Double gel with O1 / W / O2 microstructure as well as preparation method and application of double gel

Abstract

The invention discloses double gel with an O1 / W / O2 microstructure as well as a preparation method and application of the double gel. The preparation method comprises the following steps: preparing a whey protein aggregate from whey protein isolate, mixing the whey protein aggregate with oil and a hydrophobic active substance, and homogenizing to prepare oleogel loaded with the hydrophobic active substance; guar gum, water and the hydrophilic active substance are mixed and fully hydrated, and hydrogel loaded with the hydrophilic active substance is prepared; and mixing the oleogel loaded with the hydrophobic active substance and the hydrogel loaded with the hydrophilic active substance, carrying out homogenization treatment, and carrying out in-situ self-assembly to form the double gel with the O1 / W / O2 microstructure. The invention constructs a double-gel with an O1 / W / O2 microstructure, and the double-gel can give consideration to cheese texture simulation and hydrophilic / hydrophobic active substance co-delivery functions.

Description

Technical Field

[0001] This invention belongs to the field of food processing technology, specifically relating to a dual gel with an O1 / W / O2 microstructure, its preparation method, and its application. Background Technology

[0002] Traditional cheeses pose health risks due to their high fat content (≥30%), but directly reducing fat leads to a loss of the product's smooth texture and characteristics. Maintaining the unique texture of cheese while reducing fat content is a significant challenge in developing low-fat cheese alternatives. Furthermore, with the increasing demand for natural functional foods, designing multi-component synergistic systems that incorporate both hydrophobic and hydrophilic natural bioactive ingredients better meets the diverse nutritional needs of modern consumers.

[0003] Pterostilbene (PTS), a fat-soluble polyphenol derived from grapes and blueberries, has been recognized as a powerful natural antioxidant and anti-inflammatory agent. Gallic acid (GA), a hydrophilic polyphenol widely distributed in various plants, possesses high antioxidant and antibacterial activity. However, most natural active substances, including PTS and GA, are highly sensitive to the external environment and are prone to premature degradation and loss in the gastric environment, resulting in reduced bioavailability. Furthermore, given the significant differences in solubility between hydrophilic and hydrophobic active substances, food delivery systems require both hydrophobic and hydrophilic microenvironments. These bottlenecks limit the co-application of hydrophilic / hydrophobic active ingredients in the final food matrix, let alone how to construct a low-fat functional food matrix that can mimic the texture of cheese while possessing the ability to co-deliver hydrophilic / hydrophobic active substances.

[0004] Bigels are an emerging two-phase colloidal system, typically prepared by combining oleogels and hydrogels. Due to their ability to replicate the sensory and textural properties of high-fat foods, bigels are considered a novel fat alternative in the food industry. Furthermore, the structured oleogels and hydrogels in bigels provide ideal differential polar phases for the dynamic delivery of lipophilic and hydrophilic functional agents, respectively. However, the microstructure of traditional bigels is often singular (mostly O / W, W / O, or bicontinuous), frequently failing to simultaneously achieve cheese texture simulation and controlled-release functionality. Moreover, the interfacial stability of traditional bigels is usually achieved using chemical additives such as low-molecular-weight crystalline gelling agents (e.g., glyceryl stearate), which presents a challenge in aligning with the current trend of green food labeling. Additionally, the preparation of the oleogels in traditional bigels usually involves high-temperature processes, which may lead to the high-temperature degradation and inactivation of the loaded active functional agents. Therefore, there is an urgent need to develop a mild and environmentally friendly method for preparing bigels and to optimize their microstructure to achieve a balance between cheese texture simulation and the co-delivery of hydrophilic / hydrophobic active substances. Summary of the Invention

[0005] The main objective of this invention is to provide a dual gel with an O1 / W / O2 microstructure, its preparation method, and its application, in order to overcome the shortcomings of the prior art.

[0006] To achieve the aforementioned objectives, the technical solution adopted by this invention includes:

[0007] This invention provides a method for preparing a dual gel with an O1 / W / O2 microstructure, comprising:

[0008] Whey protein isolate was used to prepare whey protein aggregates. The whey protein aggregates were mixed with oil and hydrophobic active substances and homogenized to obtain an oleogel loaded with hydrophobic active substances.

[0009] Guar gum was mixed with water and a hydrophilic active substance and fully hydrated to obtain a hydrogel loaded with the hydrophilic active substance.

[0010] Furthermore, the oleogel loaded with hydrophobic active material is mixed with the hydrogel loaded with hydrophilic active material and homogenized to form a bigel with an O1 / W / O2 microstructure through in-situ self-assembly.

[0011] The present invention also provides a bigel with an O1 / W / O2 microstructure prepared by the aforementioned preparation method.

[0012] This invention also provides the application of the aforementioned dual gel with O1 / W / O2 microstructure in cheese texture simulation or co-delivery of hydrophilic / hydrophobic active substances.

[0013] This invention also provides a cheese-like texture material, which includes the aforementioned dual gel with an O1 / W / O2 microstructure.

