CN110917137A - Preparation method of ultrastable pickering emulsion with synergistic stability of prolamin nanoparticles and starch nanoparticles - Google Patents
Preparation method of ultrastable pickering emulsion with synergistic stability of prolamin nanoparticles and starch nanoparticles Download PDFInfo
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- CN110917137A CN110917137A CN201911170678.3A CN201911170678A CN110917137A CN 110917137 A CN110917137 A CN 110917137A CN 201911170678 A CN201911170678 A CN 201911170678A CN 110917137 A CN110917137 A CN 110917137A
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Images
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- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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Abstract
The invention discloses a preparation method of pickering emulsion with stable cooperation of prolamin nanoparticles and starch nanoparticles. Comprises preparing a starch nanoparticle dispersion; preparing pickering emulsion: and mixing the starch nanoparticle dispersion liquid, the prolamin nanoparticle dispersion liquid and the oil phase dissolved with the fat-soluble active substance, and homogenizing at high speed to obtain the ultra-stable Pickering emulsion. The pickering emulsion prepared by the invention has the characteristics of less emulsifier dosage, cheap and easily available raw materials, simple preparation method, environmental friendliness and the like, and can effectively prepare the pickering emulsion with ultrahigh stability and improve the encapsulation rate and bioavailability of the hydrophobic active substance curcumin.
Description
Technical Field
The invention belongs to the technical field of food, cosmetics and medicines, and particularly relates to a preparation method of a Pickering emulsion with synergistic stabilization of prolamin nanoparticles and starch nanoparticles.
Background
Pickering emulsions are a new type of emulsion stabilized with solid particles. Solid particles are adsorbed on an oil-water interface, and the liquid drops are tightly wrapped to prevent aggregation, so that the emulsion is effectively stabilized. The pickering emulsion has many advantages, and the solid particles replace the use of synthetic molecular emulsifiers, so that the cost can be saved, and the pickering emulsion is more environment-friendly. To date, there have been many studies using synthetic colloidal particles to prepare pickering emulsions. However, these particles generally have the disadvantages of poor biocompatibility, nonbiodegradability and the like, and the application of the prepared pickering emulsion in the fields of cosmetics, foods, medicines and the like is greatly limited. For this reason, many studies have been focused on colloidal particles of natural origin to develop pickering emulsions that can be applied to the above-mentioned fields.
At present, the pickering emulsion prepared from plant raw materials, which is safe, nontoxic and green, is still insufficient in stability under the condition of long-term storage. How to prepare the ultra-stable pickering emulsion which is stable from plant-derived raw materials and is safe and nontoxic is a technical problem to be solved.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The invention provides a preparation method of Pickering emulsion with prolamin nano-particles and starch nano-particles synergistically stabilized, which comprises the following steps,
preparing a starch nanoparticle dispersion;
preparing alcohol soluble protein nanoparticle dispersion liquid;
preparing pickering emulsion: and mixing the starch nanoparticle dispersion liquid, the prolamin nanoparticle dispersion liquid and the oil phase dissolved with the active substances, and homogenizing at a high speed to obtain the ultra-stable Pickering emulsion.
The preferable scheme of the preparation method of the Pickering emulsion with the prolamin nano-particles and the starch nano-particles which are synergistically stabilized is as follows: the starch nanoparticles are one or more of cereal starch nanoparticles, potato starch nanoparticles or bean starch nanoparticles; the alcohol soluble protein is one or more of zein, wheat alcohol soluble protein or kafirin.
The preferable scheme of the preparation method of the Pickering emulsion with the prolamin nano-particles and the starch nano-particles which are synergistically stabilized is as follows: the preparation of the starch nanoparticle dispersion liquid comprises the steps of weighing waxy corn starch, adding the waxy corn starch into a sulfuric acid solution with the concentration of 2M-4M, carrying out water bath reaction for 5-8 days at the temperature of 35-50 ℃, centrifugally washing an obtained product, and then dispersing the product in water to obtain the waxy corn starch particle dispersion liquid mL.
