Patent Application
20250017230
This patent application claims the benefit and priority of Chinese Patent Application No. 202310851598.4, entitled “OIL-IN-WATER EMULSION GEL AND PREPARATION METHOD AND USE THEREOF, AND FAT SUBSTITUTE”, filed with the China National Intellectual Property Administration on Jul. 11, 2023, the disclosure of which is incorporated by reference herein in its entirety as part of the present application.
The present disclosure relates to the technical field of food processing, and in particular to an oil-in-water (O/W) emulsion gel and a preparation method and use thereof, and a fat substitute.
Traditional solid fats contain more saturated fatty acids, which cause adverse effects on human health. Fat substitutes, such as plant-based fat substitutes obtained from liquid vegetable oils structured with polysaccharide macromolecules, have drawn widespread attention due to desirable fat-like processing properties, sensory properties, and green and health advantages.
3D printing, also known as additive manufacturing, specifically produces products with target models through layer-by-layer deposition. Food 3D printing is a process of manufacturing food using 3D printing. This process shows the advantages of personalized control of nutrition, accurate control of complex structures, digital production, optimization of the food supply chain, and reduction of food waste. In particular, food 3D printing has achieved unprecedented development due to convenient customization and ultra-high degree of freedom.
However, emulsion gels currently used for preparing the fat substitute based on 3D printing have low stability and poor performance in printing high-accuracy models.
The present disclosure is intended to provide an oil-in-water (O/W) emulsion gel and a preparation method and use thereof, and a fat substitute. In the present disclosure, the O/W emulsion gel has a desirable stability and can be used to prepare a fat substitute. The O/W emulsion gel is particularly suitable for preparing the fat substitute through 3D printing with a high printing accuracy.
To achieve the above object, the present disclosure provides the following technical solutions.
The present disclosure provides an oil-in-water (O/W) emulsion gel, including starch nanoparticles with a content of 8 g/L to 40 g/L, curdlan with a content of 10 g/L to 30 g/L, an oil with a volume fraction of 10% to 30%, and water.
In some embodiments, the starch nanoparticles each have a particle size of 100 nm to 500 nm.
In some embodiments, the curdlan includes at least one selected from the group consisting of carrageenan, xanthan gum, and gellan gum.
In some embodiments, the oil includes at least one selected from the group consisting of soybean oil, corn oil, peanut oil, sesame oil, wheat germ oil, and fish oil.
The present disclosure further provides a method for preparing the O/W emulsion gel described in above technical solutions, including the following steps:
In some embodiments, the first homogenization and the second homogenization are each independently conducted at a rotation speed of 12,000 rpm to 16,000 rpm for 2 minutes to 5 minutes.
In some embodiments, the gelation is conducted at a temperature of 70° C. to 80° C. for 50 minutes to 70 minutes.
The present disclosure further provides use of the O/W emulsion gel described in above technical solutions or the O/W emulsion gel prepared by the method described in above technical solutions in preparation of a fat substitute.
In some embodiments, the preparation of the fat substitute includes performing 3D printing using the O/W emulsion gel.
The present disclosure further provides a fat substitute, which is prepared from the O/W emulsion gel or the O/W emulsion gel prepared by the method described in above technical solutions through 3D printing.
The present disclosure provides an O/W emulsion gel, including: starch nanoparticles with a content of 8 g/L to 40 g/L, curdlan with a content of 10 g/L to 30 g/L, an oil with a volume fraction of 10% to 30%, and water. The starch nanoparticles serve as a stabilizer for the emulsion gel, and are combined with the curdlan to prepare the O/W emulsion gel with better stability. The O/W emulsion gel could be used to prepare a fat substitute, especially the fat substitute prepared by 3D printing with various complex models. The 3D printing shows a high printing accuracy to achieve a desirable fat-simulating effect.
