A method for regulating the plasticity of olegels
By using the emulsion template method and controlling the water content in the oil-in-water emulsion, OSA starch and chitosan are used to form an oil gel with controllable plasticity, solving the problem of oil gel plasticity adjustment, meeting the requirements of baking and spreading, and adapting to industrial production.
Patent Information
- Application Number
- CN202410834714.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-06-26
- Publication Date
- 2025-10-31
- Estimated Expiration
- 2044-06-26
AI Technical Summary
Existing technologies make it difficult to achieve controllable adjustment of the plasticity of oleogels, and may affect the continuity and efficiency of industrial production.
Olegels were constructed using an emulsion template method. The plasticity of the olegels was controlled by adjusting the water content in the oil-in-water emulsion. OSA starch and chitosan were used as olegeling agents, and olegels with different plasticities were formed by combining drying and high-speed shearing.
It achieves controllable adjustment of oleogel plasticity to meet the needs of different food processing, such as the properties of baking shortening and spreadable butter, and adapts to the diversity and stability of industrial production.
Smart Images
Figure CN118633664B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of food processing and discloses a method for regulating the plasticity of oleogels. Background Technology
[0002] Oil gels are three-dimensional networks made of liquid oil and gelling agents, possessing a certain degree of plasticity and mechanical strength. In recent years, the application of oil gels in the food industry has gradually increased, including reducing / replacing trans and saturated fat intake and serving as delivery carriers for fat-soluble nutrients or drug components. In fact, these application properties are closely related to the plasticity of oil gels; for example, higher shear thixotropic properties and viscoelasticity make them candidates for replacing baking oils / animal fats; lower viscoelasticity and moderate thermal stability make them candidates for replacing cocoa butter; and higher stability and gel strength make them candidates for nutrient delivery carriers. However, current strategies for achieving controllable plasticity in oil gels still involve increasing or decreasing the concentration of the gelling agent or changing the type of gelling agent. This not only may contradict the construction principle of oil gels (high oil phase) but may also cause problems for industrial-scale production. Summary of the Invention
[0003] This invention addresses the shortcomings of existing technologies by providing a method for preparing oleogels with controllable plasticity. The invention employs an emulsion template method to construct oleogels. By fixing the mass of the oleogeling agent / oil and controlling the water content during emulsion template preparation, oleogels with different plasticity characteristics are obtained after drying.
[0004] This invention provides a method for controlling the plasticity of olegels, which is achieved by controlling the water content in the oil-in-water emulsion during the olegel preparation process.
[0005] Furthermore, when the water content in the oil-in-water emulsion varies between 40% and 70%, the initial viscosity and modulus of the resulting olegel exhibit linear variations between 27440.7 and 91423.6 Pa·s and 42907.7 and 133544 Pa, respectively.
[0006] Furthermore, when the water content is 35-40%, the initial viscosity and elastic modulus of the prepared oil gel meet the processing requirements of baking shortening.
[0007] Furthermore, when the water content is 40-50%, the initial viscosity and elastic modulus of the prepared oil gel meet the processing requirements of spreadable butter.
[0008] Furthermore, the oleogel preparation process includes:
[0009] Step 1: Dissolve OSA starch and chitosan in aqueous solution and aqueous acetic acid solution respectively to obtain OSA starch solution and chitosan solution, then mix and stir to obtain an aqueous solution containing oleogel agent;
[0010] Step 2: Mix the aqueous solution obtained in Step 1 with soybean oil, stir to obtain an oil-in-water emulsion, and dry until the water is removed to obtain solid lipids;
[0011] Step 3: The solid lipids obtained in Step 2 are subjected to high-speed shearing to form an oleogel.
[0012] Furthermore, in step 1, the concentration of acetic acid in the aqueous acetic acid solution is 0.5% to 2%.
[0013] Furthermore, the stirring temperature in step 1 is 30–50°C.
[0014] Furthermore, the stirring speed in step 1 is 500–700 r / min.
[0015] Furthermore, in step 1, the mixing volume ratio of OSA starch solution and chitosan solution is 1:0.8 to 1.
[0016] Furthermore, in step 1, the mass ratio of OSA starch to chitosan in the aqueous solution containing the oleogel is 1:0.05 to 0.07.
[0017] Specifically, optionally, in step 1, the mass ratio of OSA starch to chitosan in the aqueous solution containing the oleogel is 1:0.06.
[0018] Furthermore, the mass of the oleogel is equal to the mass of OSA starch and chitosan.
