CN110946285A - Preparation method of water-in-oil Pickering emulsion based on phytosterol stabilization - Google Patents
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Abstract
The invention belongs to the field of water-in-oil emulsion, and discloses a water-in-oil Pickering emulsion based on phytosterol stabilization, and a preparation method and application thereof. The water-in-oil Pickering emulsion is prepared by the following method: dispersing phytosterol in absolute ethyl alcohol, heating and dissolving to obtain an ethanol solution of the phytosterol, mixing the ethanol solution with water, removing ethanol to obtain a water dispersion of phytosterol particles, and mixing the water dispersion with an oil phase and homogenizing to obtain a water-in-oil Pickering emulsion; or drying the water dispersion to obtain phytosterol powder, dispersing the phytosterol powder in the oil phase, mixing with water, and homogenizing to obtain water-in-oil Pickering emulsion. Compared with the traditional preparation method of the water-in-oil type particle stabilizer, the method can be used for producing the water-in-oil type Pickering emulsion with good stability without adding a surfactant or chemical modification, has simple process and is easy to realize industrialization.
Description
Technical Field
The invention belongs to the field of water-in-oil emulsion, and particularly relates to water-in-oil Pickering emulsion based on phytosterol stability, and a preparation method and application thereof.
Background
The water-in-oil type emulsion is an important emulsion system type and has wide application prospect in food, chemical industry and other related fields. For example, margarine is a water-in-oil emulsion used as a substitute for animal butter, and most cosmetic creams are also water-in-oil emulsions. Water-in-oil emulsions are also good carriers for entrapping water-soluble active substances.
Traditionally, the formation of water-in-oil emulsions requires the use of large amounts of surfactants, which can create environmental and safety concerns. The emulsion based on particle stabilization (i.e., Pickering emulsion) has the advantages of small using amount of emulsifier, high emulsion stability, no surfactant and the like. At present, most of particles for stabilizing Pickering emulsion are inorganic and organic synthetic particles, and the application of the particles in the industries of food, medicine and the like is very limited. Although some food-grade or bio-derived particles have been found to be useful for Pickering emulsion stabilization, they are useful for stabilizing oil-in-water emulsions. The food-grade particles which can be used for the water-in-oil Pickering emulsion are very few, and only comprise fat crystals, polyphenol crystals and the like.
Phytosterols are a series of natural compounds with cholesterol-like structures that lower blood cholesterol. It is believed that the administration of 2-3g of phytosterol per day is effective in reducing blood low density lipoprotein by 10-15%. However, its low water solubility and even fat solubility greatly limit its application in food and pharmaceutical oral formulations. The solubility and bioavailability are currently improved mainly by the following means: 1) esterification with fatty acid improves the fat solubility; 2) forming nanoparticles in the presence of a stabilizer; 3) embedded in an oil-in-water emulsion. However, very few studies have been made on the use of phytosterols as emulsion (especially water-in-oil) stabilizers, with the exception of few protein-stabilized phytosterol particles. The stable water-in-oil Pickering emulsion based on the phytosterol is natural and safe, has functionality, can be used for embedding water-soluble active substances, and has huge application prospects in the industries of food, medicine, cosmetics and the like.
Nevertheless, research on food-grade water-in-oil type Pickering emulsions has not progressed much at home and abroad. The reason for this is the lack of food grade particles that can be used to stabilize water-in-oil Pickering emulsions. The particles currently used for stabilizing the water-in-oil Pickering emulsion are mainly synthetic particles, such as hydrophobic silicon particles, modified cellulose, polystyrene colloidal particles, micro-gels and the like. However, for the application fields of soft materials requiring biocompatibility, such as food, medicine, cosmetics and the like, the development of a Pickering emulsion stabilizer obtained based on natural, degradable and renewable resources is urgently needed.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a preparation method of a water-in-oil Pickering emulsion based on phytosterol stabilization.
The invention also aims to provide the water-in-oil Pickering emulsion prepared by the method and stabilized based on the phytosterol.
The purpose of the invention is realized by the following scheme:
a preparation method of a water-in-oil Pickering emulsion based on phytosterol stabilization comprises the following steps:
(1) dispersing phytosterol in absolute ethyl alcohol, and heating and dissolving to obtain an ethanol solution of the phytosterol;
(2) mixing the ethanol solution of the phytosterol obtained in the step (1) with water, and then removing the ethanol to obtain an aqueous dispersion of phytosterol particles;
(3) mixing the water dispersion of the phytosterol particles obtained in the step (2) with an oil phase, and homogenizing to obtain a water-in-oil Pickering emulsion;
alternatively, the first and second electrodes may be,
(4) drying the aqueous dispersion of the phytosterol particles obtained in the step (2) to obtain phytosterol powder, dispersing the phytosterol powder in an oil phase, mixing with water, and homogenizing to obtain a water-in-oil Pickering emulsion.