The present disclosure further provides a method for preparing the O/W emulsion gel, including the following steps:
In the present disclosure, the starch nanoparticles and the oil are used as raw materials, and the nanoscale starch dispersion and the O/W emulsion (i.e., a Pickering emulsion stabilized by the starch nanoparticles) are obtained by first and second homogenization, respectively; the O/W emulsion is subjected to gelation under an action of the curdlan to obtain the O/W emulsion gel, thereby achieving structuring of the oil. The O/W emulsion gel prepared by the method has desirable rheological properties and emulsion stability, and could be used to prepare a fat substitute with a controllable structure. The O/W emulsion gel is particularly suitable for preparing the fat substitute through 3D printing, with high printing accuracy and high printing intensity, thereby showing an excellent application potential. In addition, the method according to the present disclosure has a simple and efficient process, does not involve harmful reagents and chemical components, and is environmentally friendly. The method achieves a more stable structured oil system under a lower oil phase proportion, and could realize all or part of the replacement of traditional solid fats, thereby expanding a practical application scope of low-fat healthy fat substitutes in the food field.
The present disclosure provides an O/W emulsion gel, including:
In the present disclosure, the emulsion gel has excellent stability through a Pickering mechanism. The Pickering mechanism refers to the construction mechanism of a new green emulsion that uses solid particles instead of small-molecule surfactants to establish packaging on the droplet surface. Specifically, the starch nanoparticles serve as a stabilizer for the emulsion gel, and are combined with the curdlan to prepare the O/W emulsion gel with a better stability. The O/W emulsion gel could be used to prepare a fat substitute, especially the fat substitute prepared by 3D printing with various complex models. The 3D printing shows a high printing accuracy and a high printing intensity to achieve a desirable simulated effect of fats. The O/W emulsion gel of the present disclosure will be described in detail below.
In the present disclosure, unless otherwise specified, the raw materials used are all commercially-available commodities well known to those skilled in the art or prepared by methods well known to those skilled in the art.
In the present disclosure, the O/W emulsion gel includes the starch nanoparticles as one of raw materials for preparation. Based on the raw materials, the starch nanoparticles have a content of 8 g/L to 40 g/L, preferably 15 g/L to 35 g/L, and more preferably 25 g/L to 32 g/L. In some embodiments, the starch nanoparticles each have a particle size of 100 nm to 500 nm. In the present disclosure, the starch nanoparticles serve as a stabilizer for the emulsion gel, and are combined with the curdlan to prepare the O/W emulsion gel with improved stability. In some embodiments, the starch nanoparticles are prepared by a nanoprecipitation method, specifically including the following steps:
In some embodiments of the present disclosure, a natural starch is mixed with a NaOH solution, and a resulting mixture is subjected to third homogenization to obtain a natural starch paste. In some embodiments, the natural starch includes at least one of corn starch, tapioca starch, and rice starch, and preferably is the corn starch, the tapioca starch, or the rice starch. In some embodiments, the NaOH solution has a concentration of 0.01 g/mL to 0.05 g/mL, and preferably 0.01 g/mL to 0.03 g/mL. In some embodiments, a ratio of the natural starch to the NaOH solution is in a range of (2-10) g: 100 mL, and preferably (4-5) g: 100 mL. In some embodiments, the third homogenization is conducted at a rotation speed of 1,500 rpm to 3,000 rpm, and preferably 2,500 rpm to 3,000 rpm. In some embodiments, the third homogenization is conducted for 1 minute to 3 minutes, and preferably 2 minutes to 3 minutes.