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0015] (1) This invention constructs a dual gel with an O1 / W / O2 microstructure;

[0016] (2) Compared with traditional single-structure dual gels, the dual gel with O1 / W / O2 microstructure in this invention can take into account both the texture simulation of cheese and the co-delivery function of hydrophilic / hydrophobic active substances. The dual gel better simulates the texture, rheological properties and melting properties of commercial cheese with its more extended and continuous network structure under multiple interfaces. It also achieves more precise intestinal controlled release of PTS / GA through a multiphase sequential degradation mode in the gastrointestinal tract. Based on the good controlled release performance, the dual gel can effectively improve the bioaccessibility and antioxidant activity of loaded PTS / GA after digestion in the gastrointestinal tract.

[0017] (3) Compared with the traditional dual-gel preparation process, the preparation of the dual-gel with O1 / W / O2 microstructure in this invention uses only natural polysaccharide (guar gum) and dairy by-product (whey protein isolate) as raw materials, which is beneficial to the green label compatibility of the product; at the same time, the mild processing technology (room temperature homogenization) effectively avoids the problem of thermal degradation of active ingredients caused by high temperature process. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 Macroscopic views of the oil gel WPO and hydrogel GGH of the present invention, the O / W type bigel WGB (O / W) of Comparative Example 1, the bicontinuous type bigel WGB (OW) of Comparative Example 2, the O1 / W / O2 type bigel WGB (O1 / W / O2) of Example 1, and commercial cream cheese.

[0020] Figure 2 Laser confocal scanning microscope (CLSM) images and corresponding structural schematic diagrams of the O / W type bigel WGB (O / W) of Comparative Example 1, the bicontinuous type bigel WGB (OW) of Comparative Example 2, and the O1 / W / O2 type bigel WGB (O1 / W / O2) of Example 1 of this invention (scale bar: 100 μm).

[0021] Figures 3a-3f Frequency-dependent viscoelasticity plots of the oleogel WPO, hydrogel GGH, O / W type bigel WGB (O / W) of Comparative Example 1, bicontinuous type bigel WGB (OW) of Comparative Example 2, O1 / W / O2 type bigel WGB (O1 / W / O2) of Example 1, and commercial cream cheese.

[0022] Figures 4a-4f Temperature-dependent viscoelasticity graphs of the oleogel WPO, hydrogel GGH, O / W type bigel WGB (O / W) of Comparative Example 1, bicontinuous type bigel WGB (OW) of Comparative Example 2, O1 / W / O2 type bigel WGB (O1 / W / O2) of Example 1, and commercial cream cheese.

[0023] Figures 5a-5cThe graph shows the hardness, cohesive force, and viscosity of the oleogel WPO, hydrogel GGH, commercial cream cheese, O / W type bigel WGB (O / W) of Comparative Example 1, bicontinuous type bigel WGB (OW) of Comparative Example 2, and O1 / W / O2 type bigel WGB (O1 / W / O2) of Example 1.

[0024] Figures 6a-6d The cumulative release rate of PTS / GA loaded in simulated gastric and intestinal fluids in the oleogel WPO, hydrogel GGH, O / W type bigel WGB (O / W) of Comparative Example 1, bicontinuous type bigel WGB (OW) of Comparative Example 2, and O1 / W / O2 type bigel WGB (O1 / W / O2) of Example 1 is shown in the figure.

[0025] Figures 7a-7b PTS / GA loaded in the oleogel WPO, hydrogel GGH, O / W type bigel WGB (O / W) of Comparative Example 1, bicontinuous type bigel WGB (OW) of Comparative Example 2, and O1 / W / O2 type bigel WGB (O1 / W / O2) of Example 1, and bioaccessibility diagram of free PTS / GA after simulated digestion.

[0026] Figures 8a-8d The PTS / GA loaded in the oleogel WPO, hydrogel GGH, O / W type bigel WGB (O / W) of Comparative Example 1, bicontinuous type bigel WGB (OW) of Comparative Example 2, and O1 / W / O2 type bigel WGB (O1 / W / O2) of Example 1, as well as free PTS / GA in ABTS after simulated digestion. + DPPH free radical scavenging activity diagram. Detailed Implementation

[0027] In view of the deficiencies of the prior art, the inventors of this case, through long-term research and extensive practice, have proposed the technical solution of this invention. The technical solution of this invention will be clearly and completely described below. Obviously, the described embodiments are only some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0028] This invention uses guar gum (GG) as a hydrogel matrix, co-hydrating it with GA and deionized water to form a GA-loaded hydrogel GGH; and uses whey protein isolate aggregates (WPA) as an oleogel agent, rapidly dispersing them with PTS and corn oil to form a PTS-loaded oleogel WPO; and prepares a bigel WGB (O1 / W / O2) with a unique O1 / W / O2 microstructure by homogenizing the oleogel WPO and the hydrogel GGH together. This structure is achieved and stabilized by hydrogen bonding crosslinking of WPA and GG at the O1 / W and W / O2 interfaces. Compared with traditional bigels, WGB (O1 / W / O2) better simulates the texture, rheological properties, and melting properties of commercial cheese due to its more extended and continuous network structure at multiple interfaces. Furthermore, the multiphase sequential degradation mode of WGB (O1 / W / O2) in the gastrointestinal tract enables more precise controlled release of PTS / GA into the intestine. The preparation of WGB (O1 / W / O2) uses only natural polysaccharides (guar gum) and dairy byproducts (whey protein isolate) as raw materials, without involving other additives. This helps improve the product's green label compatibility. Furthermore, the mild processing technology (room temperature homogenization) effectively solves the problem of heat sensitivity of loaded active substances, avoiding the risk of component degradation caused by traditional high-temperature processing. Currently, no research has constructed a dual gel with an O1 / W / O2 multi-interface structure using green processes to achieve both low-fat cheese texture simulation and the co-delivery of hydrophilic / hydrophobic active substances.

