CN112806575B - Preparation and application of water-in-oil-in-water Pickering emulsion - Google Patents
Preparation and application of water-in-oil-in-water Pickering emulsion Download PDFInfo
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- 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
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
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Abstract
The invention provides a preparation method of a water-in-oil-in-water Pickering emulsion, which comprises the following steps: mixing NMN and cellulose nanofiber CNF, adding water, and performing ultrasonic dispersion to obtain an NMN/CNF aqueous solution; mixing the NMN/CNF aqueous solution with grease, and performing ultrasonic emulsification to obtain emulsion A; and adding the NMN/CNF aqueous solution into the emulsion A, and mechanically shearing and emulsifying to obtain emulsion B, namely the water-in-oil-in-water Pickering emulsion. The method can obtain food-grade water-in-oil-in-water type Pickering emulsion with stable NMN/CNF emulsification. The preparation method utilizes NMN/CNF as an emulsion stabilizer to be cooperated with emulsification to prepare the water-in-oil-in-water type Pickering emulsion stably, can completely avoid using organic surfactant substances which are easy to generate bubbles, and the emulsifier is a green, environment-friendly, edible and renewable resource material, and has the advantages of simple production process, no environmental pollution and low production cost.
Description
Technical Field
The invention belongs to the field of food chemical industry, and particularly relates to a preparation method and application of a food-grade water-in-oil-in-water type Pickering emulsion emulsifier based on cellulose nanofibers and NMN.
Background
The emulsion is a dispersion system formed by dispersing a liquid in another liquid immiscible with the liquid, is mostly formed by mixing a water-insoluble oil phase and a water phase, and is widely applied to industries of papermaking, food, cosmetics, medicines and the like. Emulsions are thermodynamically unstable systems and in order to maintain the relative stability of the emulsion (kinetic stability) emulsifiers or stabilizers have to be added during the preparation of the emulsion. Most of the traditional emulsifiers or stabilizers are surfactants and high molecular polymers with surface activity, and the stability of the emulsion is maintained by reducing the interfacial tension between oil-water two-phase liquid, providing a stable interfacial film and improving the viscosity of a continuous phase. In recent years, since solid particles can avoid adverse effects of a surfactant on the environment, stabilize a high-concentration dispersed phase emulsion, and the emulsion is less affected by changes in pH, salt concentration, temperature, and oil phase composition, pickering emulsions stabilized by emulsification of solid particles have received increasing attention.
Cellulose Nanofibers (CNF) have a large aspect ratio and flexibility, which have been extensively studied as emulsion stabilizers for Pickering emulsions. CNFs are usually made from vegetable fibres after mechanical deconstruction, the effect on the stability of Pickering emulsions is usually related to the formation of a colloidal network at low CNF concentrations, thereby increasing the effective viscosity, which effect, together with the biocompatibility of CNFs, is beneficial in cosmetics, food and formulation of architectures for controlled drug release and additive manufacturing.
Nicotinamide mononucleotide as NAD + The intermediate in the remedy approach has the functions of resisting oxidation and reducing oxidative stress, has good performance in the treatment of some specific diseases, and in addition, the NMN can slow down the physiological decline of organisms, enhance energy metabolism and prolong the life in the aspect of anti-aging. Given that NMN is humanThe endogenous substance has high safety and good thermal stability, so that the NMN has wide prospect as an active substance in the development of the field of functional foods.
Disclosure of Invention
The invention aims to provide an NMN and CNF food-grade Pickering emulsion emulsifier and a water-in-oil-in-water emulsion emulsification technology prepared by the same, other surfactants are not required to be added, and the prepared emulsion has high stability.
In order to achieve the purpose, the invention adopts the following technical scheme.
A preparation method of a water-in-oil-in-water Pickering emulsion comprises the following steps:
(1) Mixing beta-Nicotinamide Mononucleotide (NMN) and Cellulose Nanofiber (CNF), adding water, and performing ultrasonic dispersion to obtain an NMN/CNF aqueous solution;
(2) Mixing the NMN/CNF aqueous solution with grease, and performing ultrasonic emulsification to obtain emulsion A;
(3) And adding the NMN/CNF aqueous solution into the emulsion A, and mechanically shearing and emulsifying to obtain emulsion B, namely the water-in-oil-in-water Pickering emulsion.
The mass ratio of the beta-nicotinamide mononucleotide to the cellulose nanofiber is 1-1.
