that starch adds water, and starch concentration is 1-5wt%, boiling water water-bath gelatinization 20-60min.
3. the preparation method of the Pickering emulsions of starch nanometer granule according to claim 2 stabilization, its feature exists
In dextrin is 1 with the volume ratio of absolute ethyl alcohol：(1-5).
4. the preparation method of the Pickering emulsions of starch nanometer granule according to claim 3 stabilization, its feature exists
In the profit volume ratio of step (2) oil-water mixture is (1:3)-(3:1).
5. the preparation method of the Pickering emulsions of starch nanometer granule according to claim 4 stabilization, its feature exists
In the oil phase is vegetable oil.
6. the preparation method of the Pickering emulsions of starch nanometer granule according to claim 5 stabilization, its feature exists
In the vegetable oil is selected from the one kind in soybean oil, peanut oil, corn oil, sunflower oil, castor oil.
7. the preparation method of the Pickering emulsions of starch nanometer granule according to claim 6 stabilization, its feature exists
In by mixed liquor using high-shear homogenizer with the rotating speed of 10000-30000rmp, homogeneous 2-4 minutes.
8. the preparation method of the stable Pickering emulsions of starch nanometer granule according to claim any one of 1-7, its
It is characterised by, the average grain diameter of starch nanometer granule emulsifying agent obtained in step (1) is 50nm-700nm.
9. the preparation method of the Pickering emulsions of starch nanometer granule according to claim 8 stabilization, its feature exists
In the average grain diameter of starch nanometer granule emulsifying agent obtained in step (1) is 180nm-350nm.
10. the preparation method of the stable Pickering emulsions of starch nanometer granule according to claim any one of 1-7,
Characterized in that, the starch is selected from cornstarch, sweet potato starch and tapioca.
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