CN113100417A - A kind of pollen particle-stabilized food-grade Pickering emulsion and preparation method thereof - Google Patents
A kind of pollen particle-stabilized food-grade Pickering emulsion and preparation method thereof Download PDFInfo
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- CN113100417A CN113100417A CN202110406204.5A CN202110406204A CN113100417A CN 113100417 A CN113100417 A CN 113100417A CN 202110406204 A CN202110406204 A CN 202110406204A CN 113100417 A CN113100417 A CN 113100417A
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Abstract
本发明公开了一种花粉粒子稳定的食品级Pickering乳液及其制备方法，该方法是将花粉粒子分散至水中形成水相，将所述水相与植物油油相混合后，进行超声和均质处理，即得食品级Pickering乳液。该食品级Pickering乳液高度分散、稳定性好，且富含蛋白质、脂质、黄酮、多糖、矿物质、维生素、多酚等多种具有保健功能的营养成分，满足食品、医药等领域的应用要求，且其制备方法简单、条件温和，有利于大规模生产。The invention discloses a food-grade Pickering emulsion stabilized by pollen particles and a preparation method thereof. The method comprises the steps of dispersing pollen particles in water to form an aqueous phase, mixing the aqueous phase with a vegetable oil phase, and performing ultrasonic and homogenization treatment. , that is, food-grade Pickering emulsion. The food-grade Pickering emulsion is highly dispersed, has good stability, and is rich in protein, lipid, flavonoids, polysaccharides, minerals, vitamins, polyphenols and other nutrients with health functions, meeting the application requirements in the fields of food and medicine. , and the preparation method is simple and the conditions are mild, which is favorable for large-scale production.
Description
Technical Field
The invention relates to a food-grade Pickering emulsion and a preparation method thereof, in particular to a food-grade Pickering emulsion with stable pollen particles and a preparation method thereof, and belongs to the technical field of Pickering emulsion processing.
Background
The Pickering emulsion is a novel emulsion prepared by stabilizing mutually incompatible water and oil phases by using solid (colloid) particles with hydrophilicity and hydrophobicity. The solid particles replace micromolecular surfactants in the traditional emulsion, so that the using amount of the micromolecular surfactants can be greatly reduced, the damage of the surfactants to organisms is avoided, the biocompatibility and the environment friendliness of the emulsion are improved, and more attention is paid to the solid particles in recent years.
As for the stable particles of Pickering emulsion, inorganic silicon particles, clay, metal oxide, high molecular polymer and the like have been most studied. The biocompatibility and degradability of the Pickering emulsion limit the application of the Pickering emulsion in the food and medicine industries. In recent years, the stable particles of Pickering emulsions have been expanded to biomass-derived amphiphilic macromolecules such as proteins, celluloses, polysaccharides, microorganisms, flavonoids, etc. The biological macromolecules have good biocompatibility, and the application prospect of the Pickering emulsion in the fields of food and medicine is greatly expanded. However, these particles are generally poorly dispersed and require modification and modification of their surface in order to be useful in the preparation of Pickering emulsions. Pollen (Pollen) is a male reproductive cell of a plant, produced by anthers in stamens. The pollen is used as the essence of plants, is rich in various bioactive substances such as protein, lipid, flavone, polysaccharide, mineral substances, vitamins, polyphenol and the like, has various effects of reducing blood pressure, enhancing human immunity, resisting aging, radiation and tumor, preventing and treating cardiovascular and cerebrovascular diseases, resisting oxidation and the like, and is a novel health food. At present, no related report for preparing food-grade Pickering emulsion by using natural pollen as stable particles exists.
Disclosure of Invention
Aiming at the defects existing in the preparation process of Pickering emulsion in the prior art, the invention aims to provide food-grade Pickering emulsion which is highly dispersed and has good stability and is rich in various health-care functional nutritional ingredients such as protein, lipid, flavone, polysaccharide, mineral substances, vitamins, polyphenol and the like, and the application requirements in the fields of food, medicine and the like are met.
