Molasses-edible oil oil-in-water Pickering emulsion as well as preparation method and application thereof

By mixing molasses and edible oil, a molasses-edible oil water-in-oil Pickering emulsion with high stability and low cost is prepared, which solves the high cost and safety problems of stabilizers in the existing technology and achieves high stability and antioxidant effect of the emulsion.

CN120585655APending Publication Date: 2025-09-05SHENZHEN UNIV
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Patent Information

Application Number
CN202510809604.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-17
Publication Date
2025-09-05

AI Technical Summary

Technical Problem

Existing Pickering emulsion stabilizers are expensive, have complex preparation processes, and are controversial in terms of safety in the food and medical fields. There is an urgent need for an emulsion stabilizer with low cost, high safety, and good stability.

Method used

Molasses and edible oil were mixed and treated by centrifugation, mechanical shearing and ultrasonic homogenization to prepare a molasses-edible oil-in-water Pickering emulsion with an average particle size of 10-100 μm. The stability was achieved by the irreversible adsorption of colloidal substances in molasses on the surface of oil droplets.

Benefits of technology

The prepared emulsion has good stability, no chemical additives, low cost, antioxidant activity, simple and reliable process, and is easy to scale up for production.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses molasses-edible oil oil-in-water Pickering emulsion as well as a preparation method and application thereof, and relates to the technical field of food processing. The preparation method comprises the following steps: S1, uniformly mixing raw molasses and water to prepare a dilute molasses solution with the brix of 30-65 degrees Bx; s2, carrying out centrifugal treatment on the dilute molasses solution; s3, mixing the diluted molasses solution subjected to centrifugal treatment with edible oil in a volume ratio of (8: 2)-(4: 6), and mechanically shearing to obtain molasses-edible oil mixed liquid; and S4, carrying out homogenization treatment on the molasses-edible oil mixed solution to obtain the molasses-edible oil oil-in-water Pickering emulsion. The preparation process is simple and reliable, and the prepared molasses-edible oil oil-in-water Pickering emulsion is small in particle size, high in stability and high in safety and has antioxidant activity.
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Description

Technical Field

[0001] The present invention relates to the technical field of food processing, in particular to a molasses-edible oil oil-in-water Pickering emulsion and a preparation method and application thereof. Background Art

[0002] Pickering emulsions are a type of emulsion stabilized by nano- / micron-sized solid particles. Pickering emulsions are known for their excellent stability, resistance to aggregation, flocculation, and Ostenberg ripening, resulting in a wide range of applications in the food, cosmetics, and pharmaceutical industries. Traditional emulsions are generally stabilized with small-molecule surfactants or amphiphilic biopolymers (proteins, polysaccharides, and their complexes), which effectively reduce the interfacial tension of the oil-water system. However, the stabilization mechanism of Pickering emulsions is through the irreversible adsorption of solid particles to the oil-water interface, forming a physical barrier to prevent the coalescence of oil droplets. Particles commonly used to stabilize Pickering emulsions include lipid particles, polysaccharide particles, protein particles, and inorganic particles. However, these particles are relatively expensive and complex to prepare, and the long-term safety of inorganic particles in food or medical applications is controversial.

[0003] Therefore, there is an urgent need for a food-grade, natural, safe and stable Pickering emulsion.

[0004] Molasses is a byproduct of the sugar extraction process from sugarcane and beets. It is a dark brown, viscous liquid containing carbohydrates, inorganic salts, and crude protein. It is rich in fermentable sugars such as fructose, glucose, raffinose, and sucrose, of which sucrose accounts for approximately 24% to 36% and other sugars account for approximately 12% to 24%. Molasses also contains approximately 15% to 20% water and 30% to 35% non-sugars (minerals, organic acids, vitamins, amines, etc.). Due to its low price and simple processing, molasses has great development value in industries such as chemicals, light food, medicine, and building materials. Currently, molasses is used to produce products such as pigments (melanoidins), lysine, extracellular polysaccharides, and citric acid. Based on this, how to use molasses to stabilize pickling emulsions is a current problem that needs to be solved. Summary of the Invention

[0005] In order to solve the problems existing in the above-mentioned prior art, the present invention aims to provide a molasses-edible oil oil-in-water Pickering emulsion and its preparation method and application. The molasses-edible oil oil-in-water Pickering emulsion has safe cost, simple preparation process and high stability.