[0029] Specifically, as one aspect of the technical solution of this invention, a method for preparing a dual gel with an O1 / W / O2 microstructure includes:

[0030] Whey protein isolate was used to prepare whey protein aggregates. The whey protein aggregates were mixed with oil and hydrophobic active substances and homogenized to obtain an oleogel loaded with hydrophobic active substances.

[0031] Guar gum was mixed with water and a hydrophilic active substance and fully hydrated to obtain a hydrogel loaded with the hydrophilic active substance.

[0032] Furthermore, the oleogel loaded with hydrophobic active material is mixed with the hydrogel loaded with hydrophilic active material and homogenized to form a bigel with an O1 / W / O2 microstructure through in-situ self-assembly.

[0033] In some preferred embodiments, the preparation method specifically includes:

[0034] (1) Whey protein isolate is mixed with water and subjected to a first magnetic stirring and standing treatment to obtain a whey protein isolate stock solution. Then, the pH is adjusted to acidic and subjected to water bath heating, ice bath cooling, and a first homogenization treatment. Then, it is centrifuged, washed, and freeze-dried to obtain whey protein aggregates. The whey protein aggregates are mixed with oil, and then hydrophobic active substances are added and subjected to a second magnetic stirring and a second homogenization treatment to obtain an oleogel loaded with hydrophobic active substances.

[0035] (2) Guar gum is mixed with water and subjected to a third stirring treatment to form a guar gum aqueous solution. Then, a hydrophilic active substance is added and a fourth stirring treatment is continued. After hydration treatment, a hydrogel loaded with hydrophilic active substance is obtained.

[0036] (3) The oleogel loaded with hydrophobic active material and the hydrogel loaded with hydrophilic active material are subjected to a third homogenization treatment using a high-speed dispersion device to fully mix the two phases and form a double gel with an O1 / W / O2 microstructure through in-situ self-assembly.

[0037] Further, the whey protein isolate stock solution in step (1) has a whey protein isolate concentration of 2-15 wt%.

[0038] Furthermore, the mass ratio of the whey protein aggregates to oil is 2:3 to 5:3.

[0039] Furthermore, the mass ratio of the hydrophobic active substance to the whey protein aggregate, the oil mixture, and the hydrophobic active substance is 0.05-0.2:100.

[0040] Furthermore, in step (1), the speed of the first magnetic stirring is 100-1000 rpm, and the time is 1-5 h.

[0041] Furthermore, the settling temperature is 4-10℃ and the time is 18-24h.

[0042] Furthermore, the pH of the whey protein isolate stock solution is adjusted to 5.0-6.0 using hydrochloric acid solution; preferably, the concentration of the hydrochloric acid solution is 0.5-2 mol / L.

[0043] Furthermore, the water bath heating temperature is 80-95℃, and the time is 10-25 minutes.

[0044] Furthermore, the ice bath cooling time is 5-20 minutes.

[0045] Furthermore, the first homogenization process is carried out at a speed of 10,000-15,000 rpm for a time of 2-8 minutes.

[0046] Furthermore, the centrifugation conditions include: centrifugation at 3500-6000g for 15-35 minutes at 20-35℃.

[0047] Furthermore, the washing is performed 2-4 times.

[0048] Furthermore, the second magnetic stirring speed is 100-800 rpm, and the time is 20-50 min.

[0049] Furthermore, the second homogenization process is carried out at a speed of 10,000-15,000 rpm for 5-20 minutes.

[0050] Furthermore, the oil mentioned in step (1) includes any one or more combinations of corn oil, soybean oil, sunflower oil, and flaxseed oil, and is not limited thereto.

[0051] Furthermore, the hydrophobic active substance includes any one or more combinations of pterostilbene, resveratrol, curcumin, and quercetin, and is not limited thereto.

[0052] Furthermore, the concentration of the guar gum aqueous solution in step (2) is 0.5-1.5 wt%.

[0053] Further, mix guar gum with water at 60-80°C.

[0054] Furthermore, the third stirring process is carried out at a speed of 300-1000 rpm for a duration of 1-3 hours.

[0055] Furthermore, the fourth stirring process is carried out at a speed of 300-1000 rpm for a time of 20-30 min.

[0056] Furthermore, the mass ratio of the hydrophilic active substance to the guar gum aqueous solution and the sum of the two hydrophilic active substances is 0.05-0.2:100.

[0057] Furthermore, the hydration treatment is carried out at a temperature of 4-10°C for 18-24 hours.

[0058] Furthermore, the hydrophilic active substance includes any one or more combinations of gallic acid, catechin, epigallocatechin, and chlorogenic acid, and is not limited thereto.

[0059] Further, in step (3), the mass ratio of the oleogel loaded with hydrophobic active material to the hydrogel loaded with hydrophilic active material is 3:7-7:3, preferably 6:4.

