CN111700265A - Preparation method and application of collagen-based pickering emulsion - Google Patents
Preparation method and application of collagen-based pickering emulsion Download PDFInfo
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- CN111700265A CN111700265A CN202010307609.9A CN202010307609A CN111700265A CN 111700265 A CN111700265 A CN 111700265A CN 202010307609 A CN202010307609 A CN 202010307609A CN 111700265 A CN111700265 A CN 111700265A
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- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
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Abstract
The invention discloses a preparation method and application of a collagen-based pickering emulsion, which specifically comprises the following steps: preparing collagen fibers into a suspension, and homogenizing to obtain a collagen fiber dispersion liquid; mixing the collagen fiber dispersion liquid and the dispersed phase according to a proportion to form an oil-water mixture; emulsifying the oil-water mixture to obtain the Pickering emulsion. The method has the advantages that the stabilizer is formed by the collagen fibers, and then the pickering emulsion is prepared, the preparation method is simple to operate, the prepared pickering emulsion has excellent stability and is in a gel-like state, and the pickering emulsion can be used as a food ingredient to be added into beverages, dairy products, meat products, baked foods and the like, and can be used as an oil-retaining and water-retaining agent to be added into cosmetics.
Description
Technical Field
The invention relates to the technical field of emulsion preparation, in particular to a preparation method and application of Pickering emulsion.
Background
Pickering emulsions are emulsions that form a physical barrier at the oil-water interface to prevent droplet aggregation by replacing traditional surfactants with solid particles, originally discovered by Ramsden in 1903 and formally proposed by Pickering in 1907. Compared with the traditional surfactant for preparing the emulsion, the pickering emulsification technology has the characteristics of less emulsifier dosage, low cost, high safety and the like, is high in stability, has the characteristics of long stability time, less foam, reproducibility and the like, and has excellent application prospects in the aspects of structural modification, heat reduction, coating, bioactive compound transmission and the like. At present, Pickering emulsification is mainly used in the preparation process of foods, such as dairy products, ice cream, beverages and the like, so that the prepared products have uniform texture, good mouthfeel and stronger stability; in addition, the pickering emulsion added into the meat product can replace animal fat, and is a potential good way for controlling the fat intake.
The solid particles currently used to prepare pickering emulsions are generally divided into two categories: inorganic particles and organic particles. Wherein the inorganic particles mainly comprise modified silicon dioxide, titanium dioxide, clay particles and the like. The organic particles mainly comprise protein, polysaccharide, nano-cellulose and small molecular substances with biological activity, such as flavone, phytosterol and the like, and are more suitable for green processing due to the characteristics of degradability, good biocompatibility, sustainability, no toxicity and the like, and are particularly suitable for application in the field of food. In the food field, the stabilizing agent for the pickering emulsion is mainly derived from starch, vegetable protein and the like, and the research on the fibrous emulsifier for preparing the pickering emulsion is relatively less.
Therefore, it is an urgent problem for those skilled in the art to provide a new method for preparing pickering emulsion using fibrous emulsifier.
Disclosure of Invention
In view of the above, the invention provides a preparation method and application of a collagen-based pickering emulsion, wherein a stabilizer is formed by collagen fibers, and then pickering emulsion is prepared.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the Pickering emulsion is characterized by comprising the following steps:
(1) preparing collagen fibers into a suspension, and homogenizing to obtain a collagen fiber dispersion liquid;
(2) mixing the collagen fiber dispersion liquid and the dispersed phase according to a proportion to form an oil-water mixture;
(3) emulsifying the oil-water mixture to obtain the Pickering emulsion.
The beneficial effects of the preferred technical scheme are as follows: the invention prepares the collagen fiber into the collagen fiber dispersion liquid, and utilizes the nano-scale collagen fiber as the stabilizer, thereby improving the stability of the Pickering emulsion.
Preferably, in the step (1), the collagen fibers are dissolved in an acetic acid solution to form a suspension, wherein the pH of the suspension is 1-5, and the mass concentration of the collagen fibers is 0.01-10%; the concentration of the acetic acid solution is 0.1-1 mol/L.