[0006] The present invention provides the following technical solutions:

[0007] In a first aspect, the present invention provides a method for preparing a molasses-edible oil oil-in-water Pickering emulsion, comprising the following steps:

[0008] S1, raw molasses and water are mixed uniformly to prepare a thin molasses solution with a Brix of 30-65°Bx;

[0009] S2, centrifuging the dilute molasses solution;

[0010] S3, mixing the centrifuged dilute molasses solution with edible oil in a volume ratio of (8:2) to (4:6), and mechanically shearing to obtain a molasses-edible oil mixture;

[0011] S4. Homogenize the molasses-edible oil mixture to obtain a molasses-edible oil oil-in-water Pickering emulsion.

[0012] Preferably, the molasses is selected from one of sugarcane molasses and beet molasses.

[0013] Preferably, the solid content in the molasses is not less than 65%.

[0014] Preferably, the brix of the dilute molasses solution is 40-50° Bx.

[0015] Preferably, the water is selected from at least one of deionized water and pure water; preferably, the water is deionized water.

[0016] Furthermore, in step S1, the specific steps of uniformly mixing the raw molasses and water are: adding water to the concentrated molasses or adding the concentrated molasses to the water, and then stirring at room temperature, wherein the room temperature is 0-40°C.

[0017] Preferably, the room temperature is 10-35°C.

[0018] Preferably, the room temperature is 25-30°C.

[0019] Preferably, the specific step of uniformly mixing the raw molasses and water is: adding water to the concentrated molasses and stirring evenly at room temperature.

[0020] Furthermore, the stirring parameters are: time 0.5-6h, speed 200-800rpm.

[0021] Preferably, the stirring parameters are: time 1-3h, speed 200-500rpm.

[0022] Furthermore, the conditions of the centrifugal treatment are: rotation speed 5000-15000 rpm, and centrifugation time 10-120 min.

[0023] Preferably, the centrifugal treatment conditions are: rotation speed 8000-12000 rpm, and centrifugation time 20-30 min.

[0024] Furthermore, the edible oil is selected from at least one of medium-chain fatty acids, medium-chain triglycerides, fish oil, soybean oil, corn oil, peanut oil, rapeseed oil, sesame oil, sunflower oil, walnut oil, camellia oil, corn germ oil and olive oil.

[0025] Preferably, the edible oil is selected from one of medium chain triglycerides, corn oil and soybean oil.

[0026] Preferably, the medium chain triglyceride is food grade vitamin medium chain triglyceride with a purity of not less than 99%.

[0027] Furthermore, the mechanical shearing adopts a high-speed shearing method, and its parameters are: rotation speed 5000-22000 rpm, and shearing time 2-20 min.

[0028] Preferably, the parameters of the high-speed shearing method are: rotation speed 8000-15000 rpm, and shearing time 4-8 min.

[0029] Preferably, the parameters of the high-speed shearing method are: rotation speed 10000-12000 rpm, and shearing time 5-6 min.

[0030] Furthermore, the homogenization adopts a probe ultrasonic homogenization method, and its parameters are: power 100-600W, time 2-10min, and temperature 20-65°C.

[0031] Preferably, the parameters of the probe ultrasonic homogenization method are: power 200-400W, time 3-6 minutes, temperature 30-45°C.

[0032] In a second aspect, the present invention further provides a molasses-edible oil oil-in-water Pickering emulsion, which is prepared by the above-mentioned method for preparing the molasses-edible oil oil-in-water Pickering emulsion.

[0033] Furthermore, the average particle size of the molasses-edible oil oil-in-water Pickering emulsion is 10 to 100 μm.

[0034] Preferably, the average particle size of the molasses-edible oil oil-in-water Pickering emulsion is 15 to 80 μm.

[0035] In a third aspect, the present invention further provides an application of the molasses-edible oil oil-in-water Pickering emulsion in the fields of food, cosmetics or medicine.

[0036] The present invention has the following technical effects:

[0037] The present invention prepares an oil-in-water Pickering emulsion with an average particle size of 15 to 100 μm by mixing a molasses solution and edible oil in a fixed ratio. The emulsion has good stability, no chemical additives, low cost, and is environmentally friendly. In this oil-in-water Pickering emulsion system, molasses acts as an emulsion stabilizer, and the colloidal substances within it can be irreversibly adsorbed on the surface of the oil droplets, achieving an emulsification effect without the addition of any emulsifier. The molasses-edible oil oil-in-water Pickering emulsion prepared by the method of the present invention also contains polyphenols, which give it antioxidant activity.