The preferable scheme of the preparation method of the Pickering emulsion with the prolamin nano-particles and the starch nano-particles which are synergistically stabilized is as follows: the starch: the feed-liquid ratio of the sulfuric acid solution is 30-60 g: 500 mL; the concentration of the starch nanoparticle dispersion liquid is 0.1-10 w/v% in g/mL, the pH value is 3-9, and the size of the prepared starch nanoparticles is 40-500 nanometers.
The preferable scheme of the preparation method of the Pickering emulsion with the prolamin nano-particles and the starch nano-particles which are synergistically stabilized is as follows: the concentration of the starch nanoparticle dispersion liquid is 2 w/v% in g/mL, and the pH value of the starch nanoparticle dispersion liquid is 3-4.
The preferable scheme of the preparation method of the Pickering emulsion with the prolamin nano-particles and the starch nano-particles which are synergistically stabilized is as follows: the preparation of the prolamin nanoparticle dispersion liquid comprises the steps of weighing zein, adding 60-90% of ethanol aqueous solution, stirring for dissolving, adding water, stirring for 0.5-3 h, and performing rotary evaporation at 35-45 ℃ in water bath to remove ethanol to obtain the zein nanoparticle dispersion liquid.
The preferable scheme of the preparation method of the Pickering emulsion with the prolamin nano-particles and the starch nano-particles which are synergistically stabilized is as follows: the feed-liquid ratio of the zein to the ethanol aqueous solution is 0.2-1.5 g: 25 mL; the concentration of the zein nanoparticle dispersion liquid is 0.1-10 w/v% in g/mL, the pH value of the zein nanoparticle dispersion liquid is 3-9, and the size of the zein nanoparticles is 70-500 nanometers.
The preferable scheme of the preparation method of the Pickering emulsion with the prolamin nano-particles and the starch nano-particles which are synergistically stabilized is as follows: the concentration of the zein nanoparticle dispersion liquid is 2 w/v% in g/mL, and the pH value of the zein nanoparticle dispersion liquid is 3-4.
The preferable scheme of the preparation method of the Pickering emulsion with the prolamin nano-particles and the starch nano-particles which are synergistically stabilized is as follows: the preparation method comprises the following steps of preparing pickering emulsion, wherein mixing time of the prolamin nanoparticle dispersion liquid and the starch nanoparticle dispersion liquid is 0-10 minutes, and the oil phase is vegetable oil such as soybean oil, castor oil, olive oil, peanut oil and corn oil, silicone oil such as methyl silicone oil, ethyl silicone oil, phenyl silicone oil and hydroxyl silicone oil, essential oil such as peppermint oil, rose oil, sweet orange oil and cinnamon oil, alkane such as liquid paraffin and vaseline, and common oil for cosmetics such as GTCC, polysiloxane and cetyl alcohol. The oil phase content is 10 v/v% -85 v/v%, the content of the prolamin nanoparticles and the starch nanoparticles is 0.1 w/v% -10 w/v%, and the mass ratio of the prolamin nanoparticles to the starch nanoparticles is 0.1: 1-1: 0.1.
the preferable scheme of the preparation method of the Pickering emulsion with the prolamin nano-particles and the starch nano-particles which are synergistically stabilized is as follows: the high-speed homogenization is carried out for 2-10 min at 10000-19000 rpm; the active matter comprises 0.1-5 w/v% of polyphenols such as curcumin, catechin, EGCG and the like and flavonoids such as baicalein and quercetin.
The invention has the beneficial effects that: the Pickering emulsion prepared by the invention has small particle size and is distributed in a unimodal mode, the alcohol soluble protein nano particles are firstly adsorbed on an oil-water interface to form a compact interface layer, then the starch nano particles are adsorbed on the surface of the interface layer formed by the alcohol soluble protein nano particles through electrostatic attraction to form the Pickering emulsion with obvious phase interface and stable double-layer particles, the unique particle stabilizer double-layer structure provides ultrahigh stability for the prepared Pickering emulsion, and the Pickering emulsion can be kept stable after being centrifuged for 30min under the condition of 20000 g. By loading the hydrophobic active curcumin, the encapsulation rate of more than 95 percent is still maintained after 30 days of placement. The pickering emulsion prepared by the invention has the characteristics of good biocompatibility and biodegradability of the particle stabilizer, small using amount, low price, simple preparation method and the like, and particularly, the prepared pickering emulsion has ultrahigh stability and can load and improve the bioavailability of active substances.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is an appearance of Pickering emulsion of the present invention (left panel) and an appearance of the emulsion after centrifugation at 20000g for 30min (right panel).