[0060] Furthermore, the third homogenization process is performed at a speed of 6000-12000 rpm for a time of 1-10 min.

[0061] In some preferred embodiments, the method for preparing the dual gel with the O1 / W / O2 microstructure includes the following steps:

[0062] (1) Preparation of oleogel WPO: Whey protein isolate powder was added to deionized water, magnetically stirred, and allowed to stand overnight to obtain a whey protein isolate stock solution. The pH of the stock solution was adjusted to acidic with hydrochloric acid solution, heated in a water bath, and then cooled in an ice bath. The system was then homogenized using a high-speed disperser. The homogenized system was centrifuged to collect the precipitate, which was redispersed in deionized water and centrifuged again. After repeated washing, whey protein aggregates (WPA) were obtained. The freeze-dried WPA powder was added to corn oil, along with pterostilbene (PTS). After magnetic stirring until homogenized, the mixture was homogenized using a high-speed disperser to obtain PTS-loaded oleogel WPO.

[0063] (2) Preparation of GGH hydrogel: Guar gum was added to deionized water and stirred for a certain period of time. Gallic acid (GA) was then added and stirring was continued until completely homogeneous. The solution was cooled to room temperature and allowed to stand to ensure that the system was fully hydrated, thus obtaining GA-loaded GGH hydrogel.

[0064] (3) Preparation of O1 / W / O2 microstructured bigel WGB(O1 / W / O2): Using a high-speed disperser, the oleogel WPO and hydrogel GGH were homogenized to ensure thorough mixing of the two phases, and in situ self-assembled to form bigel WGB(O1 / W / O2) with O1 / W / O2 microstructure.

[0065] Preferably, in step (1), the concentration of whey protein isolate added is (2-15%, w / w).

[0066] Preferably, in step (1), the magnetic stirring conditions are as follows: stirring continuously at a speed of 100-1000 rpm for 1-5 hours.

[0067] Preferably, in step (1), the overnight standing conditions are 18-24 h at 4-10 °C.

[0068] Preferably, in step (1), the concentration of hydrochloric acid solution is 0.5-2 mol / L.

[0069] Preferably, in step (1), the stock solution is adjusted to an acidic pH of 5.0-6.

[0070] Preferably, in step (1), the water bath heating conditions are 80-95℃ and heating for 10-25 minutes.

[0071] Preferably, in step (1), the ice bath cooling time is 5-20 min.

[0072] Preferably, in step (1), the homogenization process is performed at a speed of 10,000-15,000 rpm for 2-8 minutes.

[0073] Preferably, in step (1), the centrifugation conditions after homogenization are: centrifugation at 3500-6000g for 15-35 minutes at 20-35℃.

[0074] Preferably, in step (1), the washing is repeated 2-4 times.

[0075] Preferably, in step (1), the mixing ratio of WPA and corn oil is WPA powder: corn oil = 2:3-5:3 (w / w).

[0076] Preferably, in step (1), the concentration of added PTS is 0.05-0.2% (w / w).

[0077] Preferably, in step (1), the magnetic stirring conditions after adding PTS are: stirring at a speed of 100-800 rpm for 20-50 min.

[0078] Preferably, in step (1), the conditions for high-speed homogenization are to homogenize at a speed of 10,000-15,000 rpm for 5-20 minutes.

[0079] Preferably, in step (2), the concentration of the guar gum aqueous solution is (0.5-1.5%, w / w).

[0080] Preferably, in step (2), the temperature of the deionized water is 60-80℃.

[0081] Preferably, in step (2), the stirring conditions are: stirring at a speed of 300-1000 rpm for 1-3 hours.

[0082] Preferably, in step (2), the concentration of GA added is 0.05-0.2% (w / w).

[0083] Preferably, in step (2), the stirring time after adding gallic acid is 20-30 minutes.

[0084] As a preferred option, in step (2), the condition to ensure that the system is fully hydrated is to place it at 4-10℃ for 18-24 hours.

[0085] Preferably, in step (3), the ratio of oleogel WPO to hydrogel GGH is WPO:GGH = 6:4 (w / w).

[0086] Preferably, in step (3), the homogenization conditions are: homogenize at a speed of 6000-12000 rpm for 1-10 min.

[0087] Another aspect of the present invention provides a bigel with an O1 / W / O2 microstructure prepared by the aforementioned preparation method.

[0088] Another aspect of the present invention provides the application of the aforementioned dual gel with O1 / W / O2 microstructure in cheese texture simulation or co-delivery of hydrophilic / hydrophobic active substances.

[0089] Another aspect of the present invention provides a cheese-like texture material comprising the aforementioned dual gel having an O1 / W / O2 microstructure.

[0090] The technical solution of the present invention will be further described in detail below with reference to several preferred embodiments and accompanying drawings. This embodiment is implemented on the premise of the technical solution of the invention, and provides detailed implementation methods and specific operation processes. However, the protection scope of the present invention is not limited to the following embodiments.

[0091] Unless otherwise specified, the experimental materials used in the examples below can be purchased from conventional biochemical reagent companies.