Preferably, the collagen fibers in step (1) are obtained by mechanical stripping from acid-swollen or non-acid-swollen cowhide; or the collagen fiber is collagen extracted by acid or enzyme, and the collagen is in a fibrous shape.
Preferably, the length of the collagen fiber in the step (1) is 600-900 nm, and the diameter is 20-100 nm.
Preferably, in the step (1), the homogenizing pressure is 10-300 MPa, the homogenizing times are 1-20 times, and the collagen fiber dispersion liquid has a nanometer size.
Preferably, the dispersed phase in the step (2) is functional fatty acid or plant active lipid compound; the functional fatty acid comprises algae oil or fish oil; the plant active lipid compound comprises plant essential oil.
Preferably, the collagen fiber dispersion liquid and the dispersed phase in the step (2) are in a mass ratio of (10-99.9): (0.1-90) mixing.
Preferably, the emulsification in the step (3) comprises a homogenizing, ultrasonic or micro-jetting mode; the homogenizing pressure is 10-150MPa, and the times are 1-20.
The invention also provides an application of the pickering emulsion prepared by the method in food or cosmetics.
The beneficial effects of the preferred technical scheme are as follows: the Pickering emulsion prepared by the invention can be added into beverages, dairy products, meat products, baked foods and the like by taking an emulsion layer as a food ingredient in a full emulsion mode or centrifugation mode; and can be used as a water retention agent to be added into cosmetics, and has excellent using effect.
According to the technical scheme, compared with the prior art, the invention discloses a preparation method and application of a Pickering emulsion, and the preparation method has the following beneficial effects:
(1) the invention adopts the collagen fiber as the stabilizer, the collagen fiber is a protein fiber, the amphipathy and the flexibility are good, compared with the traditional mode that the spherical solid particles are used as the stabilizer, the fibrous emulsifier has higher length-width ratio, the structure is easier to regulate and control, and the Pickering emulsification effect is excellent.
(2) Compared with other protein fibers, the collagen fiber of the invention has simple, convenient and green preparation method and can realize mass production.
(3) The pickering emulsion prepared by utilizing the collagen fibers has high stability and wide application range.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a diagram of collagen fiber morphology under atomic force microscope observation provided by the present invention;
FIG. 2 is a graph showing the Zeta potential variation trend of the collagen fiber provided by the invention along with pH;
FIG. 3 is a drawing of a Pickering emulsion staining confocal scanning microscope image (Nile red labeled seaweed oil, Nile blue A labeled collagen fiber) provided by the present invention;
FIG. 4 is a drawing showing a visual observation and an optical microscope image of a stable Pickering emulsion containing collagen fibers of different concentrations according to the present invention; wherein a is before centrifugation, and b is after centrifugation;
FIG. 5 is a graph showing the dynamic viscoelasticity of Pickering emulsions stabilized with different concentrations of collagen fibres as a function of stress and frequency.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a preparation method of Pickering emulsion, which specifically comprises the following steps:
(1) dissolving collagen fibers in an acetic acid solution to form a suspension with the pH of 1-5 and the mass concentration of the collagen fibers of 0.1-10%, wherein the length of the collagen fibers is 600-900 nm, and the diameter of the collagen fibers is 20-100 nm; homogenizing to obtain nanometer collagen fiber dispersion liquid, wherein the homogenizing pressure is 10-300 MPa, and the homogenizing times are 1-20 times;
(2) mixing a collagen fiber dispersion liquid and a dispersion phase according to the mass ratio of (10-99.9): (0.1-90) mixing to form an oil-water mixture; the dispersed phase is functional fatty acid or plant active lipid compound; the functional fatty acid comprises algae oil or fish oil, and the plant active lipid compound comprises plant essential oil;
(3) emulsifying the oil-water mixture in a homogenizing, ultrasonic or micro-jetting mode to obtain a Pickering emulsion; homogenizing under 10-150MPa for 1-20 times;
in order to further optimize the technical scheme, the collagen fiber is obtained by mechanical stripping on cowhide which is or is not subjected to acid swelling; or the collagen fiber is collagen extracted by acid or enzyme, and the form of the collagen fiber is fibrous.