[0038] The preparation process of the invention is simple and reliable, is convenient for scaled-up production, and has great application potential. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0040] Figure 1 This is the particle size distribution diagram of the molasses-edible oil oil-in-water Pickering emulsion in Example 1.

[0041] Figure 2 This is the particle size distribution diagram of the molasses-edible oil oil-in-water Pickering emulsion in Comparative Example 1. DETAILED DESCRIPTION

[0042] The following will clearly and completely describe the technical solutions of the present invention in conjunction with the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of them. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0043] It will be understood that when used in this specification and the appended claims, the terms “comprises” and “comprising” indicate the presence of described features, integers, steps, operations, elements and / or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components and / or groups thereof.

[0044] Specifically, in the specific implementation of the present invention, the information of each raw material is as follows:

[0045] Raw molasses is sugarcane molasses, and its Brix is ​​80° Bx.

[0046] Medium-chain fatty acids, food grade, were purchased from BritzNetworks Sdn. Bhd., Malaysia.

[0047] Soybean oil, food grade, was purchased from Wilmar International Holdings Co., Ltd.

[0048] Corn oil, food grade, was purchased from Wilmar International Holdings Co., Ltd.

[0049] Specifically, in a specific embodiment of the present invention, the brix is ​​detected by an Abbe refractometer (2WAJ, Shanghai Optical Instrument Factory No. 2).

[0050] In order to more fully understand the technical content of the present invention, the technical solution of the present invention is further introduced and illustrated in conjunction with specific embodiments below.

[0051] Example 1

[0052] S1, take raw molasses, add water to make a dilute molasses solution with a Brix of 50 ° Bx, and set aside;

[0053] S2, the dilute molasses solution was placed in a high-speed centrifuge and centrifuged at 8000 rpm for 15 min to obtain a clarified molasses solution;

[0054] S3, the molasses solution obtained in step S2 was mixed with the medium-chain triglyceride solution in a volume ratio of 6:4, and high-speed shearing was performed for 5 min at a shear rate of 10000 rpm to obtain a molasses-edible oil mixture.

[0055] S4. Insert the probe of the ultrasonic homogenizer into the molasses-edible oil mixture, set the ultrasonic power to 300 W, and homogenize for 7 minutes. During the homogenization process, use cold circulating water to control the temperature of the sample to ensure that the temperature is maintained at 45°C, thereby obtaining a molasses-edible oil-in-water Pickering emulsion.

[0056] Example 2

[0057] S1, take raw molasses, add water to make a dilute molasses solution with a Brix of 50 ° Bx, and set aside;

[0058] S2, the dilute molasses solution was placed in a high-speed centrifuge, and centrifuged at a centrifugal speed of 10000 rpm for 10 min to obtain a clarified molasses solution;

[0059] S3, the molasses solution obtained in step S2 is mixed with corn oil in a volume ratio of 5:5, and high-speed shearing is performed for 5 min at a shear rate of 10000 rpm to obtain a molasses-edible oil mixture.

[0060] S4. Insert the probe of the ultrasonic homogenizer into the molasses-edible oil mixture, set the ultrasonic power to 400 W, and homogenize for 4 minutes. During the homogenization process, use cold circulating water to control the temperature of the sample to ensure that the temperature is maintained at 55°C, thereby obtaining a molasses-edible oil-in-water Pickering emulsion.

[0061] Example 3

[0062] S1, take raw molasses, add water to make a dilute molasses solution with a Brix of 30 ° Bx, and set aside;

[0063] S2, the dilute molasses solution is placed in a high-speed centrifuge, and centrifuged at a centrifugal speed of 8000 rpm for 60 min to obtain a clarified molasses solution;

[0064] S3, the molasses solution obtained in step S2 is mixed with soybean oil in a volume ratio of 8:2, and high-speed shearing is carried out for 20 min at a shear rate of 5000 rpm to obtain a molasses-edible oil mixture.

[0065] S4. Insert the probe of the ultrasonic homogenizer into the molasses-edible oil mixture, set the ultrasonic power to 100 W, and homogenize for 10 minutes. During the homogenization process, use cold circulating water to control the temperature of the sample to ensure that the temperature is maintained at 20°C, thereby obtaining a molasses-edible oil-in-water Pickering emulsion.