The second purpose of the invention is to provide a method for preparing food-grade Pickering emulsion, which is simple to operate and low in raw material cost.
In order to achieve the technical purpose, the invention provides a preparation method of food-grade Pickering emulsion with stable pollen particles.
The key point of the invention is that natural pollen is used as stable particles to prepare Pickering emulsion, the natural pollen is a complex active biological macromolecule system and comprises a plurality of components such as protein, amino acid, polysaccharide, polyphenol, lipid, nucleic acid, cellulose, pectin and the like, and the active components simultaneously comprise a large number of hydrophobic groups and hydrophilic groups and have certain hydrophily-hydrophobicity. Particularly, the pollen is rich in nutrient components, has health care effect, and can expand the application of the Pickering emulsion in food and medicine. In addition, the pollen particles can be directly used as stable particles to prepare and obtain the stable Pickering emulsion without any modification, and the preparation method is simple to operate, low in cost and beneficial to large-scale popularization and application.
Preferably, the concentration of the pollen particles in the water phase is 30-300 mg/mL. If the concentration of the pollen particles in the aqueous phase is too low, the emulsion cannot be effectively stabilized, and the formed emulsion may have excessive aqueous phase or oil phase exuded after standing. If the concentration of the pollen particles in the aqueous phase is too high, part of the pollen particles cannot effectively participate in stabilizing the emulsion, and the excessive pollen particles cannot be distributed on the interface of the aqueous phase and the oil phase and can be dispersed in the aqueous phase or the oil phase, thereby causing waste of the pollen particles. Further, when the concentration of the pollen particles is too high, the droplet size of the produced Pickering emulsion is small, and therefore, it is more preferable that the concentration of the pollen in the aqueous phase is 100 to 200 mg/mL.
As a preferred embodiment, the pollen particles include at least one of lotus pollen, rape pollen, sunflower pollen, pine pollen, platycodon pollen, begonia pollen, scutellaria pollen and jasmine pollen. The lotus pollen is the most preferable, has certain medicinal efficacy, and has the effects of refreshing, cooling blood, removing heat toxin, eliminating dampness, dispelling wind and regulating endocrine; meanwhile, the lotus flower pollen contains hydrophobic components and also contains a large number of hydrophilic groups such as carboxyl, amino, hydroxyl and the like, and the hydrophilic-hydrophobic performance of the lotus flower pollen shows unique advantages in the aspect of preparing Pickering emulsion; and the lotus pollen is rich in nutrient components, so that the Pickering emulsion is endowed with a health-care effect, and the application range of the Pickering emulsion is expanded.
As a preferable scheme, the pH value of the water phase is in the range of 2.0-12.0. The pollen particles contain amphiphilic dissociation groups such as proteins, polysaccharides, amino acids, etc., and these groups dissociate to different degrees in solutions with different pH values, resulting in different charge conditions of the pollen particles in solutions with different pH values. The electrostatic action is one of the important mechanisms for stabilizing the Pickering emulsion by the particles, so that the pH of the water phase directly influences the properties of the prepared Pickering emulsion, including the stability of the emulsion, the type of the emulsion, the size of liquid drops and the like. Further preferably, the pH of the aqueous phase is in the range of 2 to 4 or 7 to 12, and when the pH is in the range of 5 to 6, the particle size of the formed emulsion droplets is large, and in this pH range, the surface charge of the pollen particles is low, so that the stable emulsion is difficult to disperse well, and even slight agglomeration may occur before the emulsion is formed.
As a preferable scheme, the volume percentage of the water phase and the vegetable oil phase is 20-50% to 50-80%. In a preferable proportion range, as the volume fraction of the oil phase is reduced, the particle size of the emulsion liquid drops is reduced, so that pollen particles can be favorably and fully adsorbed and distributed on the interface of water and oil to form uniform liquid drops with small particle size, and as the volume fraction of the oil phase is increased, the pollen particles are not enough to completely cover the interface of water and oil, the liquid drops are tightly stacked together, and part of the interface structure is damaged, so that the volume percentage composition of the water phase and the vegetable oil phase is further preferably 30-40% to 60-70%.