Example 1
The embodiment 1 of the invention discloses a preparation method of Pickering emulsion, which comprises the following steps:
(1) removing fat and impurity protein from cattle second-layer skin, washing the cattle second-layer skin with distilled water thoroughly to approach neutrality, cutting cattle hide into 5cm × 5cm pieces, and mixing the cattle hide with hydrochloric acid 1: 3(W/V) adding 0.5M hydrochloric acid, swelling at 4 deg.C for 24 hr, washing with hydrochloric acid, and carefully tearing collagen fibers from the swollen cowhide;
(2) dissolving collagen fibers in 0.1M acetic acid solution, preparing suspension with the concentration of 0.01 wt% respectively, adding the suspension into a high-pressure homogenizer, and setting the homogenizing pressure to be 80MPa and the homogenizing times to be 4 times to obtain collagen fiber solution;
(3) then adding the algae oil according to the oil-water volume ratio of 3:7, and mixing the algae oil with the collagen fiber solution to form an oil-water mixture;
(4) carrying out ultrasonic treatment on the oil-water mixture, wherein the working parameters of the ultrasonic cell disruption instrument are as follows: the power is 450W, the ultrasound is 3s, the gap is 3s, and the total time is 10min, so that the Pickering emulsion is obtained.
Example 2
The embodiment 2 of the invention discloses a preparation method of Pickering emulsion, which comprises the following steps:
(1) removing fat and impurity protein from cattle second-layer skin, washing the cattle second-layer skin with distilled water thoroughly to approach neutrality, cutting cattle hide into 5cm × 5cm pieces, and mixing the cattle hide with hydrochloric acid 1: 3(W/V) adding 0.5M hydrochloric acid, swelling at 4 deg.C for 24 hr, washing with hydrochloric acid, and carefully tearing collagen fibers from the swollen cowhide;
(2) dissolving collagen fibers in 0.1M acetic acid solution, preparing suspension with the concentration of 0.05 wt% respectively, adding the suspension into a high-pressure homogenizer, and setting the homogenizing pressure to be 80MPa and the homogenizing times to be 4 times to obtain collagen fiber solution;
(3) then adding the algae oil according to the oil-water volume ratio of 3:7, and mixing the algae oil with the collagen fiber solution to form an oil-water mixture;
(4) carrying out ultrasonic treatment on the oil-water mixture, wherein the working parameters of the ultrasonic cell disruption instrument are as follows: the power is 450W, the ultrasound is 3s, the gap is 3s, and the total time is 10min, so that the Pickering emulsion is obtained.
Example 3
The embodiment 3 of the invention discloses a preparation method of Pickering emulsion, which comprises the following steps:
(1) removing fat and impurity protein from cattle second-layer skin, washing the cattle second-layer skin with distilled water thoroughly to approach neutrality, cutting cattle hide into 5cm × 5cm pieces, and mixing the cattle hide with hydrochloric acid 1: 3(W/V) adding 0.5M hydrochloric acid, swelling at 4 deg.C for 24 hr, washing with hydrochloric acid, and carefully tearing collagen fibers from the swollen cowhide;
(2) dissolving collagen fibers in 0.1M acetic acid solution, preparing suspension with the concentration of 0.1 wt% respectively, adding the suspension into a high-pressure homogenizer, and setting the homogenizing pressure to be 100MPa and the homogenizing times to be 5 times to obtain collagen fiber solution;
(3) then adding the algae oil according to the oil-water volume ratio of 3:7, and mixing the algae oil with the collagen fiber solution to form an oil-water mixture;
(4) carrying out ultrasonic treatment on the oil-water mixture, wherein the working parameters of the ultrasonic cell disruption instrument are as follows: the power is 450W, the ultrasound is 3s, the gap is 3s, and the total time is 10min, so that the Pickering emulsion is obtained.