The concentration of the cellulose nanofibers in the NMN/CNF aqueous solution is 0.1% -3%, preferably 0.5% -1.2%.
The cellulose nano-fiber is cationic aminated nano-cellulose fiber with the diameter of 30-100nm and the length of 1-10 μm.
The temperature of the ultrasonic emulsification is 0-20 ℃, and the preferable temperature is 2-5 ℃; the power is 600-3000W; the time is 2-20min.
The oil is selected from animal and vegetable oil or solution with animal and vegetable oil as solvent, such as fish oil, oleum Helianthi, oleum Maydis, soybean oil, oleum Olivarum, plant essential oil, vegetable oil containing fat-soluble vitamins, algae oil containing DHA, and soybean oil containing soybean isoflavone.
In the emulsion A, the mass fraction of the grease is 20-78%.
The temperature of the mechanical shearing emulsification is 0-20 ℃; the rotating speed is 1000-20000rpm, preferably 5000-15000rpm; the time is 1-30min.
In the emulsion B, the mass fraction of the grease is 15-70%.
The emulsion A is oil-in-water Pickering emulsion, and the emulsion B is water-in-oil-in-water Pickering emulsion.
A water-in-oil-in-water Pickering emulsion obtained by the above method.
A product comprising the above water-in-oil-in-water Pickering emulsion. The product is selected from food, health food, medicine or cosmetic.
The invention has the following advantages:
the preparation method can obtain food-grade water-in-oil-in-water type Pickering emulsion with stable NMN/CNF emulsification. The preparation method utilizes NMN/CNF as an emulsion stabilizer to be cooperated with emulsification to prepare the water-in-oil-in-water type Pickering emulsion stably, can completely avoid using organic surfactant substances which are easy to generate bubbles, and the emulsifier is a green, environment-friendly, edible and renewable resource material, and has the advantages of simple production process, no environmental pollution and low production cost. The invention firstly prepares oil-in-water type Pickering emulsion by inducing NMN/CNF vacancy stabilization effect through ultrasonic emulsification and dispersion, and then further generates a three-dimensional cross-linked network structure through shearing emulsification on the basis to prepare the water-in-oil-in-water composite Pickering emulsion. The prepared water-in-oil-in-water Pickering emulsion has ultrahigh stability and viscoelasticity, NMN and CNF are mutually combined through the electrostatic attraction, the molecular structure of the NMN and the original property of the CNF are not damaged, the surface wettability of the CNF is only simply improved, meanwhile, the formed water-in-oil-in-water emulsion structure can also effectively protect the NMN molecules in the water phase of the inner layer from being damaged by oxidation, the activity of the NMN component is prolonged, and the water-in-oil-in-water Pickering emulsion is expected to become an effective additive and stabilizer of milk food or cosmetics. The embodiment shows that the NMN/CNF prepared by the invention has good emulsification and stabilization effects on edible oil, and the emulsion does not generate particle aggregation and precipitation after being placed for 180 days, does not have any phase body precipitation and demulsification phenomena, and has good stability.
Drawings
FIG. 1 is a photograph of the appearance of water-in-oil-in-water sunflower seed oil Pickering emulsions prepared in example 1 at different CNF concentrations;
FIG. 2 is a micrograph of a water-in-oil-in-water fish oil Pickering emulsion prepared in example 2 with a scale of 100 μm.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings, but the present invention is not limited by the following examples.
Example 1 preparation of a Water-in-oil-in-Water sunflower oil Pickering emulsion
(1) Mixing beta-Nicotinamide Mononucleotide (NMN) and cellulose nanofibers (amino CNF, the average diameter is 35nm, the average length is 1.2 microns) according to a mass ratio of 1;
(2) Mixing the NMN/CNF aqueous solution obtained in the step (1) with sunflower seed oil (commercial edible oil) according to the mass fraction of an oil phase of 20%, and performing ultrasonic emulsification and dispersion for 2min at the temperature of 0 ℃ and the power of 600W to obtain an emulsion A, namely an oil-in-water sunflower seed oil Pickering emulsion, wherein the average particle size of the emulsion is 22 mu m, and the viscosity of the emulsion is 233Pa & s;
(3) Adding the NMN/CNF aqueous solution obtained in the step (1) into the emulsion A to enable the mass fraction of an oil phase to be 15%, and shearing and emulsifying for 1min at 0 ℃ by using a shearing and emulsifying machine at 1000rpm to obtain emulsion B, namely the water-in-oil-in-water sunflower seed oil Pickering emulsion, wherein the average particle size of the emulsion is 41 mu m, and the viscosity of the emulsion is 297 Pa s. After the emulsion is placed for 180 days at normal temperature, no phase body is separated out, and no demulsification phenomenon occurs.