In some embodiments of the present disclosure, after obtaining the natural starch paste, the natural starch paste is added dropwise into ethanol, and a resulting mixture is subjected to fourth homogenization and precipitation in ethanol, to obtain a mixture after precipitation. In some embodiments, the ethanol is anhydrous ethanol. In some embodiments, a volume ratio of the natural starch paste to the ethanol is in a range of 1:1, 1:2 or 1:3, and preferably 1:1 or 1:2. In some embodiments, the natural starch paste is added dropwise to the ethanol. In some embodiments, the fourth homogenization is conducted at a rotation speed of 3,000 rpm to 15,000 rpm, and preferably 10,000 rpm to 15,000 rpm. In some embodiments, the fourth homogenization is conducted for 2 minutes to 5 minutes, and preferably 4 minutes to 5 minutes, and the time accounts after the dropwise addition of the natural starch paste is completed. In some embodiments, the natural starch paste is added dropwise to the ethanol at a rotational speed the same as the fourth homogenization, and after the dropwise addition is completed, the fourth homogenization is conducted at the rotational speed. The fourth homogenization is performed under the above conditions to promote the formation of the starch nanoparticles.
In some embodiments of the present disclosure, after obtaining the mixture after precipitation, the mixture after precipitation is centrifuged, and a resulting precipitate is collected, and subjected to washing, drying, grinding, and sieving sequentially to obtain the starch nanoparticles. In some embodiments of the present disclosure, the centrifugation is conducted at a rotation of 1,000 rpm to 2,000 rpm, and preferably 1,500 rpm to 2,000 rpm. In some embodiments, the centrifugation is conducted for 5 minutes to 10 minutes, and preferably 8 minutes to 10 minutes. In some embodiments, a reagent for the washing is ethanol, and preferably absolute ethanol. In some embodiments, the drying is conducted at a temperature of 35° C. to 75° C., and preferably 40° C. to 50° C. There is no special limitation to a drying time, as long as sufficient drying is ensured. There are no special restrictions on the grinding and the sieving, as long as the starch nanoparticles that meet particle size requirements could be obtained. In examples of the present disclosure, a 200-mesh sieve is used for sieving.
In the present disclosure, the O/W emulsion gel includes the curdlan as one of raw materials for preparation. Based on the raw materials, the curdlan has a content of 10 g/L to 30 g/L, preferably 15 g/L to 25 g/L, and more preferably 20 g/L. In some embodiments, the curdlan includes at least one of carrageenan, xanthan gum, and gellan gum, and preferably is the carrageenan, the xanthan gum, or the gellan gum. In some embodiments, the curdlan shows a high gelation speed and a desirable gelation effect.
In the present disclosure, the O/W emulsion gel includes the oil as one of raw materials for preparation. Based on the raw materials, the oil has a volume fraction of 10% to 30%, preferably 15% to 25%, and more preferably 20%. In some embodiments, the oil includes at least one of soybean oil, corn oil, peanut oil, sesame oil, wheat germ oil, and fish oil, and preferably is the soybean oil, the corn oil, the peanut oil, the sesame oil, the wheat germ oil, or the fish oil.
In the present disclosure, the O/W emulsion gel includes water as one of raw materials for preparation, and the water is used in an amount sufficient to ensure that the contents of the starch nanoparticles and the curdlan and the volume fraction of the oil meet the above requirements.
In the present disclosure, the O/W emulsion gel includes oil droplets formed from the oil. In some embodiments, the oil droplets each have a size of 5 μm to 60 μm.
The present disclosure further provides a method for preparing the O/W emulsion gel, including the following steps:
In the present disclosure, the starch nanoparticles are mixed with the water, and a resulting mixture is subjected to first homogenization to obtain a nanoscale starch dispersion. In some embodiments, the first homogenization is conducted at a rotation speed of 12,000 rpm to 16,000 rpm, and preferably 15,000 rpm. In some embodiments, the first homogenization is conducted for 2 minutes to 5 minutes, and preferably 3 minutes.
In the present disclosure, after obtaining the nanoscale starch dispersion, the nanoscale starch dispersion is mixed with the oil, and a resulting mixture is subjected to second homogenization to obtain an O/W emulsion. In some embodiments, the second homogenization is conducted at a rotation speed of 12,000 rpm to 16,000 rpm, and preferably 15,000 rpm. In some embodiments, the second homogenization is conducted for 2 minutes to 5 minutes, and preferably 3 minutes. In the O/W emulsion, the oil is a dispersed phase, and the nanoscale starch dispersion is a continuous phase.