Example 4
The embodiment 4 of the invention discloses a preparation method of Pickering emulsion, which comprises the following steps:
(1) removing fat and impurity protein from cattle second-layer skin, washing the cattle second-layer skin with distilled water thoroughly to approach neutrality, cutting cattle hide into 5cm × 5cm pieces, and mixing the cattle hide with hydrochloric acid 1: 3(W/V) adding 0.5M hydrochloric acid, swelling at 4 deg.C for 24 hr, washing with hydrochloric acid, and carefully tearing collagen fibers from the swollen cowhide;
(2) dissolving collagen fibers in 0.2M acetic acid solution, preparing suspension with the concentration of 0.3 wt% respectively, adding the suspension into a high-pressure homogenizer, and setting the homogenizing pressure to be 100MPa and the homogenizing times to be 4 times to obtain collagen fiber solution;
(3) then adding the algae oil according to the oil-water volume ratio of 3:7, and mixing the algae oil with the collagen fiber solution to form an oil-water mixture;
(4) carrying out ultrasonic treatment on the oil-water mixture, wherein the working parameters of the ultrasonic cell disruption instrument are as follows: the power is 450W, the ultrasound is 3s, the gap is 3s, and the total time is 10min, so that the Pickering emulsion is obtained.
Example 5
The embodiment 5 of the invention discloses a preparation method of Pickering emulsion, which comprises the following steps:
(1) removing fat and impurity protein from cattle second-layer skin, washing the cattle second-layer skin with distilled water thoroughly to approach neutrality, cutting cattle hide into 5cm × 5cm pieces, and mixing the cattle hide with hydrochloric acid 1: 3(W/V) adding 0.5M hydrochloric acid, swelling at 4 deg.C for 24 hr, washing with hydrochloric acid, and carefully tearing collagen fibers from the swollen cowhide;
(2) dissolving collagen fibers in 0.5M acetic acid solution, preparing suspension with the concentration of 0.5 wt% respectively, adding the suspension into a high-pressure homogenizer, and setting the homogenization pressure to be 120MPa and the homogenization times to be 4 times to obtain collagen fiber solution;
(3) then adding the algae oil according to the oil-water volume ratio of 3:7, and mixing the algae oil with the collagen fiber solution to form an oil-water mixture;
(4) carrying out ultrasonic treatment on the oil-water mixture, wherein the working parameters of the ultrasonic cell disruption instrument are as follows: the power is 450W, the ultrasound is 3s, the gap is 3s, and the total time is 10min, so that the Pickering emulsion is obtained.
Example 6
The embodiment 6 of the invention discloses a preparation method of Pickering emulsion, which comprises the following steps:
(1) removing fat and impurity protein from cattle second-layer skin, washing the cattle second-layer skin with distilled water thoroughly to approach neutrality, cutting cattle hide into 5cm × 5cm pieces, and mixing the cattle hide with hydrochloric acid 1: 3(W/V) adding 0.5M hydrochloric acid, swelling at 4 deg.C for 24 hr, washing with hydrochloric acid, and carefully tearing collagen fibers from the swollen cowhide;
(2) dissolving collagen fibers in 0.1M acetic acid solution, preparing suspension with the concentration of 1 wt% respectively, adding the suspension into a high-pressure homogenizer, and setting the homogenizing pressure to be 100MPa and the homogenizing times to be 4 times to obtain collagen fiber solution;
(3) then adding the algae oil according to the oil-water volume ratio of 3:7, and mixing the algae oil with the collagen fiber solution to form an oil-water mixture;
(4) carrying out ultrasonic treatment on the oil-water mixture, wherein the working parameters of the ultrasonic cell disruption instrument are as follows: the power is 450W, the ultrasound is 3s, the gap is 3s, and the total time is 10min, so that the Pickering emulsion is obtained.