FIG. 2 is a laser confocal image of the Pickering emulsion of the present invention.
Fig. 3 is a pickering emulsion prepared from comparative example 1 zein nanoparticles alone (left panel) and waxy corn starch nanoparticles alone (right panel) using soybean oil as the oil phase at pH 4.
FIG. 4 is the stability of a Pickering emulsion prepared after stirring the zein nanoparticle and waxy corn starch nanoparticle dispersions of comparative example 2 for more than ten minutes after centrifugation at 10000g for 10 min.
FIG. 5 is a graph of the stability of Pickering emulsions of the invention and comparative example 3 (left panel) and 4 (right panel) prepared using a conventional layer-by-layer build-up process at 10000g for 10 min.
FIG. 6 is an appearance diagram of the prepared Pickering emulsion and its stability after centrifugation at 10000g for 10min when the concentrations of the zein nanoparticles and the waxy corn starch nanoparticles of the present invention are 0.05%, respectively.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The preparation method of the ultra-stable pickering emulsion comprises the following steps:
1) the preparation method of the starch nanoparticle dispersion liquid comprises the following steps:
weighing starch in a container, adding the starch into a sulfuric acid solution with the concentration of 2-4M, carrying out mechanical stirring for 5-8 days in a water bath at the temperature of 35-50 ℃ so as to carry out full acidolysis on the starch to obtain a starch nanoparticle acidolysis solution, washing and centrifuging the acidolysis solution for multiple times until the starch nanoparticle is weakly acidic, and then carrying out freeze drying to obtain the starch nanoparticle, wherein the starch: the feed-liquid ratio of the sulfuric acid solution is 30-60 g: 500 mL. Adding the obtained starch nanoparticles into deionized water, and fully stirring to obtain a starch nanoparticle dispersion liquid, wherein the concentration of the starch nanoparticles is 0.1 w/v% -10 w/v%.
2) The preparation method of the zein nanoparticle dispersion comprises the following steps:
weighing zein in a container, adding 60-90% of ethanol aqueous solution, performing magnetic stirring to fully disperse the zein, adding deionized water with the volume being 3-4 times that of the ethanol solution, stirring for 0.5-3 h under high-speed mechanical stirring, and performing rotary evaporation to remove ethanol in a water bath at 35-45 ℃ to obtain zein nanoparticle dispersion liquid, wherein the material-to-liquid ratio of the zein to the ethanol aqueous solution is 0.2-1.5 g: 25 mL.
3) Adjusting the pH of the starch nanoparticle dispersion liquid and the zein nanoparticle dispersion liquid obtained in the steps 1) and 2) by using NaOH and HCl, mixing, adding soybean oil dissolved with fat-soluble active substances into the starch nanoparticle dispersion liquid and the zein nanoparticle dispersion liquid, wherein the concentration of the starch nanoparticles and the zein nanoparticles is 1-100 g/L, and the mass-to-volume ratio of the starch nanoparticle dispersion liquid to the zein nanoparticle dispersion liquid to the soybean oil is (0.1-10 g): 100mL, and homogenizing at a high speed for 2-10 min under the condition of 10000-19000 rpm to obtain the stable pickering emulsion of the starch nanoparticles and the zein nanoparticles.