[0092] Example 1

[0093] (1) Preparation of whey protein isolate (WPO): Whey protein isolate powder was dissolved in deionized water (10%, w / w), stirred at 500 rpm for 2 h, and then allowed to stand at 4 °C for 24 h to obtain a whey protein isolate stock solution. The pH of the stock solution was adjusted to 5.7 using 1 mol / L hydrochloric acid solution, heated in an 85 °C water bath for 15 min, cooled in an ice bath for 5 min, and then homogenized at 13000 rpm for 3 min. The homogenized solution was centrifuged at 25 °C and 4000 g for 20 min, and the precipitate was collected. The precipitate was redispersed in deionized water and centrifuged twice, and the precipitate was collected to obtain whey protein aggregates (WPA). The freeze-dried WPA powder was mixed with corn oil at a ratio of 4:3 (w / w), PTS (0.1%, w / w) was added, and the mixture was magnetically stirred for 30 min, and then homogenized again at 13000 rpm for 10 min to obtain PTS-loaded oleogel (WPO).

[0094] (2) Preparation of hydrogel GGH: Guar gum (1%, w / w) was added to deionized water at 75℃ and stirred at 700 rpm for 1.5 h. GA (0.1%, w / w) was added and stirring was continued for 30 min. After the solution cooled to room temperature, it was placed at 4℃ for 24 h to ensure complete hydration of the system, and finally GA-loaded hydrogel GGH was obtained.

[0095] (3) Preparation of O1 / W / O2 microstructured bigel WGB (O1 / W / O2): Using a high-speed disperser, oleogel WPO and hydrogel GGH (WPO:GGH=6:4) were homogenized at 10000 rpm for 1 min to ensure that the two phases were fully mixed and self-assembled in situ to form bigel WGB (O1 / W / O2) with O1 / W / O2 microstructure.

[0096] Example 2

[0097] (1) Preparation of whey protein isolate (WPO): Whey protein isolate powder was dissolved in deionized water (8%, w / w), stirred at 500 rpm for 2 h, and then allowed to stand at 4 °C for 24 h to obtain a whey protein isolate stock solution. The pH of the stock solution was adjusted to 5.7 using 1 mol / L hydrochloric acid solution, heated in a 90 °C water bath for 15 min, cooled in an ice bath for 5 min, and then homogenized at 13000 rpm for 3 min. The homogenized solution was centrifuged at 25 °C and 5000 g for 20 min, and the precipitate was collected. The precipitate was redispersed in deionized water and centrifuged twice, and the precipitate was collected to obtain whey protein aggregates (WPA). The freeze-dried WPA powder was mixed with corn oil at a ratio of 4:3 (w / w), PTS (0.1%, w / w) was added, and the mixture was magnetically stirred for 30 min, and then homogenized again at 13000 rpm for 10 min to obtain PTS-loaded WPO oleogel.

[0098] (2) Preparation of hydrogel GGH: Guar gum (1%, w / w) was added to deionized water at 75℃ and stirred at 700 rpm for 1.5 h. GA (0.1%, w / w) was added and stirring was continued for 30 min. After the solution cooled to room temperature, it was placed at 4℃ for 24 h to ensure complete hydration of the system, and finally GA-loaded hydrogel GGH was obtained.

[0099] (3) Preparation of O1 / W / O2 microstructured bigel WGB (O1 / W / O2): Using a high-speed disperser, oleogel WPO and hydrogel GGH (WPO:GGH=6:4) were homogenized at 10000 rpm for 1 min to ensure that the two phases were fully mixed and self-assembled in situ to form bigel WGB (O1 / W / O2) with O1 / W / O2 microstructure.

[0100] Example 3

[0101] (1) Preparation of whey protein isolate (WPO): Whey protein isolate powder was dissolved in deionized water (10%, w / w), stirred at 500 rpm for 2 h, and then allowed to stand at 4 °C for 24 h to obtain a whey protein isolate stock solution. The pH of the stock solution was adjusted to 5.7 using 1 mol / L hydrochloric acid solution, heated in an 85 °C water bath for 15 min, cooled in an ice bath for 5 min, and then homogenized at 13000 rpm for 3 min. The homogenized solution was centrifuged at 25 °C and 4000 g for 20 min, and the precipitate was collected. The precipitate was redispersed in deionized water and centrifuged twice, and the precipitate was collected to obtain whey protein aggregates (WPA). The freeze-dried WPA powder was mixed with corn oil at a ratio of 4:3 (w / w), PTS (0.2%, w / w) was added, and the mixture was magnetically stirred for 30 min, and then homogenized again at 13000 rpm for 10 min to obtain PTS-loaded oleogel (WPO).

[0102] (2) Preparation of hydrogel GGH: Guar gum (1%, w / w) was added to deionized water at 60℃ and stirred at 800 rpm for 1.5 h. GA (0.1%, w / w) was added and stirring was continued for 30 min. After the solution cooled to room temperature, it was placed at 4℃ for 24 h to ensure complete hydration of the system, and finally GA-loaded hydrogel GGH was obtained.

[0103] (3) Preparation of O1 / W / O2 microstructured bigel WGB (O1 / W / O2): Using a high-speed disperser, oleogel WPO and hydrogel GGH (WPO:GGH=6:4) were homogenized at 10000 rpm for 1 min to ensure that the two phases were fully mixed and self-assembled in situ to form bigel WGB (O1 / W / O2) with O1 / W / O2 microstructure.