Example 7
The embodiment 7 of the invention discloses a preparation method of Pickering emulsion, which comprises the following steps:
(1) removing fat and impurity protein from cattle second-layer skin, washing the cattle second-layer skin with distilled water thoroughly to approach neutrality, cutting cattle hide into 5cm × 5cm pieces, and mixing the cattle hide with hydrochloric acid 1: 3(W/V) adding 0.5M hydrochloric acid, swelling at 4 deg.C for 24 hr, washing with hydrochloric acid, and carefully tearing collagen fibers from the swollen cowhide;
(2) dissolving collagen fibers in 0.1M acetic acid solution, preparing suspension with the concentration of 2 wt% respectively, adding the suspension into a high-pressure homogenizer, and setting the homogenizing pressure to be 80MPa and the homogenizing times to be 10 times to obtain collagen fiber solution;
(3) then adding the algae oil according to the oil-water volume ratio of 3:7, and mixing the algae oil with the collagen fiber solution to form an oil-water mixture;
(4) carrying out ultrasonic treatment on the oil-water mixture, wherein the working parameters of the ultrasonic cell disruption instrument are as follows: the power is 450W, the ultrasound is 3s, the gap is 3s, and the total time is 10min, so that the Pickering emulsion is obtained.
Example 8
The embodiment 8 of the invention discloses a preparation method of Pickering emulsion, which comprises the following steps:
(1) removing fat and impurity protein from cattle second-layer skin, washing the cattle second-layer skin with distilled water thoroughly to approach neutrality, cutting cattle hide into 5cm × 5cm pieces, and mixing the cattle hide with hydrochloric acid 1: 3(W/V) adding 0.5M hydrochloric acid, swelling at 4 deg.C for 24 hr, washing with hydrochloric acid, and carefully tearing collagen fibers from the swollen cowhide;
(2) dissolving collagen fibers in 0.1M acetic acid solution, preparing suspensions with the concentration of 5 wt% respectively, adding the suspensions into a high-pressure homogenizer, and setting the homogenization pressure to be 80MPa and the homogenization times to be 4 times to obtain collagen fiber solution;
(3) then adding the algae oil according to the oil-water volume ratio of 3:7, and mixing the algae oil with the collagen fiber solution to form an oil-water mixture;
(4) carrying out ultrasonic treatment on the oil-water mixture, wherein the working parameters of the ultrasonic cell disruption instrument are as follows: the power is 450W, the ultrasound is 3s, the gap is 3s, and the total time is 10min, so that the Pickering emulsion is obtained.
Effect verification
Characterization of collagen fibers
(1) Atomic force microscope
Preparing the collagen fibers prepared in the step (1) of example 1 into 0.65% suspension by using distilled water, and setting the homogenization pressure to be 80MPa by using a high-pressure homogenizer for 4 times to form a nano-sized collagen fiber dispersion liquid;
then observing the shape and size of the collagen fiber by an atomic force microscope, firstly diluting 2 mul of the prepared collagen fiber dispersion liquid by 10 times, then uniformly coating the diluted collagen fiber dispersion liquid on the surface of a mica sheet, standing the mica sheet at room temperature for one day for drying, and observing the obtained result under the atomic force microscope, wherein the obtained result is shown in figure 1.
The results in FIG. 1 show that the collagen fibers observed by AFM are thin, mainly between 600 and 800nm in length, about 20nm in diameter, and about 1.8nm in height, indicating that the particle size of the extracted collagen fibers has been successfully reduced to nanometer level after a series of treatments.
(2) Measurement of Zeta potential
The potential change of the collagen fibers under different pH (2-10) conditions is determined by a Zeta potential analyzer, and each sample is parallelly determined for three times, and the obtained result is shown in figure 2
Collagen is a polyampholyte like most other proteins, the Zeta potential of collagen fibers at 25 ℃ varies with pH as shown in FIG. 2, collagen fibers are positively charged at pH 2.0 (+24.52mV), collagen fibers are negatively charged at pH 10.0 (-4.16mV), the Zeta potential at pH 3.0 +18.37 mV. presents a zero charge point between pH 7-8, commonly referred to as the isoelectric point3 +and-COOH) to dominate the positive charge, while the same group (-NH) increases with pH2and-COO-) The deprotonation of (a) leads to a predominance of negative charges.