In the present disclosure, the O/W emulsion is mixed with the curdlan, and a resulting mixture is subjected to gelation to obtain the O/W emulsion gel. In some embodiments, the O/W emulsion and the curdlan are mixed under stirring. In some embodiments, the stirring is conducted at a rotation speed of 100 rpm to 120 rpm, and preferably 110 rpm. In some embodiments, the stirring is conducted for 1 minute to 2 minutes. In some embodiments, the gelation is conducted at a temperature of 70° C. to 80° C., and preferably 70° C. to 75° C. In some embodiments, the gelation is conducted for 50 minutes to 70 minutes, and preferably 55 minutes to 60 minutes. During the gelation, the curdlan is gradually dissolved in the O/W emulsion and adheres to each other to form a gel grid. In some embodiments, the method further includes, after the gelation is completed, cooling a material obtained from the gelation to room temperature. There is no special limitation on a cooling means, and water bath cooling or natural cooling at room temperature may be adopted. In some embodiments, the O/W emulsion and the curdlan are mixed, heated in a water bath, and subjected to gelation, and a resulting product is then naturally cooled to room temperature to obtain the O/W emulsion gel.
The present disclosure further provides use of the O/W emulsion gel described in above technical solutions or the O/W emulsion gel prepared by the method described in above technical solutions in preparation of a fat substitute. In some embodiments, the preparation of the fat substitute includes performing 3D printing. A customized fat substitute product with certain self-supporting properties could be obtained through 3D printing. In some embodiments, a process for preparing the fat substitute using the O/W emulsion gel through 3D printing includes the following steps:
In the present disclosure, the O/W emulsion gel is preheated to a fluid state and then fed into a 3D printing needle tube. There is no particular limitation to a preheating temperature, as long as the O/W emulsion gel is heated to a flowing state. In some embodiments, the O/W emulsion gel in a flowing state is fed into the 3D printing needle tube without introducing air bubbles, while ensuring that the O/W emulsion gel in the 3D printing needle tube is uniform and in non-stratified state. In some embodiments, the 3D printing needle tube has a capacity of 10 mL. In some embodiments, a needle of the 3D printing needle tube is a tapered needle. In some embodiments, the needle has a diameter of 0.26 mm to 0.6 mm.
In the present disclosure, a printing nozzle is adjusted to a predetermined temperature and loaded with a 3D printing needle, and an X-axis, a Y-axis, and a Z-axis of a 3D printer are adjusted to zero through program settings. In some embodiments, the printing nozzle is at a temperature of 4° C. to 35° C., and preferably 10° C. to 25° C.
In the present disclosure, a 3D model is designed with data modeling software, and corresponding layers of three-dimensional slices are generated with slicing software to obtain a slice model; a path of each layer of the three-dimensional slices is calculated using a programming G code and the path is imported into the 3D printer. In some embodiments, the data modeling software is CAD 2007 version, and the 3D model exported is in STL (“.stl”) format. In some embodiments, the slicing software is slic3r version 1.3.1, and a file after slicing is in GCODE (“.gcode”) format.
In the present disclosure, 3D printing is performed by air pump extrusion or mechanical extrusion using the 3D printer according to preset 3D printing parameters, obtaining a fat substitute. In some embodiments, the 3D printing is conducted by the air pump extrusion. In some embodiments, the 3D printing parameters includes: a printing layer height of 0.2 mm to 0.4 mm, preferably 0.2 mm to 0.3 mm; a filling density of 80% to 100%, preferably 90% to 100%; an air pump extrusion pressure of 10 kPa to 25 kPa, preferably 10 kPa to 20 kPa; and a printing speed of 8 mm/s to 15 mm/s, preferably 9 mm/s to 11 mm/s.