[0066] Example 4

[0067] S1, take raw molasses, add water to make a dilute molasses solution with a Brix of 40 ° Bx, and set aside;

[0068] S2, the dilute molasses solution is placed in a high-speed centrifuge, and centrifuged at a centrifugal speed of 5000 rpm for 120 min to obtain a clarified molasses solution;

[0069] S3, the molasses solution obtained in step S2 is mixed with corn oil in a volume ratio of 4:6, and high-speed shearing is carried out for 10 min at a shear rate of 16000 rpm to obtain a molasses-edible oil mixture.

[0070] S4. Insert the probe of the ultrasonic homogenizer into the molasses-edible oil mixture, set the ultrasonic power to 400 W, and homogenize for 4 minutes. During the homogenization process, use cold circulating water to control the temperature of the sample to ensure that the temperature is maintained at 55°C, thereby obtaining a molasses-edible oil-in-water Pickering emulsion.

[0071] Example 5

[0072] S1, take raw molasses, add water to make a dilute molasses solution with a Brix of 65 ° Bx, and set aside;

[0073] S2, placing the dilute molasses solution in a high-speed centrifuge, and centrifuging at a centrifugal speed of 15000 rpm for 10 min to obtain a clarified molasses solution;

[0074] S3, the molasses solution obtained in step S2 is mixed with corn oil in a volume ratio of 5:5, and high-speed shearing is performed for 2 min at a shear rate of 220,000 rpm to obtain a molasses-edible oil mixture.

[0075] S4. Insert the probe of the ultrasonic homogenizer into the molasses-edible oil mixture, set the ultrasonic power to 600 W, and homogenize for 2 minutes. During the homogenization process, use cold circulating water to control the temperature of the sample to ensure that the temperature is maintained at 65°C, thereby obtaining a molasses-edible oil-in-water Pickering emulsion.

[0076] In order to illustrate the technical effect of the present invention, comparative examples 1-4 are set as follows based on Example 1 and Example 2:

[0077] Comparative Example 1

[0078] The only difference between this comparative example and Example 1 is that the volume ratio of the molasses solution to the corn oil in step S3 is 1:9.

[0079] Comparative Example 2

[0080] The only difference between this comparative example and Example 1 is that the volume ratio of the molasses solution to the corn oil in step S3 is 5:1.

[0081] Comparative Example 3

[0082] The only difference between this comparative example and Example 2 is that the Brix of the dilute molasses solution in this comparative example is 15° Bx.

[0083] Comparative Example 4

[0084] The only difference between this comparative example and Example 2 is that the Brix of the dilute molasses solution in this comparative example is 75° Bx.

[0085] In order to verify the technical effect of the present invention, the following tests were performed on the molasses-edible oil oil-in-water Pickering emulsions of Examples 1-5 and Comparative Examples 1-4:

[0086] (1) Average particle size detection and polyphenol content detection

[0087] The average particle size is one of the important parameters for measuring the stability of an emulsion. Therefore, in the present invention, the average particle size of the molasses-edible oil oil-in-water Pickering emulsion is detected by a static light scattering method.

[0088] The polyphenol content was determined as follows: 100 μL of sample was dissolved in 300 μL of anhydrous ethanol, followed by the addition of 0.1 mL of Folin's phenol reagent. The mixture was vortexed for 30 seconds and allowed to stand at room temperature for 15 minutes. Then, 200 μL of 10% sodium carbonate (Na2CO3) and 300 μL of deionized water were added, respectively. The resulting mixture was incubated in the dark for 90 minutes to form a blue reduced molybdate. After the reaction, the sample solution was centrifuged at 12,000 rpm for 15 minutes, and the absorbance of the supernatant was measured at 765 nm.

[0089] The test results are shown in Table 1 below:

[0090] Table 1 Average particle size and polyphenol content test results of Examples 1-5 and Comparative Examples 1-4

[0091] Average particle size (μm) Polyphenol content (mg / g) Example 1 45 0.14 Example 2 57 0.12 Example 3 28 0.21 Example 4 64 0.10 Example 5 54 0.13 Comparative Example 1 190 0.03 Comparative Example 2 75 0.06 Comparative Example 3 120 0.05 Comparative Example 4 118 0.23

[0092] As shown in Table 1, the molasses-edible oil oil-in-water Pickering emulsion prepared by the present invention has an average particle size of 10 to 100 μm and contains polyphenols, showing antioxidant activity. Modifying the process parameters of the present invention significantly increases the average particle size of the molasses-edible oil oil-in-water Pickering emulsion and significantly reduces the polyphenol content. This indicates that the preparation process of the present invention can maintain the polyphenol content while ensuring a small average particle size. The resulting molasses-edible oil oil-in-water Pickering emulsion has high stability and maintains its antioxidant activity.