As a preferred embodiment, the vegetable oil includes at least one of rapeseed oil, peanut oil, sesame oil, corn oil, olive oil, sunflower oil, rice bran oil, soybean oil, and algal oil. The preferable vegetable oil can form stable Pickering emulsion with the aqueous phase containing pollen particles, and the vegetable oil is adopted to meet the preparation requirement of food-grade Pickering emulsion.
As a preferable mode, the homogenization treatment conditions are: the shearing speed of the homogenizer is 2000-15000 r/min, and the time is 1-10 min.
The invention also provides a food-grade Pickering emulsion which is prepared by the preparation method.
The pollen related to the invention is a conventional commercial product, and can be used for preparing Pickering emulsion only by crushing, sieving and drying pretreatment after purchase. The sieve is generally a No. 2 sieve. Drying is vacuum drying at 50 ℃.
Compared with the prior art, the technical scheme of the invention has the following beneficial technical effects:
the food-grade Pickering emulsion provided by the invention has the characteristics of high dispersion, good stability and the like, can form a stable gel state after being placed for one month, is basically free from water and oil phase exudation, utilizes pollen particles to introduce various nutritional ingredients with health care functions such as protein, lipid, flavone, polysaccharide, mineral substances, vitamins, polyphenol and the like, and meets the application requirements in the fields of food, medicine and the like.
The preparation method of the food-grade Pickering emulsion provided by the invention is simple to operate, low in raw material cost and beneficial to large-scale production.
Drawings
FIG. 1 is a scanning electron microscope (a in FIG. 1) and a partial enlarged view (b in FIG. 1) of lotus pollen particles after crushing and sieving.
Fig. 2 shows the results of the sieving of the pulverized lotus pollen particles in the oil phase (a in fig. 2) and the aqueous phase (PBS buffer, pH 8.0,
dispersion in b) in fig. 2.
FIG. 3 is an appearance of Pickering emulsion prepared in example 1.
FIG. 4 shows the dispersion of the Pickering emulsion prepared in example 2 in water and in the oil phase.
FIG. 5 is an appearance graph of Pickering emulsions prepared from different concentrations of pollen particles in water phase in example 3 at different time periods.
Fig. 6 is an appearance diagram (a in fig. 6) and its average particle size (b in fig. 6) of Pickering emulsions prepared in different water phase and oil phase ratios of example 4 at different time periods.
FIG. 7 is a graph of the distribution of droplet sizes for the different Pickering emulsions of example 5 prepared from aqueous phases of different pH.
Detailed Description
The following examples are intended to further illustrate the present disclosure, but not to limit the scope of the claims.
The pollen referred to in the following examples was purchased from Henan Progami bee products GmbH. Pulverizing the obtained flos Nelumbinis pollen with pulverizer, sieving with No. 2 sieve, and vacuum drying at 50 deg.C.
Example 1
Before the preparation of the Pickering emulsion, the dispersibility of lotus pollen particles in the water phase and the oil phase was tested. Adding a small amount of lotus pollen particles into soybean oil and water phase (PBS buffer solution, pH 8), shaking, ultrasonic dispersing for 10min, and observing the dispersion condition of pollen particles in the two phases. As shown in FIG. 2, lotus pollen has poor dispersibility in oil phase, rapidly sinks to the bottom of soybean oil (a in FIG. 2), and can be uniformly dispersed in water phase (b in FIG. 2).
Preparation of food-grade Pickering emulsion: 0.45g of dried lotus pollen particles were dispersed in 3mL of PBS buffer (pH 8) and sonicated for 20 min. Mixing with corn oil at a volume ratio of 3:7, and ultrasonically dispersing for 10 min. Then shearing at a high speed of 10000rpm/min for 5min by using a handheld homogenizer to obtain the Pickering emulsion with stable lotus pollen particles.