[0104] Example 4

[0105] (1) Preparation of whey protein isolate (WPO): Whey protein isolate powder was dissolved in deionized water (10%, w / w), stirred at 500 rpm for 2 h, and then allowed to stand at 4 °C for 24 h to obtain a whey protein isolate stock solution. The pH of the stock solution was adjusted to 5.7 using 0.5 mol / L hydrochloric acid solution, heated in an 85 °C water bath for 15 min, cooled in an ice bath for 5 min, and then homogenized at 13000 rpm for 3 min. The homogenized solution was centrifuged at 25 °C and 4000 g for 20 min, and the precipitate was collected. The precipitate was redispersed in deionized water and centrifuged twice, and the precipitate was collected to obtain whey protein aggregates (WPA). The freeze-dried WPA powder was mixed with corn oil at a ratio of 4:3 (w / w), PTS (0.1%, w / w) was added, and the mixture was magnetically stirred for 30 min, and then homogenized again at 13000 rpm for 10 min to obtain PTS-loaded oleogel (WPO).

[0106] (2) Preparation of hydrogel GGH: Guar gum (1%, w / w) was added to deionized water at 75℃ and stirred at 1000 rpm for 1.5 h. GA (0.2%, w / w) was added and stirring was continued for 20 min. After the solution cooled to room temperature, it was placed at 4℃ for 20 h to ensure complete hydration of the system, and finally GA-loaded hydrogel GGH was obtained.

[0107] (3) Preparation of O1 / W / O2 microstructured bigel WGB(O1 / W / O2): Using a high-speed disperser, oleogel WPO and hydrogel GGH (WPO:GGH=6:4) were homogenized at 8000 rpm for 2 min to allow the two phases to be fully mixed and self-assembled in situ to form bigel WGB(O1 / W / O2) with O1 / W / O2 microstructure.

[0108] Comparative Example 1

[0109] (1) Preparation of whey protein isolate (WPO): Whey protein isolate powder was dissolved in deionized water (10%, w / w), stirred at 500 rpm for 2 h, and then allowed to stand at 4 °C for 24 h to obtain a whey protein isolate stock solution. The pH of the stock solution was adjusted to 5.7 using 1 mol / L hydrochloric acid solution, heated in an 85 °C water bath for 15 min, cooled in an ice bath for 5 min, and then homogenized at 13000 rpm for 3 min. The homogenized solution was centrifuged at 25 °C and 4000 g for 20 min, and the precipitate was collected. The precipitate was redispersed in deionized water and centrifuged twice, and the precipitate was collected to obtain whey protein aggregates (WPA). The freeze-dried WPA powder was mixed with corn oil at a ratio of 4:3 (w / w), PTS (0.1%, w / w) was added, and the mixture was magnetically stirred for 30 min, and then homogenized again at 13000 rpm for 10 min to obtain PTS-loaded oleogel (WPO).

[0110] (2) Preparation of hydrogel GGH: Guar gum (1%, w / w) was added to deionized water at 75℃ and stirred at 700 rpm for 1.5 h. GA (0.1%, w / w) was added and stirring was continued for 30 min. After the solution cooled to room temperature, it was placed at 4℃ for 24 h to ensure complete hydration of the system, and finally GA-loaded hydrogel GGH was obtained.

[0111] (3) Preparation of O1 / W / O2 microstructured bigel WGB (O1 / W / O2): Using a high-speed disperser, oleogel WPO and hydrogel GGH (WPO:GGH=3:7) were homogenized at 10000 rpm for 1 min to allow the two phases to be fully mixed and self-assembled in situ to form bigel WGB (O / W) with O / W structure.

[0112] Comparative Example 2

[0113] (1) Preparation of whey protein isolate (WPO): Whey protein isolate powder was dissolved in deionized water (10%, w / w), stirred at 500 rpm for 2 h, and then allowed to stand at 4 °C for 24 h to obtain a whey protein isolate stock solution. The pH of the stock solution was adjusted to 5.7 using 1 mol / L hydrochloric acid solution, heated in an 85 °C water bath for 15 min, cooled in an ice bath for 5 min, and then homogenized at 13000 rpm for 3 min. The homogenized solution was centrifuged at 25 °C and 4000 g for 20 min, and the precipitate was collected. The precipitate was redispersed in deionized water and centrifuged twice, and the precipitate was collected to obtain whey protein aggregates (WPA). The freeze-dried WPA powder was mixed with corn oil at a ratio of 4:3 (w / w), PTS (0.1%, w / w) was added, and the mixture was magnetically stirred for 30 min, and then homogenized again at 13000 rpm for 10 min to obtain PTS-loaded oleogel (WPO).

[0114] (2) Preparation of hydrogel GGH: Guar gum (1%, w / w) was added to deionized water at 75℃ and stirred at 700 rpm for 1.5 h. GA (0.1%, w / w) was added and stirring was continued for 30 min. After the solution cooled to room temperature, it was placed at 4℃ for 24 h to ensure complete hydration of the system, and finally GA-loaded hydrogel GGH was obtained.