[0019] Furthermore, in step 2, the mass ratio of soybean oil to oleogel in the aqueous solution is 18:0.5 to 0.7.
[0020] Specifically, optionally, the mass ratio of soybean oil to oleogel in the aqueous solution in step 2 is 18:0.636.
[0021] Furthermore, in step 2, the mass ratio of the aqueous solution to soybean oil is 12–42:18.
[0022] Furthermore, the change in the mass ratio of aqueous solution to soybean oil in step 2 corresponds to the change in water content in the oil-in-water emulsion. Specifically, when the mass ratio of aqueous solution to soybean oil is 42:18, the initial viscosity and modulus of the resulting oil gel are 27440.7 Pa·s and 42907.7 Pa, respectively; when the mass ratio of aqueous solution to soybean oil is 12:18, the initial viscosity and modulus of the resulting oil gel are 91423.6 Pa·s and 133544 Pa, respectively.
[0023] Furthermore, the drying temperature in step 2 is 40–60°C.
[0024] Furthermore, the rotational speed during high-speed shearing in step 3 is 8000–12000 rpm.
[0025] Furthermore, the high-speed shearing time in step 3 is 0.8 to 1.2 minutes.
[0026] This invention provides a plastic controllable oleogel, the plasticity of which is controlled by adjusting the water content in an oil-in-water emulsion. After adjustment, the oil-in-water emulsion is dried and then sheared at high speed to obtain the oleogel.
[0027] Furthermore, the oil-in-water emulsion consists of oil, an oil gelling agent, and water.
[0028] Furthermore, the oleogel is composed of OSA starch and chitosan.
[0029] Furthermore, the mass ratio of OSA starch to chitosan is 1:0.05 to 0.07.
[0030] Specifically, the mass ratio of OSA starch to chitosan can be 1:0.06.
[0031] Furthermore, the mass ratio of oil to oil gelling agent is 18:0.5 to 0.7.
[0032] Specifically, the mass ratio of oil to oil gelling agent is 18:0.636.
[0033] Furthermore, the water content in the oil-in-water emulsion is 40–70% by mass.
[0034] Furthermore, the initial viscosity and elastic modulus of the obtained olegel were 27440.7–91423.6 Pa·s and 42907.7–133544 Pa, respectively.
[0035] Beneficial effects
[0036] This invention prepares an oleogrin agent by mixing OSA starch and chitosan. By controlling the proportion of this oleogrin agent, a plasticity-controllable oleogrin system can be obtained. The plasticity of the oleogrin can be adjusted by regulating the water content within this system, resulting in oleogrins with different plasticities to meet various processing purposes. For example, the initial viscosity of baking shortening is approximately 33127.3 Pa·s, and the initial elastic modulus is approximately 58160.9 Pa; the initial viscosity of spreadable butter is approximately 68430.8 Pa·s, and the initial elastic modulus is approximately 123544 Pa. All these properties can be achieved by oleogrins controlled using this method.
[0037] The plastic controllable oil gel of this invention has a wide adjustment range, which can be adjusted between 40% and 70% water content. The initial viscosity and modulus of the resulting oil gel are between 27440.7 and 91423.6 Pa·s and 42907.7 and 133544 Pa, respectively. The viscosity and modulus have a linear relationship with water content, which can be easily adjusted for different processing purposes. In addition, the viscosity of the plastic controllable oil gel decreases linearly with increasing shear rate, and the modulus increases slightly with increasing angular frequency. This is consistent with commercial baking shortening and butter, proving that the plastic controllable oil gel of this invention can meet various industrial needs. Attached Figure Description
[0038] Figure 1 Microstructure of oleogels in Comparative Examples 1-2 and Examples 1-5;
[0039] Figure 2 Apparent viscosity of oleogels in Comparative Examples 1-2 and Examples 1-5;
[0040] Figure 3 Thixotropic properties of oleogels in Comparative Examples 1-2 and Examples 1-5;
[0041] Figure 4 : Frequency scanning of oleogels in Comparative Examples 1-2 and Examples 1-5;
[0042] Figure 5 Temperature scans of oleogels in Comparative Examples 1-2 and Examples 1-4. Detailed Implementation
[0043] The present invention will now be described in detail with reference to the accompanying drawings and embodiments.
[0044] Source of raw materials
[0045] Octenyl succinic anhydride starch (OSA starch) was purchased from Hangzhou Prostar Starch Co., Ltd., and chitosan was purchased from Aladdin Reagent Co., Ltd.