The Pickering emulsion prepared in this example is pale yellow (a in FIG. 3), stable in nature, and only a small amount of water in the lower layer (b in FIG. 3) separated out after standing at room temperature for 4 days. The emulsion was allowed to stand at room temperature for 1 month without any significant change, gradually became gel-like and was inverted (c in FIG. 3). The emulsion prepared under the condition is in a cream shape as a whole, gradually solidifies after being placed for a period of time, and does not have obvious demixing and oil phase exudation after being placed for one month.
Example 2
Preparation of food-grade Pickering emulsion: 0.30g of dried plum-leaf crab pollen particles were dispersed in 3mL of PBS buffer (pH 8) and ultrasonically dispersed for 10 min. Mixing with soybean oil at a volume of 3:7, and performing ultrasonic treatment for 15 min. And then shearing at a high speed of 8000rpm/min for 3min by using a homogenizer to obtain the Pickering emulsion with stable plum-leaf crab pollen particles.
To further verify the type of emulsion prepared (oil-in-water or water-in-oil), several points of the emulsion were added dropwise to the water and oil phases. As shown in fig. 4, after the emulsion was added dropwise to water, the droplets collapsed immediately and dispersed in water (screw bottle on the left side of fig. 4). If the emulsion droplets are added dropwise to toluene, the droplets retain their original appearance. This is a good indication that the Pickering emulsion prepared is an oil-in-water emulsion.
Example 3
Effect of pollen particle concentration on Pickering emulsion:
preparation of food-grade Pickering emulsion: dried lotus pollen particles (0.15 g, 0.30g, 0.50g, 0.75g, 1.00g, 1.50 g) were dispersed in 5mL of PBS buffer (pH 8) and ultrasonically dispersed for 20min, respectively. Mixing with corn oil at a volume ratio of 5:5, and ultrasonically dispersing for 20 min. Then shearing at a high speed of 10000rpm/min for 5min by using a handheld homogenizer to obtain the Pickering emulsion with stable lotus pollen particles.
Freshly prepared Pickering emulsion as in a of fig. 5, when the amount of lotus pollen particles used is greater than or equal to 0.50g, all water and oil participate in the formation of the emulsion. The emulsion gradually coagulates into cream after standing at room temperature for 4 days, and when the amount of lotus pollen particles is less than or equal to 0.50g, a small amount of water seeps out from the bottom of the emulsion. And the lower the amount of lotus pollen particles, the more water seeps out after the emulsion is placed. The emulsion had a small amount of water exuded after being left for one month. This is because when the amount of lotus pollen particles is too low, the lotus pollen particles in the system are not sufficiently distributed at the water-oil interface to form a "physical barrier", and either the aqueous phase or the oil phase cannot be completely emulsified, so that the emulsion will exude after standing. In the lotus pollen particle concentration range of this example, all emulsions were largely sufficient to resist droplet fusion. The creaming degree of the emulsion is higher with the increase of the concentration of the lotus pollen particles, and on the other hand, the high concentration of the lotus pollen particles can promote the formation of gelation.
Example 4
Effect of water-oil ratio on Pickering emulsion:
preparation of food-grade Pickering emulsion: 3.00g of dried lotus pollen particles were dispersed in 20mL of PBS buffer (pH 8) and sonicated for 20 min. Mixing 2mL, 3mL, 4mL, 5mL and 6mL of pollen dispersion with corn oil according to the volume of 2:8, 3:7, 4:6, 5:5 and 6:4, then shearing at a high speed of 10000rpm/min by using a handheld homogenizer for 5min to obtain a Pickering emulsion with stable lotus pollen particles, and researching the influence of the water-oil ratio on the visual appearance of the emulsion and the particle size of emulsion droplets under a fixed lotus pollen particle concentration. Freshly prepared emulsions as in fig. 6, the water phase and the oil phase all participate in forming the emulsion when the volume ratio of the water phase to the oil phase is 2: 8. As the amount of the aqueous phase increases, the lower layer of the emulsion gradually bleeds more aqueous phase. As the oil phase volume fraction decreases from 0.8 to 0.4, the droplet size of the emulsion decreases from 28.9 μm to 7.8 μm (see b in FIG. 6). Increasing the volume fraction of the oil phase can result in a higher volume fraction of the emulsified phase (emulsion) and larger droplet size. When the proportion of the oil phase is low, lotus pollen particles can be fully dripped and adsorbed and distributed on the interface of water and oil to form liquid droplets with uniform particle size. When the proportion of the oil phase is high, pollen particles are not enough to completely cover the water-oil interface, liquid drops are tightly packed together, and part of the interface structure is damaged.