Characterization of the emulsion
(1) Confocal laser scanning microscope observation
The distribution, size and interfacial layer of oil droplets in the emulsion were evaluated by confocal microscopy. Pickering emulsion prepared in example was colored with mixed dyes (1mg/mL of Nile Red and Nile blue A dissolved in isopropanol). Dropping the dyed Pickering emulsion on a glass slide, covering the drop with a cover glass to ensure that the drop is uniform and has no bubbles, dyeing the algae oil and the collagen fiber in the emulsion into red and blue by Nile red and Nile blue A respectively, and then placing the emulsion under a confocal microscope for observation.
The microstructure (including the interface structure and the droplet flocculation state) affecting the formation and physical properties of the emulsion was evaluated by a laser confocal microscope, and as a result, as shown in fig. 3, the collagen fiber solution and the algal oil were mixed at a volume ratio of 7:3, and the pH of the emulsion system was 3.0. The seaweed oil is dyed by Nile red to be red fluorescence and distributed in the spherical liquid drops, the collagen fibers are dyed by Nile blue A to be blue fluorescence and distributed around the liquid drops to tightly wrap the red fluorescence, and the formed emulsion is further explained to be o/w emulsion, wherein the collagen fibers are uniformly dispersed on the surfaces of the oil drops to form compact interface layers, and meanwhile, adjacent liquid drops are stacked to form seepage network structures to prevent the liquid drops from coalescing, so that the emulsion is endowed with the characteristics of viscoelasticity solid-like and the stability of emulsification resistance and coalescence resistance.
(2) Macroscopic/microscopic morphological observation before and after emulsion centrifugation
The emulsion volume of pickering emulsions of different collagen fiber concentrations prepared in examples 1 to 8 was measured to evaluate the emulsion efficiency of collagen fibers. The emulsification efficiency is reflected through visual observation, and the volume of each layer of the emulsion in the centrifugal tube after 24 hours of storage is recorded; the emulsion was then centrifuged at 8000g for 5min and the emulsion layer volumes were again recorded to observe the centrifuge stability. Then, microscopic morphological changes of the emulsion before and after centrifugation were observed using an optical microscope. The macroscopic/microscopic morphology observation results of the obtained emulsion before and after centrifugation are shown in fig. 4.
The concentration of collagen fibrils has a significant effect on the stability of the emulsion and the droplet size. In FIG. 4a, the concentration of collagen fibers is between 0.01% and 1.5%, and the pH of the emulsion in the sample is 3.0. In all emulsions, the pH of the emulsion was 3.0. As can be seen from FIG. 4a, macroscopic phase separation occurred at a collagen fiber concentration of 0.01 to 0.05 wt%. After centrifugation, FIG. 4b, the emulsion volume was gradually increased until the concentration reached 1.0 wt.%. When the concentration reached 1.5 wt%, the total volume decreased slightly, indicating that the droplets had aggregated. The optical microscope images before and after centrifugation further demonstrate that the pickering emulsion is stable against coalescence within a concentration range of 0.1 to 1.0 wt%. Meanwhile, the droplet size gradually decreases with increasing concentration. Also, when the concentration reached 1.5 wt%, aggregation of the droplets occurred.
(3) Rheological observations
The rheological properties of the pickering emulsion were measured by a dynamic rheometer at 25 ℃. About 1ml of the emulsion prepared in the example was placed uniformly on a steel plate (diameter 35mm, gap 1mm) and then tested. All dynamic tests were performed in the linear viscoelastic region, including oscillation amplitude sweep (stress 0.1-100Pa, frequency 1Hz) and oscillation frequency sweep (stress 1-10Hz, stress 1 Pa). The elastic (G ') and viscous (G') moduli were recorded as a function of frequency and pressure. All measurements were performed in triplicate.
Rheology plays a crucial role in the analysis of physical properties of emulsions, such as appearance, stability and complex structure. In the experimental process, the emulsion is subjected to oscillation amplitude scanning and oscillation frequency scanning, and the relationship between the rheology and the microstructure of the emulsion is discussed.