[0046] Example 1
[0047] Step 1: Disperse 0.6g OSA starch and 0.036g chitosan in 21mL of aqueous solution and 21mL of 1% acetic acid solution, respectively. Stir at 40℃ for 12h until completely dissolved.
[0048] Step 2: Mix the solutions obtained in Step 1 in equal volumes and stir at a stirring speed of 600 r / min for 4 h to obtain an aqueous solution containing the oleogel.
[0049] Step 3: Mix the aqueous solution obtained in Step 2 with 18g of soybean oil, and stir at 12000rpm for 3min using a stator-rotor disperser to obtain an oil-in-water emulsion (containing 18g of oil, 0.636g of oil gelling agent and 42mL of water). Pour the emulsion into a petri dish and dry it in a 45℃ oven until the moisture is removed to obtain solid lipids.
[0050] Step 4: The solid lipids obtained in Step 3 are subjected to high-speed shearing at 10,000 rpm for 1 min at room temperature to form an oil gel. The solid content of the obtained oil gel is 3.41275%.
[0051] Example 2
[0052] Step 1: Disperse 0.6g OSA starch and 0.036g chitosan in 13.5mL of aqueous solution and 13.5mL of 1% acetic acid solution, respectively. Stir at 40℃ for 12 hours until completely dissolved.
[0053] Step 2: Mix the solutions obtained in Step 1 in equal volumes and stir at a stirring speed of 600 r / min for 4 h to obtain an aqueous solution containing the oleogel.
[0054] Step 3: Mix the aqueous solution obtained in Step 2 with 18g of soybean oil, and stir at 12000rpm for 3min using a stator-rotor disperser to obtain an oil-in-water emulsion (containing 18g of oil, 0.636g of oil gelling agent and 27mL of water). Pour the emulsion into a petri dish and dry it in a 45℃ oven until the moisture is removed to obtain solid lipids.
[0055] Step 4: The solid lipids obtained in Step 3 are subjected to high-speed shearing at 10,000 rpm for 1 min at room temperature to form an oil gel. The solid content of the obtained oil gel is 3.41275%.
[0056] Example 3
[0057] Step 1: Disperse 0.6g OSA starch and 0.036g chitosan in 9mL of aqueous solution and 9mL of 1% acetic acid solution, respectively. Stir at 40℃ for 12 hours until completely dissolved.
[0058] Step 2: Mix the solutions obtained in Step 1 in equal volumes and stir at a stirring speed of 600 r / min for 4 h to obtain an aqueous solution containing the oleogel.
[0059] Step 3: Mix the aqueous solution obtained in Step 2 with 18g of soybean oil, and stir at high speed of 12000rpm for 3min using a stator-rotor disperser to obtain an oil-in-water emulsion (containing 18g of oil, 0.636g of oil gelling agent and 18mL of water). Pour the emulsion into a petri dish and dry it in an oven at 45℃ until the moisture is removed to obtain solid lipids.
[0060] Step 4: The solid lipids obtained in Step 3 are subjected to high-speed shearing at 10,000 rpm for 1 min at room temperature to form an oil gel. The solid content of the obtained oil gel is 3.41275%.
[0061] Example 4
[0062] Step 1: Disperse 0.6g OSA starch and 0.036g chitosan in 6mL of aqueous solution and 6mL of 1% acetic acid solution, respectively. Stir at 40℃ for 12 hours until completely dissolved.
[0063] Step 2: Mix the solutions obtained in Step 1 in equal volumes and stir at a stirring speed of 600 r / min for 4 h to obtain an aqueous solution containing the oleogel.
[0064] Step 3: Mix the aqueous solution obtained in Step 2 with 18g of soybean oil, and stir at high speed of 12000rpm for 3min using a stator-rotor disperser to obtain an oil-in-water emulsion (containing 18g of oil, 0.636g of oil gelling agent and 12mL of water). Pour the emulsion into a petri dish and dry it in an oven at 45℃ until the moisture is removed to obtain solid lipids.
[0065] Step 4: The solid lipids obtained in Step 3 are subjected to high-speed shearing at 10,000 rpm for 1 min at room temperature to form an oil gel. The solid content of the obtained oil gel is 3.41275%.
[0066] Example 5
[0067] Step 1: Disperse 0.6g OSA starch and 0.036g chitosan in 3.86mL of aqueous solution and 3.86mL of 1% acetic acid solution, respectively. Stir at 40℃ for 12 hours until completely dissolved.