Example 1:
(1) adding 10g of waxy corn starch into 100mL of 3.16M sulfuric acid solution, mechanically stirring for one week at 100rpm/min, centrifuging and washing for multiple times until the pH value is 5-6, and freeze-drying to obtain starch nanoparticles;
(2) dissolving 0.1g of the starch nanoparticles obtained in the step (1) into about 5mL of deionized water to obtain a starch nanoparticle dispersion liquid;
(3) dropwise adding 1M HCl to the starch nanoparticle dispersion liquid obtained in step (2), and adjusting the pH to 4 to obtain a 2 w/v% (g/mL) starch nanoparticle dispersion liquid having a pH of 4;
(4) dissolving 1g zein in 80% ethanol water solution, and magnetically stirring for 30 min;
(5) dissolving the zein ethanol solution obtained in the step (4) by drops into 75mL of deionized water under the condition of 500rpm/min, and stirring for 2 hours to obtain zein nanoparticle ethanol water dispersion liquid;
(6) performing rotary evaporation on the dispersion liquid obtained in the step (5) at 42 ℃ to remove ethanol and part of water to obtain zein nanoparticle dispersion liquid of about 2 w/v% (g/mL);
(7) dropwise adding 1M HCl or 1M NaOH into the zein nanoparticle dispersion liquid obtained in the step (6) to adjust the pH to 4, so as to obtain the zein nanoparticle dispersion liquid with the pH to 4 and the concentration of 2 w/v%;
(8) 5mL of the dispersion of step (3) and 5mL of the dispersion of step (7) and 10mL of soybean oil were mixed and homogenized at 17000rpm for 2min at high speed to obtain a Pickering emulsion.
The Pickering emulsion obtained by the method can still keep stable after being centrifuged for 10min by 10000g, a double-layer interface structure can be obtained by a laser confocal microscope, 1 w/v% (g/mL) of hydrophobic active curcumin is loaded into the Pickering emulsion and is stored for 30 days at 40 ℃, and the retention rate reaches 92.97% by detection of an ultraviolet spectrophotometer. Loading 1 wt% of hydrophobic active substance curcumin into Pickering emulsion, storing for 30 days at 40 ℃, mixing and oscillating 10 microliter of emulsion with 10mL of ethyl acetate, passing through a filter membrane to obtain clear ethyl acetate extract, taking ethyl acetate as a blank sample, and detecting by using an ultraviolet spectrophotometer, wherein the retention rate reaches 92.97%. Wherein the formula for the retention is A/A0, A is the absorbance value measured after 40 days, A0 is the absorbance value measured for the freshly prepared emulsion.
Example 2:
(1) adding 5g of waxy corn starch into 50mL of 3.16M sulfuric acid solution, mechanically stirring for one week at 100rpm/min, centrifuging and washing for multiple times until the pH value is 5-6, and freeze-drying to obtain starch nanoparticles;
(2) dissolving 0.2g of the starch nanoparticles obtained in the step (1) into about 10mL of deionized water to obtain a starch nanoparticle dispersion liquid;
(3) dropwise adding 1M HCl to the starch nanoparticle dispersion liquid obtained in step (2), and adjusting the pH to 4 to obtain a 2 w/v% (g/mL) starch nanoparticle dispersion liquid having a pH of 4;
(4) dissolving 0.5g zein in 12.5mL 80% ethanol water solution, and magnetically stirring for 30 min;
(5) dissolving the zein ethanol solution obtained in the step (4) by drops into 37.5mL of deionized water under the condition of 500rpm/min, and stirring for 3h to obtain zein nanoparticle ethanol water dispersion liquid;
(6) and (3) performing rotary evaporation on the dispersion liquid obtained in the step (5) at the temperature of 45 ℃ to remove ethanol and part of water, so as to obtain a zein nanoparticle dispersion liquid of 2 w/v% (g/mL).
(7) Dropwise adding 1M HCl or 1M NaOH into the zein nanoparticle dispersion liquid obtained in the step (6) to adjust the pH to 4, so as to obtain the zein nanoparticle dispersion liquid with the pH to 4;
(8) dissolving curcumin in soybean oil to obtain 0.5% w/v soybean oil dissolved with curcumin;
(9) homogenizing 10mL of the dispersion of step (3) and 10mL of the dispersion of step (7) and 20mL of the soybean oil of step (8) in which 0.5w/v curcumin was dissolved at 17000rpm for 2min at high speed to obtain Pickering emulsion.
Centrifuging the obtained Pickering emulsion for 10min by 10000g, keeping the stability, obtaining a double-layer interface structure by a laser confocal microscope, loading 0.5 w/v% (g/mL) of hydrophobic active substance curcumin into the Pickering emulsion, storing for 30 days at 40 ℃, and detecting by an ultraviolet spectrophotometer, wherein the retention rate reaches 96.72%.