Relatively speaking, under the condition of the same total sterol content, the particle size of the emulsion produced by using high-purity sterol is more uniform, so that the phytosterol in the step (1) preferably refers to the phytosterol with the total sterol content of more than or equal to 95%, wherein the phytosterol is β -sitosterol, campesterol, brassicasterol and stigmasterol, preferably one or a mixture of β -sitosterol, campesterol, brassicasterol and stigmasterol, however, the commercial price of the mixed sterol is obviously lower than that of the high-purity sterol, so that the mixed phytosterol has industrial and commercial significance.
The heating and dissolving in the step (1) is preferably carried out at 45-85 ℃ for 5-10 min to obtain an ethanol solution of the phytosterol, and is preferably carried out at 45 ℃ for 10 min;
the dosage of the phytosterol and the ethanol in the step (1) meets the following requirements: adding 0.05-0.12 kg of phytosterol powder into every 10L of absolute ethyl alcohol, preferably adding 0.08-0.10 kg of phytosterol powder into every 10L of absolute ethyl alcohol;
the dosage of the ethanol solution of the phytosterol and the water in the step (2) meets the requirement that the volume ratio of the ethanol solution of the phytosterol to the water is 1-8: 9-2;
the mixing in the step (2) is preferably carried out by homogenizing for 1-4 minutes under the condition of 1000-10000 r/min;
removing the ethanol in the step (2) preferably by rotary evaporation and concentrating to 2-4% (kg phytosterol/L water);
the oil phase in the step (3) and the oil phase in the step (4) are relatively and independently a non-polar solvent or vegetable oil; the vegetable oil is preferably at least one of soybean oil, corn oil and blend oil, and the nonpolar solvent is preferably at least one of n-hexane, dodecane and ethyl acetate;
the volume ratio of the water dispersion liquid of the phytosterol particles to the oil phase in the step (3) is 3-7: 7-3;
homogenizing in the step (3) and the step (4) is to homogenize for 1-3 minutes under the condition of 1000-10000 r/min;
the amount of the plant sterol powder and the oil phase in the step (4) of dispersing the plant sterol powder in the oil phase meets the following requirements: setting the saturated concentration of the phytosterol in the oil phase at normal temperature as X% w/v, wherein the unit of w is kg, the unit of v is L, and correspondingly adding more than or equal to (X +0.5) kg of phytosterol powder into each 100L of oil phase to form a dispersion liquid; the water consumption in the step (4) meets the following requirements: the volume ratio of the dispersion liquid formed by dispersing the phytosterol powder in the oil phase to water is 3-7: 7-3, and preferably 3-5: 7-5.
A stable water-in-oil Pickering emulsion based on phytosterol prepared by the above method.
The water-in-oil type Pickering emulsion based on the stable phytosterol can be used as a nutritional food product, can also be used as an embedding carrier of a plurality of water-soluble active substances, and is widely used for development of functional (health care) food, medicines, cosmetics and the like. For example, the invention can be used to produce water-in-oil Pickering emulsions containing polypeptide actives to improve the stability of the actives.
The mechanism of the invention is as follows:
the water-dispersed phytosterol particles are prepared by an anti-solvent precipitation method, in the process, the surface wettability of the phytosterol is slightly changed through self-assembly (part of hydrophilic groups are exposed), and the phytosterol is changed from extremely hydrophobic to relatively hydrophobic, so that the water-in-oil Pickering emulsion can be stabilized. Water-dispersible phytosterol particles can also be frozen and dried to form phytosterol particle powder, and the powder still has certain amphipathy (mainly hydrophobicity) and can be used for stabilizing water-in-oil Pickering emulsion.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention adopts a new production process, does not need any additional stabilizer and produces the water-in-oil Pickering emulsion with good stability. The process solves the defects of the existing water-in-oil Pickering emulsion stabilizer preparation process.
2. The production process provided by the invention is simple, efficient, low in production cost, environment-friendly and safe, and is suitable for industrial production.
3. The water-in-oil type Pickering emulsion produced by the invention not only can be used as a nutritional food product, but also can be used as an embedding carrier of a plurality of water-soluble active substances, and can be widely used for developing functional (health care) foods, medicines, cosmetics and the like. For example, water-in-oil Pickering emulsions containing polypeptide actives, which may be produced in accordance with the present invention, are expected to greatly improve the stability of the actives.