[0093] (2) Particle size distribution test

[0094] Particle size distribution is another important indicator for measuring the stability of an emulsion. Therefore, the present invention uses a laser diffractometer (Mastersizer 3000, Malvern, UK) to test the particle size distribution of the molasses-edible oil-in-water Pickering emulsions of Example 1 and Comparative Example 3. The particle size distribution results of the molasses-edible oil-in-water Pickering emulsions of Example 1 and Comparative Example 1 are shown as follows: Figure 1 and Figure 2 As shown in the figure, it can be seen that the particle size distribution of Example 1 is more uniform, ranging from 22.6 to 198 μm and basically concentrated around 50 μm. In contrast, the particle size distribution of the molasses-edible oil oil-in-water Pickering emulsion in Comparative Example 1 is 16 to 400 μm, which is a larger span compared to the examples of the present invention and the particle size distribution is not highly uniform. Therefore, the preparation process of the present invention can produce a highly stable molasses-edible oil oil-in-water Pickering emulsion.

[0095] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any person skilled in the art can easily conceive of various equivalent modifications or substitutions within the technical scope disclosed in the present invention, and such modifications or substitutions are intended to be within the scope of protection of the present invention. Therefore, the scope of protection of the present invention shall be subject to the scope of protection of the claims.

Claims

1. A method for preparing a molasses-edible oil oil-in-water Pickering emulsion, characterized in that: The following steps are involved: S1. Mix raw molasses and water to prepare a dilute molasses solution with a Brix of 30 to 65°Bx; S2, centrifuging the dilute molasses solution; S3, mixing the centrifuged dilute molasses solution with edible oil in a volume ratio of (8:2) to (4:6), and mechanically shearing to obtain a molasses-edible oil mixture; S4. Homogenize the molasses-edible oil mixture to obtain a molasses-edible oil oil-in-water Pickering emulsion.

2. The method for preparing the molasses-edible oil oil-in-water Pickering emulsion according to claim 1, wherein The brix of the dilute molasses solution is 40-50°Bx.

3. The method for preparing the molasses-edible oil oil-in-water Pickering emulsion according to claim 1, wherein: The conditions of the centrifugal treatment are: rotation speed 5000-15000 rpm, and centrifugation time 10-120 min.

4. The method for preparing the molasses-edible oil oil-in-water Pickering emulsion according to claim 1, wherein: The edible oil is selected from at least one of medium-chain fatty acids, medium-chain triglycerides, fish oil, soybean oil, corn oil, peanut oil, rapeseed oil, sesame oil, sunflower oil, walnut oil, camellia oil, corn germ oil and olive oil.

5. The method for preparing the molasses-edible oil oil-in-water Pickering emulsion according to claim 1, wherein: The mechanical shearing adopts a high-speed shearing method, and its parameters are: shearing speed 5000-22000 rpm, and shearing time 2-20 minutes.

6. The method for preparing the molasses-edible oil oil-in-water Pickering emulsion according to claim 1, wherein: The homogenization treatment adopts a probe ultrasonic homogenization method, and its parameters are: power 100-600W, time 2-10min, and temperature 20-65°C.

7. A molasses-edible oil oil-in-water Pickering emulsion, characterized in that The emulsion is prepared by the method for preparing the molasses-edible oil-in-water Pickering emulsion according to any one of claims 1 to 6.

8. The molasses-edible oil oil-in-water Pickering emulsion according to claim 7, wherein The average particle size of the molasses-edible oil-in-water Pickering emulsion is 10-100 μm.

9. The method for preparing the molasses-edible oil oil-in-water Pickering emulsion according to claim 8, wherein: The average particle size of the molasses-edible oil-in-water Pickering emulsion is 15-80 μm.

10. Use of the molasses-edible oil oil-in-water Pickering emulsion according to any one of claims 7 to 9 in the fields of food, cosmetics or medicine.