FIG. 1 is an appearance chart of the emulsion of example 2 and its stability after centrifugation at 10000g for 10 min. FIG. 2 is a confocal laser microscopy of Pickering emulsion.
Example 3:
(1) adding 7.5g of waxy corn starch into 50mL of 3.16M sulfuric acid solution, mechanically stirring for one week at 100rpm/min, centrifuging and washing for multiple times until the pH value is 5-6, and freeze-drying to obtain starch nanoparticles;
(2) dissolving 0.1g of the starch nanoparticles obtained in the step (1) into about 5mL of deionized water to obtain a starch nanoparticle dispersion liquid;
(3) dropwise adding 1M HCl to the starch nanoparticle dispersion liquid obtained in step (2), and adjusting the pH to 3 to obtain a 2 w/v% (g/mL) starch nanoparticle dispersion liquid having a pH of 3;
(4) dissolving 1g of zein in 25mL of 80% ethanol water solution, and magnetically stirring for 30 min;
(5) dissolving the zein ethanol solution obtained in the step (4) by drops into 75mL of deionized water under the condition of 500rpm/min, and stirring for 2 hours to obtain zein nanoparticle ethanol water dispersion liquid;
(6) performing rotary evaporation on the dispersion liquid obtained in the step (5) at 45 ℃ to remove ethanol and part of water, and obtaining 2% zein nanoparticle dispersion liquid;
(7) dropwise adding 1M HCl or 1M NaOH into the zein nanoparticle dispersion liquid obtained in the step (6) to adjust the pH to 3, so as to obtain a zein nanoparticle dispersion liquid with the pH to 3;
(8) and (3) homogenizing the dispersion liquid obtained in the step (3) and the step (7) in 5mL of soybean oil in 10mL at a high speed at 17000rpm for 2min to obtain the Pickering emulsion.
Centrifuging the obtained Pickering emulsion for 10min at 10000g, keeping the stability, obtaining a double-layer interface structure by a laser confocal microscope, loading 0.1% of hydrophobic active substance curcumin into the Pickering emulsion, storing for 30 days at 40 ℃, and detecting by an ultraviolet spectrophotometer, wherein the retention rate reaches 94.32%.
Comparative example 1:
a 2 w/v% (g/mL) starch nanoparticle dispersion having pH 4 prepared in step (3) of example 2 and soybean oil were mixed in a volume ratio of 1: 1, homogenizing at 17000rpm for 2min at a high speed to prepare pickering emulsion;
and 2 w/v% (g/mL) zein nanoparticles pH 4 prepared in example 2, step (7) and soybean oil 1: and (3) carrying out high-speed homogenization at 17000rpm for 2min under the condition of 1 to prepare the Pickering emulsion.
And centrifuging the two pickering emulsions at 5000g for 5min, and demulsifying the two emulsions.
FIG. 3 is a graph showing the emulsion of comparative example 1, and turbidity of the aqueous phase and delamination were observed after standing for 24 hours.
Comparative example 2:
the starch nanoparticle dispersion liquid with pH of 4 prepared in step (3) of example 2 and the zein nanoparticle dispersion liquid with pH of 4 prepared in step (7) of example 2 were mixed and stirred for 2 hours to form a starch nanoparticle-zein nanoparticle composite particle dispersion liquid, and then the composite particle dispersion liquid was mixed in a volume ratio of 1: 1 mixing with soybean oil, and homogenizing at 17000rpm for 2min to form Pickering emulsion.
Centrifuging the pickering emulsion at 10000g for 10min, and demulsifying the emulsion. See fig. 4.
Comparative example 3:
the starch nanoparticle dispersion with pH 4 prepared in step (3) of example 2 was mixed with soybean oil and homogenized at 17000rpm for 1min, followed by the addition of the zein nanoparticle dispersion with pH 4 prepared in step (7) of example 2 and homogenized at 17000rpm for 1min to form pickering emulsion.
Centrifuging the pickering emulsion at 10000g for 10min to separate out oil. See fig. 5.