[0068] Step 2: Mix the solutions obtained in Step 1 in equal volumes and stir at a stirring speed of 600 r / min for 4 h to obtain an aqueous solution containing the oleogel.
[0069] Step 3: Mix the aqueous solution obtained in Step 2 with 18g of soybean oil, and stir at 12000rpm for 3min using a stator-rotor disperser to obtain an oil-in-water emulsion (containing 18g of oil, 0.636g of oil gelling agent and 7.72mL of water). Pour the emulsion into a petri dish and dry it in a 45℃ oven until the moisture is removed to obtain solid lipids.
[0070] Step 4: The solid lipids obtained in Step 3 are subjected to high-speed shearing at 10,000 rpm for 1 min at room temperature to form an oil gel. The solid content of the obtained oil gel is 3.41275%.
[0071] Comparative Example 1
[0072] Step 1: Disperse 0.8g OSA starch and 0.12g chitosan in 9mL of aqueous solution and 9mL of 1% acetic acid solution, respectively. Stir at 40℃ for 12h until completely dissolved.
[0073] Step 2: Mix the solutions obtained in Step 1 in equal volumes and stir at a stirring speed of 600 r / min for 4 h to obtain an aqueous solution containing the oleogel.
[0074] Step 3: Mix the aqueous solution obtained in Step 2 with 18g of soybean oil, and stir at 12000rpm for 3min using a stator-rotor disperser to obtain an oil-in-water emulsion (containing 18g of oil, 0.81g of oil gelling agent and 27mL of water). Pour the emulsion into a petri dish and dry it in a 45℃ oven until the moisture is removed to obtain solid lipids.
[0075] Step 4: The solid lipids obtained in Step 3 are subjected to high-speed shearing at 10,000 rpm for 1 min at room temperature to form an oil gel. The solid content of the obtained oil gel is 4.862579%.
[0076] Comparative Example 2
[0077] Step 1: Disperse 0.5g OSA starch and 0.03g chitosan in 4mL of aqueous solution and 4mL of 1% acetic acid solution, respectively. Stir at 40℃ for 12 hours until completely dissolved.
[0078] Step 2: Mix the solutions obtained in Step 1 in equal volumes and stir at a stirring speed of 600 r / min for 4 h to obtain an aqueous solution containing the oleogel.
[0079] Step 3: Mix the aqueous solution obtained in Step 2 with 18g of soybean oil, and stir at 12000rpm for 3min using a stator-rotor disperser to obtain an oil-in-water emulsion (containing 18g of oil, 0.59g of oil gelling agent and 8mL of water). Pour the emulsion into a petri dish and dry it in a 45℃ oven until the moisture is removed to obtain solid lipids.
[0080] Step 4: The solid lipids obtained in Step 3 are subjected to high-speed shearing at 10,000 rpm for 1 min at room temperature to form an oil gel. The solid content of the obtained oil gel is 2.860227%.
[0081] Performance testing
[0082] (1) Determination of microstructure:
[0083] Prior to microstructure testing, the oleogel was labeled with FITC (0.1%, excitation 561 nm), and images of the sample were recorded using a digital camera attached to a laser confocal microscope.
[0084] The microstructures of the oleogels in Examples 1-5 and Comparative Examples 1-2, as captured by laser confocal microscopy, are as follows: Figure 1 As shown in Examples 1-5, under fixed oleogel and oil phase mass conditions, the network structure of the oleogel is closely related to the amount of water added during the preparation of the emulsion template. Specifically, the lower the water content, the denser and more uniform the network structure. In Comparative Example 1, with a medium water content, increasing the oleogel concentration (relative to the oil phase) yields a dense network structure. In Comparative Example 2, with a low water content, decreasing the oleogel concentration (relative to the oil phase) yields a uniform and dense structure.
[0085] (2) Rheological measurements:
[0086] The rheological properties of the oleogel were analyzed using a TA-type rotary rheometer. A 40mm diameter aluminum plate was selected as the clamp, with a 1mm test gap. The oleogel sample was uniformly coated between the upper and lower clamps of the rheometer, and excess sample was removed along the clamp edges. The apparent viscosity was determined under static shear rates of 0.1–100 s⁻¹. Thixotropy was measured using time-scan tests at 300-s intervals, with alternating shear rates of 0.1 s⁻¹ and 10 s⁻¹. The G' and G” values were determined by frequency scans (angular frequency = 0.1–100 rad / s, strain = 0.1%), strain scans (strain = 0.01–1%, frequency = 1 Hz), and temperature scans (25–80 °C, 1 Hz).