The CNF Pickering emulsion with the mass fraction of 0.5, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8, 2.0% water-in-oil-in-water sunflower oil was prepared according to the above conditions, and the appearance is shown in fig. 1. As can be seen, the emulsion was milky white in color, creamy in texture and did not flow upon inversion.
Example 2 preparation of a Water-in-oil-in-Water Fish oil Pickering emulsion
(1) Mixing beta-Nicotinamide Mononucleotide (NMN) and cellulose nanofibers (amino CNF, the average diameter is 55nm, the average length is 3.1 microns) according to a mass ratio of 1;
(2) Mixing the NMN/CNF aqueous solution obtained in the step (1) with fish oil containing DHA according to the oil phase mass fraction of 50%, and ultrasonically emulsifying and dispersing for 5min at the temperature of 5 ℃ and the power of 1800W to obtain emulsion A which is oil-in-water fish oil Pickering emulsion, wherein the average particle size of the emulsion is 33 mu m, and the viscosity of the emulsion is 331 Pa.s;
(3) Adding the NMN/CNF aqueous solution obtained in the step (1) into the emulsion A to ensure that the mass fraction of an oil phase is 45%, and performing shear emulsification at 5 ℃ for 10min by using a shear emulsifier at 5000rpm to obtain emulsion B, namely water-in-oil-in-water fish oil Pickering emulsion, wherein the average particle size of the emulsion is 34 mu m, and the viscosity of the emulsion is 477 Pa s. After the emulsion is placed for 180 days at normal temperature, no phase body is separated out, and no demulsification phenomenon occurs. The obtained water-in-oil-in-water fish oil Pickering emulsion was subjected to microscopic observation, and the picture is shown in FIG. 2. As can be seen from the figure, the Pickering emulsion had relatively uniformly dispersed water-in-oil fish oil droplets, and each of the droplets was also coated with water-in-oil fish oil. The middle phase body sandwiched by the outer water phase and the innermost water phase is an oil phase containing NMN/CNF ingredients.
Example 3 preparation of water in oil in water corn oil Pickering emulsion
(1) Mixing beta-Nicotinamide Mononucleotide (NMN) and cellulose nanofibers (amino CNF, the average diameter is 72nm, the average length is 6.7 microns) according to a mass ratio of 1 to 12, adding deionized water to enable the mass fraction of the CNF to be 1.2%, and performing ultrasonic emulsification and dispersion for 15min at the temperature of 10 ℃ and the power of 2000W to obtain an NMN/CNF aqueous solution, wherein the average particle size of the NMN/CNF composite particles is 271nm;
(2) Mixing the NMN/CNF aqueous solution obtained in the step (1) with medical refined corn oil containing 33.33% of vitamin E according to the mass fraction of an oil phase of 60%, and performing ultrasonic emulsification and dispersion at 10 ℃ and 2000W for 15min to obtain an emulsion A which is an oil-in-water type corn oil Pickering emulsion, wherein the average particle size of the emulsion is 18.5 mu m, and the viscosity of the emulsion is 417Pa & s;
(3) Adding the NMN/CNF aqueous solution obtained in the step (1) into the emulsion A to ensure that the mass fraction of an oil phase is 55%, and performing shear emulsification at 5 ℃ for 10min by using a shear emulsifier at 15000rpm to obtain emulsion B, namely water-in-oil-in-water corn oil Pickering emulsion, wherein the average particle size of the emulsion is 27.2 mu m, and the viscosity of the emulsion is 451 Pa.s. After the emulsion is placed for 180 days at normal temperature, no phase body is separated out, and no demulsification phenomenon occurs.