[0115] (3) Preparation of O1 / W / O2 microstructured bigel WGB (O1 / W / O2): Using a high-speed disperser, oleogel WPO and hydrogel GGH (WPO:GGH=5:5) were homogenized at 10000 rpm for 1 min to allow the two phases to be fully mixed and self-assembled in situ to form bigel WGB (OW) with a bicontinuous structure.

[0116] according to Figure 1 The macroscopic behavioral results show that the oleogel WPO exhibits a semi-solid state, while the hydrogel GGH exhibits fluid-like behavior. The bigels WGB (O / W) with an O / W structure, WGB (OW) with a bicontinuous structure, and WGB (O1 / W / O2) with an O1 / W / O2 microstructure, prepared from a mixture of WPO and GGH, exhibit more solid-like properties. Furthermore, WGB (O1 / W / O2) with the O1 / W / O2 microstructure most closely resembles the appearance of commercial cream cheese. This is because the encapsulated aqueous phase between the two oil phases enhances the lubrication properties of the bigel, making it closer to the texture of traditional cheese products.

[0117] Figure 2 The microstructures and schematic diagrams of the O / W, bicontinuous, and O1 / W / O2 of the bigel WGB(O / W), bigel WGB(OW), and bigel WGB(O1 / W / O2) are shown.

[0118] Figures 3a-3f The rheological frequency scanning results show that the traditional O / W structure WGB(O / W)( Figure 3c ) and the dual continuous structure WGB(OW)( Figure 3d The G′ values ​​of the ) were 40 times lower and 1.63 times higher than those of commercial cheese, respectively. However, after forming the O1 / W / O2 bigel WGB (O1 / W / O2), its G′ / G″ value and frequency response were closer to those of commercial cheese. Figure 3e The difference is only 1.01 times. Therefore, WGB(O1 / W / O2) avoids excessive rigidity in texture while maintaining structural stability. This balanced viscoelastic-ductile property satisfies the stability requirements of bigels in functional food applications while maintaining the authenticity of cheese texture.

[0119] Figures 4a-4f The rheological temperature scanning results showed that the modulus-temperature curve of the commercial cheese exhibited three distinct stages: (1) a sharp increase in modulus between 30-40℃; (2) a gradual increase in modulus between 40-70℃; and (3) a final decrease in modulus after 70℃. Figure 4f It is worth noting that WGB(O1 / W / O2) is highly consistent with this three-phase mode. Figure 4e Specifically, the initial modulus decrease of WGBs at 30-40°C, dominated by oil-phase melting, may simulate the melting process of cheese during human oral processing. The subsequent modulus increase (40-70°C) may simulate the functional properties of cheese during heat treatment processes such as baking, including melting uniformity, stringiness, and anti-exudation properties. When the temperature exceeds 70°C, the final modulus decrease simulates the process of cheese completely melting and integrating with food ingredients at high temperatures. In short, bigel WGBs (O1 / W / O2) with an O1 / W / O2 structure can simulate the multi-stage temperature response behavior of commercial cream cheese during heating, including "network softening, partial cross-linking, and complete melting."

[0120] Figures 5a-5c Texture analysis results showed that the hardness, cohesiveness, and viscosity values ​​of the O1 / W / O2 microstructured WGB (O1 / W / O2) were closest to those of commercial cheese, with no significant differences (p < 0.05). This indicates that WGB (O1 / W / O2) achieves an optimal balance between fat reduction and texture simulation, and can effectively simulate the mouthfeel smoothness of commercial cheese, as well as its integrity during processing, such as slicing.

[0121] Figures 6a-6d The results show that, compared to WGB(O / W) and WGB(OW), WGB(O1 / W / O2) achieves the best gastric environmental protection effect in terms of PTS and GA load. Figures 6a-6b(lowest cumulative release rate in gastric juice) and precise controlled release effect in the intestine ( Figures 6c-6d The highest cumulative release rate is observed in intestinal fluid. This may stem from the sacrificial protective effect of the outermost O2 layer on the inner O1 / W droplets, delaying the release of PTS and GA during gastric digestion. During intestinal digestion, the rapid expansion of the intermediate aqueous phase W in the SIF leads to structural disruption, while the inner oil phase O1 is exposed and subsequently decomposed by pancreatic lipases. This triggers the simultaneous and precise release of PTS and GA in the intestinal tract.

[0122] like Figures 7a-7b As shown, free PTS and GA exhibited significantly lower bioavailability (7.40% and 9.32%, respectively) due to their instability in the digestive environment. Compared with the free compounds, loading into the bigel WGB significantly improved their bioavailability. Furthermore, compared with the conventional structures of WGB(O / W) and WGB(OW), WGB(O1 / W / O2) maximized the bioavailability of the two active ingredients (PTS 73.56%; GA 79.59%) due to its superior gastric environmental protection and intestinal controlled-release effects.

[0123] Figures 8a-8d The results showed that, as phenolic compounds, free PTS and GA exhibited significantly poorer ABTS after digestion. + And DPPH free radical scavenging activity. Although loading of monogel WPO and GGH, and bigel WGB(O / W) and WGB(OW) improved the free radical scavenging activity of PTS and GA, the antioxidant capacity provided by these systems was still limited. In contrast, WGB(O1 / W / O2) showed the best performance in enhancing antioxidant effect (PTS: 54.86% ABTS, 63.28% DPPH; GA: 86.08% ABTS, 32.68% DPPH), a result consistent with the bioavailability test results. These findings confirm that the microstructure of the bigel determines its controlled-release performance during gastrointestinal digestion. Compared with the traditional O / W or bicontinuous structure, WGB(O1 / W / O2) with the novel O1 / W / O2 microstructure can achieve precise co-delivery of hydrophilic and hydrophobic bioactive ingredients in the intestine, and can maximize their bioavailability and antioxidant activity.