The results of the oscillation amplitude scan of the emulsion are shown in fig. 5a, which shows that: at lower amplitudes, the elastic modulus (G ') is greater than the corresponding viscous modulus (G ') for different concentrations of collagen fibers, a crossing point occurs with increasing oscillation amplitude, and then the viscous modulus (G ") is greater than the elastic modulus (G '), which may be caused by the structural rearrangement of the emulsion under higher stress, and it can be observed that the crossing point (about 10Pa) occurs at lower amplitudes for emulsions with collagen fiber concentrations below 0.5 wt%, and approximately between 40 and 80Pa for concentrations between 0.5 and 1.5 wt%, indicating that the emulsion with properly increased collagen fiber concentrations is more stable.
The oscillation frequency scanning result of the emulsion is shown in fig. 5b, and G 'of the emulsion is higher than the corresponding G' in the whole measuring frequency range of 0.1-10Hz, which is a typical gel-like behavior. As the concentration of the collagen fibers is increased, the protective effect on the liquid drops formed by the adsorption of the collagen fibers on the surface of the oil drops is enhanced, so that the viscoelastic response is increased.
The comprehensive analysis of the results shows that the natural nano-collagen fiber prepared by high-pressure homogenization and the Pickering emulsion prepared by taking the natural nano-collagen fiber as the raw material are characterized, and an atomic force microscope shows that the length of the prepared collagen fiber is between 600 and 800nm, and the diameter is about 20 nm. The mixture (7:3, v/v) of the seaweed oil can form a stable oil-in-water emulsion after ultrasonic treatment, the concentration of collagen fibers has an important influence on the stability of the emulsion and the size of liquid drops, and the particle size of the liquid drops is gradually reduced along with the increase of the concentration. The collagen fiber with lower concentration (less than 0.1 wt%) can not completely wrap the oil drop to form obvious layering, the viscoelasticity is lower, the external force resistance is relatively lower (10 Pa), the oil drop can be completely wrapped in the collagen fiber after the concentration of the collagen fiber is increased to 0.1-1.5 wt%, and the external force resistance is increased (40-80 Pa). The emulsion prepared by using the collagen fiber with proper concentration as the emulsifier has good stabilizing effect, and can be used as a novel Pickering emulsifier to be applied to the fields of food and cosmetics.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A preparation method of collagen-based pickering emulsion is characterized by comprising the following steps:
(1) preparing collagen fibers into a suspension, and homogenizing to obtain a collagen fiber dispersion liquid;
(2) mixing the collagen fiber dispersion liquid and the dispersed phase according to a proportion to form an oil-water mixture;
(3) emulsifying the oil-water mixture to obtain the Pickering emulsion.
2. The method for preparing pickering emulsion according to claim 1, wherein the collagen fibers in step (1) are dissolved in acetic acid solution to form a suspension, the pH of the suspension is 1-5, and the mass concentration of the collagen fibers is 0.01-10%; the concentration of the acetic acid solution is 0.1-1 mol/L.
3. The method for preparing a collagen-based pickering emulsion according to claim 2, wherein said collagen fibers in step (1) are mechanically peeled from acid-swollen or non-acid-swollen cowhide; or the collagen fiber is collagen extracted by acid or enzyme, and the collagen is in a fibrous shape.
4. The method for preparing a collagen-based pickering emulsion according to claim 3, wherein the length of the collagen fiber in step (1) is 600 to 900nm, and the diameter is 20 to 100 nm.
5. The method of claim 1, wherein the homogenizing pressure in step (1) is 10-300 MPa for 1-20 times, and the collagen fiber dispersion has a nano size.
6. The method of claim 1, wherein the dispersed phase in step (2) is a functional fatty acid or a phytoactive lipid compound; the functional fatty acid comprises algae oil or fish oil; the plant active lipid compound comprises plant essential oil.
7. The method for preparing a collagen-based pickering emulsion according to claim 6, wherein the collagen fiber dispersion liquid and the dispersed phase in the step (2) are in a mass ratio of (10-99.9): (0.1-90) mixing.
8. The method of claim 1, wherein the emulsifying step (3) comprises homogenizing, ultrasonic or micro-jetting; the homogenizing pressure is 10-150MPa, and the times are 1-20.
9. Use of a collagen-based pickering emulsion prepared by the method of any one of claims 1 to 8 in food or cosmetics.
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