4. The quality of the water-in-oil type Pickering emulsion produced by the invention can be adjusted by sterol particle concentration, water phase proportion and oil phase type, and the specific formula can be conveniently adjusted according to actual requirements, so that a series of water-in-oil type Pickering emulsions with different properties can be produced.
Drawings
FIG. 1 is a schematic diagram of the mechanism of the present invention;
FIG. 2 is an appearance and optical microscope photograph of the water-in-oil Pickering emulsion prepared in example 1;
FIG. 3 is an appearance and optical microscope photograph of the water-in-oil Pickering emulsion prepared in example 2;
FIG. 4 is an appearance and optical microscope photograph of the water-in-oil Pickering emulsion prepared in example 3;
FIG. 5 is an appearance and optical microscope photograph of the water-in-oil Pickering emulsion prepared in example 4.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The reagents used in the examples are commercially available without specific reference.
Example 1
(1) Dispersing phytosterol (purchased from Shaanxi Haishi bioengineering Co., Ltd., wherein the total sterol content is more than or equal to 95%, β -sitosterol 55%, campesterol 30%, stigmasterol 10%, brassicasterol 0.49%) in absolute ethanol at normal temperature according to a solid-liquid ratio of 1:100, and then heating at 45 ℃ for 5min to obtain an ethanol solution of the phytosterol, wherein the solid dosage unit is kilogram and the liquid dosage unit is liter.
(2) Mixing the phytosterol ethanol solution with water according to the volume ratio of 5:5, simultaneously shearing and homogenizing at 10000 r/min for 2min, removing ethanol through rotary evaporation, and concentrating to 3% w/v to obtain a high-concentration phytosterol particle water dispersion; the unit of w is kilogram, and the unit of v is liter;
(3) mixing the aqueous dispersion of the phytosterol particles with corn oil in a volume ratio of 5:5, and carrying out homogeneous dispersion for 2 minutes by a high-speed shearing machine under the condition that the rotating speed is 5000 r/min to obtain the water-in-oil Pickering emulsion. Through dyeing experiments and optical microscope observation, the appearance and the optical microscope image of the water-in-oil Pickering emulsion prepared in example 1 after being placed for 1 day are shown in figure 2, the obtained emulsion sample is the water-in-oil emulsion, the particle size analysis shows that the average particle size is 88.3 microns, and the appearance and the particle size of the emulsion after being placed for 1 month are not obviously changed.
Example 2
(1) Dispersing phytosterol (purchased from Shaanxi Haishi bioengineering Co., Ltd., wherein the total sterol content is more than or equal to 95%, β -sitosterol 55%, campesterol 30%, stigmasterol 10%, brassicasterol 0.49%) in absolute ethanol at normal temperature according to a solid-liquid ratio of 1:100, and then heating at 85 ℃ for 5min to obtain an ethanol solution of the phytosterol, wherein the solid dosage unit is kilogram and the liquid dosage unit is liter.
(2) Mixing the phytosterol ethanol solution with water according to the volume ratio of 5:5, simultaneously shearing and homogenizing at 8000 rpm for 4min, removing ethanol by rotary evaporation, and concentrating to 2% w/v to obtain high-concentration phytosterol particle water dispersion; the units w are kilograms and v is liters.
(3) And mixing the aqueous dispersion of the high-concentration phytosterol particles with dodecane according to the volume ratio of 5:5, and carrying out homogeneous dispersion for 2 minutes by using a high-speed shearing machine under the condition that the rotating speed is 5000 r/min to obtain the water-in-oil Pickering emulsion.
Through dyeing experiments and optical microscope observation, the appearance and the optical microscope image of the water-in-oil Pickering emulsion prepared in example 2 after being placed for 1 day are shown in figure 3, the obtained emulsion sample is the water-in-oil emulsion, the particle size analysis shows that the average particle size is 33.3 microns, and the appearance and the particle size of the emulsion after being placed for 1 month are not obviously changed.
Example 3
(1) Dispersing phytosterol (purchased from Shaanxi Haishi bioengineering Co., Ltd., wherein the total sterol content is more than or equal to 95%, β -sitosterol 55%, campesterol 30%, stigmasterol 10%, brassicasterol 0.49%) in absolute ethanol at normal temperature according to a solid-liquid ratio of 1:100, and then heating at 45 ℃ for 5min to obtain an ethanol solution of the phytosterol, wherein the solid dosage unit is kilogram and the liquid dosage unit is liter.
(2) Mixing the phytosterol ethanol solution with water according to the volume ratio of 3:7, simultaneously shearing and homogenizing for 2min at 1000 r/min, removing ethanol through rotary evaporation, and concentrating to 3% w/v to obtain a high-concentration phytosterol particle water dispersion; the units w are kilograms and v is liters.