Comparative example 4:
the zein nanoparticle dispersion with pH 4 prepared in step (3) of example 2 was mixed with soybean oil and homogenized at 17000rpm for 1min, followed by addition of 2 w/v% (g/mL) of the starch nanoparticle dispersion with pH 4 prepared in step (7) of example 2 and homogenization at 17000rpm for 1min to form a pickering emulsion.
Centrifuging the pickering emulsion at 10000g for 10min to separate out oil from the emulsion. See fig. 5.
Comparative example 5:
the starch nanoparticle dispersion of example 2 was adjusted to have a nanoparticle concentration of 0.05 w/v% and a zein nanoparticle dispersion of 0.05 w/v%, and the remaining steps were the same as in example 2. The pickering emulsion obtained is shown in FIG. 6.
10000g of the pickering emulsion obtained in the above way is centrifuged for 10min, and oil is separated out from the emulsion, which is shown in figure 6.
Comparative example 6:
the starch nanoparticle dispersion concentration of example 2 was adjusted to 15 w/v% and the zein nanoparticle dispersion concentration was adjusted to 15 w/v%, and the remaining steps were the same as in example 2.
10000g of the pickering emulsion obtained in the previous step is centrifuged for 10min, and particle precipitation is generated at the bottom of the emulsion.
In summary, as shown in fig. 1 and 2, the pickering prepared by the present invention can be centrifuged at 20000g for 30min to maintain stability, and has ultrahigh stability, in addition, the pickering emulsion of the present invention has a double-layer interface structure, providing a stability foundation thereof, fig. 3 is an emulsion of comparative example 1, and after standing for 24h, water phase turbidity and delamination phenomena can be observed, which illustrates that the present invention greatly improves the stability of zein and waxy corn starch nanoparticle pickering emulsions, and fig. 4 is an emulsion of comparative example 2, which proves that the method of the present invention is more stable than the method of preparing composite particle-stabilized pickering emulsions widely at present. FIG. 5 is a graph of the emulsions of comparative examples 3 and 4, demonstrating that the process of the present invention is more stable than the conventional layer-by-layer build-up process for preparing a two-layer pickering emulsion. FIG. 6 is the emulsion of comparative example 5, and it can be seen that when the concentration of the waxy corn starch nanoparticle dispersion was 0.1 w/v%, the emulsion was unstable and broke after centrifugation. In addition, the curcumin-containing composite material can wrap the hydrophobic active substance curcumin by 96.72 percent, and proves that the curcumin-containing composite material can be used as a carrier of the hydrophobic active substance to improve the bioavailability of the hydrophobic active substance.
The Pickering emulsion prepared by the method has small droplet size and is distributed in a unimodal mode, the zein nanoparticles are firstly adsorbed on an oil-water interface to form a compact interface layer, then the starch nanoparticles are adsorbed on the surface of the zein nanoparticles through electrostatic attraction to form the Pickering emulsion with the double-layer compact interface layer, the double-layer interface structure provides ultrahigh stability for the emulsion, the emulsion can be centrifuged for 30min under the condition of 20000g to keep stable, and the hydrophobic active substance curcumin is loaded, so that the wrapping rate of the emulsion is still more than 95% after the emulsion is placed for 30 days. The pickering emulsion prepared by the invention has the characteristics of less emulsifier dosage, cheap and easily available raw materials, simple preparation method, environmental friendliness and the like, and can effectively prepare the pickering emulsion with ultrahigh stability and improve the encapsulation rate and bioavailability of the hydrophobic active substance curcumin.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A method for preparing ultra-stable Pickering emulsion with prolamin nano-particles and starch nano-particles synergistically stabilized is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
preparing a starch nanoparticle dispersion;
preparing alcohol soluble protein nanoparticle dispersion liquid;
preparing pickering emulsion: and mixing the starch nanoparticle dispersion liquid, the prolamin nanoparticle dispersion liquid and the oil phase dissolved with the active substances, and homogenizing at a high speed to obtain the ultra-stable Pickering emulsion.