Example 5
Influence of the pH of the dispersed phase (aqueous phase) of lotus pollen particles on the preparation of Pickering emulsion:
dispersing dried lotus pollen particles into PBS buffer (pH 8), performing ultrasonic dispersion for 20min to form dispersion liquid with the concentration of 150mg/mL, dividing the dispersion liquid into 7 parts with equal amount, respectively adjusting the pH value of the dispersion liquid to 2, 3, 5, 6, 8, 10 and 12 by using 1mol/L dilute hydrochloric acid or 1mol/L NaOH solution, respectively, adding soybean oil according to the volume ratio of an aqueous phase to an oil phase of 3:7, shearing and homogenizing for 5min at 10000rpm of a handheld homogenizer to prepare Pickering emulsion with stable pollen particles, and researching the influence of the pH value on the emulsion stability. The particle size distribution of the emulsion droplets can well reflect the stability of the emulsion. Within the pH range of this example, the emulsion is monodisperse. From the appearance of the emulsion, almost all emulsions have similar morphology, the droplet size of the emulsion is about 20-60 μm (fig. 7), and when the pH value of the water phase is 5.0 and 6.0, the droplet size of the emulsion is larger, because the lotus pollen particle surface charge is low, the emulsion is difficult to disperse well and stabilize, and even slight agglomeration may occur before the emulsion is formed, so that the particles cannot be effectively adsorbed and distributed on the interface of the water phase when the emulsion is formed, and the low charge amount on the particle surface is insufficient to provide sufficient electrostatic repulsion to resist flocculation and fusion of the droplets.
Example 6
Preparing Pickering emulsion by using the pinus thunbergii pollen particles:
dispersing 0.75g of dried pinus thunbergii pine pollen into 5mL of PBS buffer (pH 8), ultrasonically dispersing for 20min to form a dispersion liquid with the concentration of 150mg/mL, mixing the dispersion liquid with soybean oil according to the volume ratio of an aqueous phase to an oil phase of 3:7, shearing and homogenizing for 5min at 10000rpm of a handheld homogenizer to obtain the Pickering emulsion stabilized by the pine pollen. The prepared emulsion is light yellow in appearance and stable in property, gradually turns into a gel after being placed at room temperature for 4 days, no excessive water phase or oil phase seeps out, and the average droplet size of the emulsion is about 14 mu m.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and the technical solution and the inventive concept thereof according to the present invention should be equally exchanged or changed within the scope of the present invention.
Claims (10)
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| JP2000189052A (en) * | 1998-12-25 | 2000-07-11 | Asahi Denka Kogyo Kk | Edible oil and fat composition containing pollen |
| US20140350168A1 (en) * | 2011-09-22 | 2014-11-27 | Ariel-University Research And Development Company Ltd. | Emulsions and methods of making emulsions |
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|---|---|---|---|---|
| JP2000189052A (en) * | 1998-12-25 | 2000-07-11 | Asahi Denka Kogyo Kk | Edible oil and fat composition containing pollen |
| US20140350168A1 (en) * | 2011-09-22 | 2014-11-27 | Ariel-University Research And Development Company Ltd. | Emulsions and methods of making emulsions |
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| CN113907355A (en) * | 2021-10-19 | 2022-01-11 | 南昌大学 | A kind of water-phase crystalline water-in-oil emulsion and preparation method thereof |
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Application publication date: 20210713 Assignee: HENAN ZHUO YU BEES INDUSTRY Co.,Ltd. Assignor: XUCHANG University Contract record no.: X2024980025982 Denomination of invention: A food grade Pickering lotion stabilized by pollen particles and its preparation method Granted publication date: 20231027 License type: Common License Record date: 20241118 |