(3) And mixing the aqueous dispersion of the high-concentration phytosterol particles with dodecane according to the volume ratio of 7:3, and carrying out homogeneous dispersion for 2 minutes by using a high-speed shearing machine under the condition that the rotating speed is 7000 r/min to obtain the water-in-oil Pickering emulsion.
The appearance and optical microscope image of the water-in-oil Pickering emulsion prepared in example 3 after being left for 1 day are shown in FIG. 4, and the obtained emulsion sample is water-in-oil emulsion; particle size analysis showed that the average particle size was 27.4 microns; the appearance and the particle size of the emulsion are not obviously changed after the emulsion is placed for 1 month.
Example 4
(1) Dispersing phytosterol (purchased from Shaanxi Haishi bioengineering Co., Ltd., wherein the total sterol content is more than or equal to 95%, β -sitosterol 55%, campesterol 30%, stigmasterol 10%, brassicasterol 0.49%) in absolute ethanol at normal temperature according to a solid-liquid ratio of 1:100, and then heating at 45 ℃ for 5min to obtain an ethanol solution of the phytosterol, wherein the solid dosage unit is kilogram and the liquid dosage unit is liter.
(2) Mixing the above phytosterol ethanol solution with water at ratio of 5:5, shearing, homogenizing at 10000 r/min for 2min, removing ethanol by rotary evaporation, and concentrating to 3.5% w/v to obtain high concentration phytosterol granule water dispersion; the units w are kilograms and v is liters.
(3) Freeze drying the dispersion to obtain the phytosterol particle powder.
(4) Dispersing the obtained phytosterol particle powder into dodecane at the concentration of 2% w/v (the saturation concentration of sterol in dodecane is 0.55% w/v at room temperature), mixing with water at the volume ratio of 5:5, and homogenizing and dispersing for 2 minutes by a high-speed shearing machine under the condition that the rotating speed is 5000 r/min to obtain the water-in-oil Pickering emulsion. The units w are kilograms and v is liters.
The appearance and optical microscope image of the water-in-oil Pickering emulsion prepared in example 4 after being left for 1 day are shown in FIG. 5, and the obtained emulsion sample is water-in-oil emulsion; particle size analysis showed that the average particle size was 41.9 microns; the appearance and the particle size of the emulsion are not obviously changed after the emulsion is placed for 1 month.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of a water-in-oil Pickering emulsion based on phytosterol stabilization is characterized by comprising the following steps:
(1) dispersing phytosterol in absolute ethyl alcohol, and heating and dissolving to obtain an ethanol solution of the phytosterol;
(2) mixing the ethanol solution of the phytosterol obtained in the step (1) with water, and then removing the ethanol to obtain an aqueous dispersion of phytosterol particles;
(3) mixing the water dispersion of the phytosterol particles obtained in the step (2) with an oil phase, and homogenizing to obtain a water-in-oil Pickering emulsion;
alternatively, the first and second electrodes may be,
(4) drying the aqueous dispersion of the phytosterol particles obtained in the step (2) to obtain phytosterol powder, dispersing the phytosterol powder in an oil phase, mixing with water, and homogenizing to obtain a water-in-oil Pickering emulsion.
2. The method of preparing a phytosterol-stabilized-water-in-oil Pickering emulsion as recited in claim 1, wherein:
the phytosterol in the step (1) is the phytosterol with the total sterol content of more than or equal to 95%.
3. The method of preparing a phytosterol-stabilized-based water-in-oil Pickering emulsion as recited in claim 2, wherein:
the phytosterol in the step (1) is at least one of β -sitosterol, campesterol, brassicasterol and stigmasterol.
4. The method of preparing a phytosterol-stabilized-water-in-oil Pickering emulsion as recited in claim 1, wherein:
the heating and dissolving in the step (1) is to heat at 45-85 ℃ for 5-10 min to obtain an ethanol solution of the phytosterol;
the dosage of the phytosterol and the ethanol in the step (1) meets the following requirements: 0.05-0.12 kg of phytosterol powder is correspondingly added into 10L of absolute ethyl alcohol.
5. The method of preparing a phytosterol-stabilized-water-in-oil Pickering emulsion as recited in claim 1, wherein:
the dosage of the ethanol solution of the phytosterol and the water in the step (2) meets the requirement that the volume ratio of the ethanol solution of the phytosterol to the water is 1-8: 9-2;
the mixing in the step (2) is to mix the mixture by homogenizing for 1 to 4 minutes under the condition of 1000 to 10000 r/min;
the step (2) of removing ethanol refers to removing ethanol by rotary evaporation and concentrating to 2-4 kg of phytosterol per 100L of water.