2. The method of making a Pickering emulsion of claim 1, wherein the emulsion is synergistically stabilized by prolamin nanoparticles and starch nanoparticles, comprising: the starch granules are one or more of cereal starch, potato starch or bean starch; the alcohol soluble protein is one or more of zein, wheat alcohol soluble protein or kafirin.
3. A method of making a pick's emulsion of synergistic stabilization of prolamin and starch nanoparticles as claimed in claim 1 or 2, wherein: the preparation method of the starch nanoparticle dispersion liquid comprises the steps of weighing waxy corn starch, adding the waxy corn starch into a sulfuric acid solution with the concentration of 2M-4M, carrying out water bath reaction for 5-8 days at the temperature of 35-50 ℃, centrifugally washing an obtained product, and then dispersing the product in water to obtain the waxy corn starch nanoparticle dispersion liquid.
4. A method of making a pick's emulsion of claim 3 wherein the prolamin nanoparticles and the starch nanoparticles are synergistically stabilized, the method comprising: the starch: the feed-liquid ratio of the sulfuric acid solution is 30-60 g: 500 mL; the concentration of the starch nanoparticle dispersion liquid is 0.1-10 w/v% in g/mL, the pH value is 3-9, and the size of the starch nanoparticles is 40-500 nanometers.
5. The method of making a Pickering emulsion of claim 4, wherein the emulsion is synergistically stabilized by prolamin nanoparticles and starch nanoparticles, comprising: the concentration of the starch nanoparticle dispersion liquid is 2 w/v% in g/mL, and the pH value of the starch nanoparticle dispersion liquid is 3-4.
6. A method of making a pick's emulsion of synergistic stabilization of prolamin and starch nanoparticles as claimed in claim 1 or 2, wherein: the preparation of the prolamin nanoparticle dispersion liquid comprises the steps of weighing zein, adding 60-90% of ethanol aqueous solution, stirring for dissolving, adding water, stirring for 0.5-3 h, and performing rotary evaporation to remove ethanol in water bath at 35-45 ℃ to obtain the zein nanoparticle dispersion liquid.
7. The method of making a Pickering emulsion of claim 6, wherein the emulsion is synergistically stabilized by prolamin nanoparticles and starch nanoparticles, comprising: the feed-liquid ratio of the zein to the ethanol aqueous solution is 0.2-1.5 g: 25 mL; the concentration of the zein nanoparticle dispersion liquid is 0.1-10 w/v% in g/mL, the pH value of the zein nanoparticle dispersion liquid is 3-9, and the size of zein nanoparticles is 7-500 nanometers.
8. The method of making a Pickering emulsion of claim 7, wherein the emulsion is synergistically stabilized by prolamin nanoparticles and starch nanoparticles, comprising: the concentration of the zein nanoparticle dispersion liquid is 2 w/v% in g/mL, and the pH value of the zein nanoparticle dispersion liquid is 3-4.
9. A method of making a pick's emulsion of synergistic stabilization of prolamin and starch nanoparticles as claimed in claim 1 or 2, wherein: the method for preparing the pickering emulsion comprises the following steps of mixing a prolamin particle dispersion liquid and a starch nanoparticle dispersion liquid for 0-10 minutes, wherein an oil phase comprises one or more of vegetable oil such as soybean oil, castor oil, olive oil, peanut oil and corn oil, silicone oil such as methyl silicone oil, ethyl silicone oil, phenyl silicone oil and hydroxyl silicone oil, peppermint oil, rose oil, sweet orange oil, cinnamon oil, liquid paraffin, vaseline, GTCC, polysiloxane and cetyl alcohol, the content of the oil phase is 10 v/v-85 v/v%, the content of prolamin nanoparticles and starch nanoparticles is 0.1 w/v-10 w/v%, and the mass ratio of the prolamin nanoparticles to the starch nanoparticles is 0.1: 1-1: 0.1.
10. the method of making a Pickering emulsion of claim 7, wherein the emulsion is synergistically stabilized by prolamin nanoparticles and starch nanoparticles, comprising: the high-speed homogenization is carried out for 2-10 min at 10000-19000 rpm; the active matter comprises 0.1-5 w/v% of curcumin, catechin, EGCG and flavonoid.
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