The present disclosure further provides a fat substitute, wherein the fat substitute is prepared from the O/W emulsion gel as described in above technical solutions or the O/W emulsion gel prepared by the method as described in above technical solutions through 3D printing. In some embodiments of the present disclosure, a process and operating conditions for preparing the fat substitute using the O/W emulsion gel through the 3D printing are consistent with the above technical solutions, and will not be repeated here.
The technical solutions of the present disclosure will be clearly and completely described below with reference to the examples of the present disclosure. Apparently, the described examples are merely a part rather than all of the examples of the present disclosure. All other examples obtained by those skilled in the art based on the examples of the present disclosure without creative efforts shall fall within the scope of the present disclosure.
The characterization and performance testing methods involved in the following examples and comparative examples are as follows:
5 g of a natural corn starch was mixed with 100 mL of a NaOH solution with a concentration of 0.01 g/mL, and a resulting mixture was sheared and homogenized at 3,000 rpm for 3 min, such that the natural corn starch was dissolved in the NaOH solution and completely gelatinized, obtaining a natural starch paste. 100 mL of the natural starch paste was added dropwise into 100 mL of absolute ethanol at 15,000 rpm, and after the adding dropwise was completed, a resulting mixture was homogenized at 15,000 rpm for 5 min. A resulting liquid was centrifuged at 2,000 rpm for 10 min. A resulting precipitate was washed with absolute ethanol, dried at 50° C., then ground and sieved to pass through a 200-mesh sieve, obtaining starch nanoparticles with a particle size of 100 nm to 500 nm.
The starch nanoparticles was mixed with water and a resulting mixture was homogenized at 15,000 rpm for 3 min, obtaining a nanoscale starch dispersion with a concentration of 4 wt. %.
20 mL of soybean oil was added to 80 mL of the nanoscale starch dispersion, and a resulting mixture was homogenized at 15,000 rpm for 3 min, obtaining an O/W emulsion, wherein in the O/W emulsion the soybean oil acted as a dispersed phase and the nanoscale starch dispersion acted as a continuous phase.
2 g of carrageenan was added to 100 mL of the O/W emulsion. A resulting mixture was stirred at 110 rpm for 2 min, heated in a 70° C. water bath for 1 h, and cooled to room temperature, obtaining an O/W emulsion gel.
3D printing was performed on the O/W emulsion gel prepared in Example 1, which was performed according to the following procedures:
An O/W emulsion gel was prepared according to the method as described in Example 1, except that the soybean oil was replaced with fish oil.
3D printing was performed using the O/W emulsion gel prepared in this example according to the procedures as described in Example 1, except that the air pump extrusion pressure was 10 kPa.
An O/W emulsion gel was prepared according to the method as described in Example 1, except that the nanoscale starch dispersion was replaced with water.
3D printing was performed using the O/W emulsion gel prepared in this comparative example according to the procedures as described in Example 1, except that the air pump extrusion pressure was 15 kPa.
An O/W emulsion gel was prepared according to the method as described in Example 1, except that the starch nanoparticles were replaced with natural corn starch.
3D printing was performed using the O/W emulsion gel prepared in this comparative example according to the procedures as described in Example 1.
The emulsion gels prepared in Example 1, Example 2, Comparative Example 1, and Comparative Example 2 were subjected to a rheological property test. The results are shown in
The emulsion gels prepared in Example 1, Example 2, Comparative Example 1, and Comparative Example 2 were subjected to an emulsion stability test. The results are shown in
The above descriptions are merely preferred embodiments of the present disclosure. It should be noted that a person of ordinary skill in the art may further make several improvements and modifications without departing from the principle of the present disclosure, but such improvements and modifications should be deemed as falling within the scope of the present disclosure.
| Number | Date | Country | Kind |
|---|---|---|---|
| 202310851598.4 | Jul 2023 | CN | national |