[0087] Table 1
[0088]
[0089] Table 1, Figure 2 , Figure 3 ,and Figure 4 The apparent viscosity, thixotropic properties, and frequency sweep results of the oleogels in Examples 1-5 and Comparative Examples 1-2 are shown respectively. It can be seen that, under fixed oleogel agent and oil phase mass conditions, when preparing the emulsion template, the water content is in the range of 40-60%. The lower the water content, the higher the apparent viscosity, elastic modulus, and viscous modulus of the oleogel. However, when the added water content is as low as 30% of the total emulsion mass, the smaller oil droplets are difficult to bind to the network structure, resulting in collapse and a sharp decrease in the apparent viscosity, elastic modulus, and viscous modulus of the oleogel. The structural recovery rate of the oleogel also exhibits the same phenomenon.
[0090] Furthermore, when the concentration of the oleogel agent was increased (Comparative Example 1), a dense structure was found to be formed at a water content of 50%. Once the concentration of the oleogel agent was further increased, a more sufficient polymer network was obtained, resulting in an excessively large oleogel modulus that could not meet the requirements for plasticity control.
[0091] When the concentration of the oleogel was reduced (Comparative Example 2), it was found that the pores were too large at a water content of 33%. When the water content was increased, the oleogel obtained exhibited significant oil leakage because there was not enough polymer network to bind the oil droplets, which could not meet the needs of food processing.
[0092] Table 1 summarizes the viscosity and elastic modulus values of the oleogels in Examples 1-5 and Comparative Examples 1-2 under different shear conditions. It can be seen that, under the same shear conditions, the viscosity and elastic modulus values of the oleogels are affected by the amount of water added during emulsion preparation. This result further indicates that the plasticity of the oleogels can be controlled by changing the amount of water added during emulsion template preparation. Temperature scanning results of the oleogels show that the decrease in elastic modulus varies among all samples as the temperature increases from 25°C to 80°C, indicating that the thermal stability of the oleogels is also closely related to the amount of water added during emulsion template preparation.
[0093] The embodiments provided above are not intended to limit the scope of the invention, nor are the described steps intended to limit the order of execution. Any obvious modifications made to the invention by those skilled in the art based on existing common knowledge also fall within the scope of protection defined by the claims.
Claims
1. A method for controlling the plasticity of olegels, characterized in that, The method is achieved by controlling the water content in the oil-in-water emulsion during the preparation of the oleogel; when the water content in the oil-in-water emulsion varies between 40% and 70%, the initial viscosity and modulus of the obtained oleogel change linearly between 27440.7~91423.6 Pa·s and 42907.7~133544 Pa, respectively. The oleogel preparation process includes: Step 1: Dissolve octenyl succinic anhydride starch and chitosan in aqueous solution and aqueous acetic acid solution respectively to obtain octenyl succinic anhydride starch solution and chitosan solution, then mix and stir to obtain an aqueous solution containing oleogel agent; Step 2: Mix the aqueous solution obtained in Step 1 with soybean oil, stir to obtain an oil-in-water emulsion, and dry until the water is removed to obtain solid lipids; the mass ratio of soybean oil to oil gelling agent in the aqueous solution is 18: 0.5~0.7; the mass of the oil gelling agent is the mass of octenyl succinic anhydride starch and chitosan. Step 3: The solid lipids obtained in Step 2 are subjected to high-speed shearing to form an oleogel.
2. The method according to claim 1, characterized in that, In step 1, the concentration of acetic acid in the acetic acid aqueous solution is 0.5~2%; the stirring temperature in step 1 is 30~50℃; and the stirring speed in step 1 is 500~700 r / min.
3. The method according to claim 1, characterized in that, In step 1, the mixing volume ratio of octenyl succinic anhydride starch solution and chitosan solution is 1:0.8~1.
4. The method according to claim 1, characterized in that, In step 1, the mass ratio of octenyl succinic anhydride starch to chitosan in the aqueous solution containing the oleogel is 1:0.05~0.
07.
5. The method according to claim 1, characterized in that, In step 3, the rotation speed during high-speed shearing is 8000~12000 rpm; the time during high-speed shearing is 0.8~1.2 min.
6. The method according to claim 1, characterized in that, When the water content is 35-40%, the initial viscosity and elastic modulus of the prepared oil gel meet the processing requirements of shortening for baking.
7. The method according to claim 1, characterized in that, When the water content is 40-50%, the initial viscosity and elastic modulus of the prepared oil gel meet the processing requirements of spreadable butter.