6. The method of preparing a phytosterol-stabilized-water-in-oil Pickering emulsion as recited in claim 1, wherein:
the oil phase in the step (3) is a non-polar solvent or vegetable oil;
the volume ratio of the water dispersion liquid of the phytosterol particles to the oil phase in the step (3) is 3-7: 7-3;
the homogenizing in the step (3) is homogenizing for 1-3 minutes under the condition of 1000-10000 r/min.
7. The method of preparing a phytosterol-stabilized-water-in-oil Pickering emulsion as recited in claim 1, wherein:
the oil phase in the step (4) is a non-polar solvent or vegetable oil;
homogenizing in the step (4) is to homogenize for 1-3 minutes under the condition of 1000-10000 r/min;
the amount of the plant sterol powder and the oil phase in the step (4) of dispersing the plant sterol powder in the oil phase meets the following requirements: setting the saturated concentration of the phytosterol in the oil phase at normal temperature as X% w/v, wherein the unit of w is kg, the unit of v is L, and correspondingly adding more than or equal to (X +0.5) kg of phytosterol powder into each 100L of oil phase to form a dispersion liquid; the water consumption in the step (4) meets the following requirements: the volume ratio of dispersion liquid formed by dispersing the phytosterol powder in the oil phase to water is 3-7: 7-3.
8. The method for preparing a phytosterol-stabilized-based water-in-oil Pickering emulsion as recited in claim 6 or 7, wherein the method comprises the following steps:
the vegetable oil is at least one of soybean oil, corn oil and blend oil, and the nonpolar solvent is at least one of n-hexane, dodecane and ethyl acetate.
9. A phytosterol-based stable water-in-oil Pickering emulsion prepared according to the method of any one of claims 1-8.
10. Use of a phytosterol-stabilized water-in-oil-based Pickering emulsion as claimed in claim 9 as a nutraceutical product and as an embedding carrier for water-soluble active substances.
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| CN201911199370.1A CN110946285B (en) | 2019-11-29 | 2019-11-29 | Preparation method of water-in-oil Pickering emulsion based on phytosterol stabilization |
| PCT/CN2020/130009 WO2021104144A1 (en) | 2019-11-29 | 2020-11-19 | Method for preparing oil-in-water pickering emulsion based on phytosterol stability |
| ZA2022/00292A ZA202200292B (en) | 2019-11-29 | 2022-01-05 | Method for preparing phytosterol-stabilized water-in-oil pickering emulsion |
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| CN112164800A (en) * | 2020-09-30 | 2021-01-01 | 东莞力朗电池科技有限公司 | Negative electrode material, negative electrode plate, preparation method of negative electrode plate and secondary battery |
| WO2021104144A1 (en) * | 2019-11-29 | 2021-06-03 | 暨南大学 | Method for preparing oil-in-water pickering emulsion based on phytosterol stability |
| CN113907355A (en) * | 2021-10-19 | 2022-01-11 | 南昌大学 | Water-phase crystallization type water-in-oil emulsion and preparation method thereof |
| CN114468062A (en) * | 2022-02-16 | 2022-05-13 | 江南大学 | Double-network zero-trans fat emulsion gel capable of being printed in 3D/4D mode and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021104144A1 (en) * | 2019-11-29 | 2021-06-03 | 暨南大学 | Method for preparing oil-in-water pickering emulsion based on phytosterol stability |
| CN112164800A (en) * | 2020-09-30 | 2021-01-01 | 东莞力朗电池科技有限公司 | Negative electrode material, negative electrode plate, preparation method of negative electrode plate and secondary battery |
| CN113907355A (en) * | 2021-10-19 | 2022-01-11 | 南昌大学 | Water-phase crystallization type water-in-oil emulsion and preparation method thereof |
| CN114468062A (en) * | 2022-02-16 | 2022-05-13 | 江南大学 | Double-network zero-trans fat emulsion gel capable of being printed in 3D/4D mode and preparation method thereof |
| WO2023155338A1 (en) * | 2022-02-16 | 2023-08-24 | 江南大学 | 3d/4d printable dual-network zero-trans fat emulsion gel and preparation |
| CN114468062B (en) * | 2022-02-16 | 2023-08-25 | 江南大学 | Dual-network zero-trans fat emulsion gel capable of being printed in 3D/4D mode and preparation method thereof |
Also Published As
| Publication number | Publication date |
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| WO2021104144A1 (en) | 2021-06-03 |
| ZA202200292B (en) | 2022-08-31 |
| CN110946285B (en) | 2023-03-24 |
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