EXAMPLE 4 preparation of Water in oil in Water type Olive oil Pickering emulsion
(1) Mixing beta-Nicotinamide Mononucleotide (NMN) and cellulose nanofibers (amino CNF, the average diameter is 72nm, the average length is 6.7 microns) according to a mass ratio of 1 to 20, adding deionized water to enable the mass fraction of the CNF to be 3%, and performing ultrasonic emulsification and dispersion for 20min at 20 ℃ and 3000W power to obtain an NMN/CNF aqueous solution, wherein the average particle size of the NMN/CNF composite particles is 592nm;
(2) Mixing the NMN/CNF aqueous solution obtained in the step (1) with olive oil containing hydroxytyrosol according to the oil phase mass fraction of 78%, and performing ultrasonic emulsification and dispersion for 20min at 20 ℃ under 3000W power to obtain emulsion A which is oil-in-water type olive oil Pickering emulsion, wherein the average particle size of the emulsion is 55.2 mu m, and the viscosity of the emulsion is 529Pa & s;
(3) Adding the NMN/CNF aqueous solution obtained in the step (1) into emulsion A to ensure that the mass fraction of an oil phase is 70%, and performing shear emulsification at 20000rpm for 20min by using a shear emulsifier at 20 ℃ to obtain emulsion B, namely water-in-oil-in-water type olive oil Pickering emulsion, wherein the average particle size of the emulsion is 57.2 mu m, and the viscosity of the emulsion is 671Pa s. After the emulsion is placed for 180 days at normal temperature, no phase body is separated out, and no demulsification phenomenon occurs.
Comparative example 1
An oil-in-water sunflower seed oil Pickering emulsion was prepared as in example 1, except that: the sonication and shear emulsification temperatures were 25 ℃. The finally obtained emulsion B coalesces, delaminates and breaks during storage at ambient temperature (25 ℃,180 days), which indicates that the emulsification temperature has a significant influence on the stability of the finally obtained Pickering emulsion during the preparation process.
Comparative example 2
An oil-in-water sunflower seed oil Pickering emulsion was prepared as in example 1, except that: when preparing the emulsion A, a shearing emulsifying machine is adopted to shear and emulsify for 2min at 1000rpm, and the average grain diameter of the obtained emulsion is 20 mu m. The emulsion B finally obtained is not a water-in-oil-in-water emulsion.
An oil-in-water sunflower oil Pickering emulsion was prepared as in example 1, except that: when emulsion B is prepared, if 600W ultrasonic emulsification dispersion is adopted for 2min, the prepared emulsion B is not water-in-oil-in-water emulsion.
This indicates that the emulsification process has a significant effect on the state of the final emulsion B during the emulsion preparation.
Claims (9)
1. A preparation method of a water-in-oil-in-water Pickering emulsion is characterized by comprising the following steps:
(1) Mixing beta-nicotinamide mononucleotide and cellulose nanofiber, adding water, and performing ultrasonic dispersion to obtain an NMN/CNF aqueous solution;
(2) Mixing the NMN/CNF aqueous solution with grease, and performing ultrasonic emulsification to obtain emulsion A;
(3) Adding the NMN/CNF aqueous solution into the emulsion A, and mechanically shearing and emulsifying to obtain emulsion B, namely water-in-oil-in-water Pickering emulsion;
the mass ratio of the beta-nicotinamide mononucleotide to the cellulose nanofiber is 1-1; the concentration of the cellulose nano-fibers in the NMN/CNF aqueous solution is 0.1% -3%;
in the step (2), the temperature of ultrasonic emulsification is 0-20 ℃;
in the step (3), the temperature of the mechanical shearing emulsification is 0-20 ℃;
in the step (2), the power of ultrasonic emulsification is 600-3000W; the time is 2-20min;
in the step (3), the rotating speed of the mechanical shearing emulsification is 1000-20000rpm; the time is 1-30min;
in the emulsion A, the mass fraction of the grease is 50% -78%; in the emulsion B, the mass fraction of the grease is 15-70%.
2. The method according to claim 1, wherein the cellulose nanofibers are cationic aminated nanocellulose fibers having a diameter of 30-100nm and a length of 1-10 μm.
3. The method according to claim 1, wherein the fat or oil is selected from an animal or vegetable oil or a solution in which an animal or vegetable oil is used as a solvent.
4. The method according to claim 3, wherein the animal or vegetable oil is selected from the group consisting of fish oil, sunflower oil, corn oil, soybean oil, olive oil, and plant essential oil.
5. The method according to claim 3, wherein the solution containing animal or vegetable oil as a solvent is selected from vegetable oil containing fat-soluble vitamins, algae oil containing DHA, and soybean oil containing soybean isoflavone.
6. A Pickering emulsion of water-in-oil-in-water type obtained by the preparation method according to any one of claims 1 to 5.
7. A product comprising the water-in-oil-in-water Pickering emulsion of claim 6.
8. The product according to claim 7, wherein the product is selected from the group consisting of food, pharmaceutical, and cosmetic products.
9. The product of claim 8, wherein the food product is a health food product.
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