[0124] In addition, the inventors of this case also conducted experiments with other raw materials, process operations, and process conditions described in this specification, referring to the aforementioned embodiments, and obtained relatively ideal results in all cases.

[0125] It should be understood that the technical solutions of the present invention are not limited to the specific embodiments described above. Any technical modifications made to the technical solutions of the present invention without departing from the spirit and scope of the claims are within the scope of protection of the present invention.

Claims

1. A method for preparing a bigel with an O1 / W / O2 microstructure, characterized in that, include: Whey protein isolate was used to prepare whey protein aggregates. The whey protein aggregates were mixed with oil and hydrophobic active substances and homogenized to obtain an oleogel loaded with hydrophobic active substances. Guar gum was mixed with water and a hydrophilic active substance and fully hydrated to obtain a hydrogel loaded with the hydrophilic active substance. Furthermore, the oleogel loaded with hydrophobic active material is mixed with the hydrogel loaded with hydrophilic active material and homogenized to form a bigel with an O1 / W / O2 microstructure through in-situ self-assembly.

2. The preparation method according to claim 1, characterized in that, Specifically, it includes: (1) Whey protein isolate is mixed with water and subjected to a first magnetic stirring and standing treatment to obtain a whey protein isolate stock solution. Then, the pH is adjusted to acidic and subjected to water bath heating, ice bath cooling, and a first homogenization treatment. Then, it is centrifuged, washed, and freeze-dried to obtain whey protein aggregates. The whey protein aggregates are mixed with oil, and then hydrophobic active substances are added and subjected to a second magnetic stirring and a second homogenization treatment to obtain an oleogel loaded with hydrophobic active substances. (2) Guar gum is mixed with water and subjected to a third stirring treatment to form a guar gum aqueous solution. Then, hydrophilic active substances are added and a fourth stirring treatment is continued. After hydration treatment, a hydrogel loaded with hydrophilic active substances is obtained. (3) The oleogel loaded with hydrophobic active material and the hydrogel loaded with hydrophilic active material are subjected to a third homogenization treatment using a high-speed dispersion device to fully mix the two phases and form a double gel with an O1 / W / O2 microstructure through in-situ self-assembly.

3. The preparation method according to claim 2, characterized in that: The whey protein isolate stock solution described in step (1) has a mass concentration of 2-15 wt%; And / or, the mass ratio of the whey protein aggregates to oil is 2:3 to 5:3; And / or, the mass ratio of the hydrophobic active substance to the whey protein aggregate, the oil mixture, and the hydrophobic active substance is 0.05-0.2:

100.

4. The preparation method according to claim 2, characterized in that: In step (1), the speed of the first magnetic stirring is 100-1000 rpm, and the time is 1-5 h; And / or, the settling temperature is 4-10℃ and the time is 18-24h; And / or, the pH of the whey protein isolate stock solution is adjusted to 5.0-6.0 using hydrochloric acid solution; preferably, the concentration of the hydrochloric acid solution is 0.5-2 mol / L; And / or, the water bath heating temperature is 80-95℃, and the time is 10-25 min; And / or, the ice bath cooling time is 5-20 minutes; And / or, the first homogenization process is performed at a speed of 10,000-15,000 rpm for a time of 2-8 min; And / or, the centrifugation conditions include: centrifugation at 3500-6000g for 15-35 min at 20-35°C; And / or, the number of washes is 2-4; And / or, the second magnetic stirring speed is 100-800 rpm, and the time is 20-50 min; And / or, the second homogenization process is performed at a speed of 10,000-15,000 rpm for 5-20 minutes.

5. The preparation method according to claim 2, characterized in that: The oil mentioned in step (1) includes any one or more combinations of corn oil, soybean oil, sunflower oil, and flaxseed oil; And / or, the hydrophobic active substance includes any one or more combinations of pterostilbene, resveratrol, curcumin, and quercetin.

6. The preparation method according to claim 2, characterized in that: The concentration of the guar gum aqueous solution in step (2) is 0.5-1.5 wt%. And / or, mix guar gum with water at 60-80°C; And / or, the third stirring treatment is performed at a speed of 300-1000 rpm for a time of 1-3 hours; And / or, the fourth stirring treatment is performed at a speed of 300-1000 rpm for a time of 20-30 min; And / or, the mass ratio of the hydrophilic active substance to the guar gum aqueous solution and the sum of the hydrophilic active substances is 0.05-0.2:100; And / or, the hydration treatment is performed at a temperature of 4-10°C for a time of 18-24 hours; And / or, the hydrophilic active substance includes any one or more combinations of gallic acid, catechin, epigallocatechin, and chlorogenic acid.

7. The preparation method according to claim 2, characterized in that: The mass ratio of the oleogel loaded with hydrophobic active material to the hydrogel loaded with hydrophilic active material in step (3) is 3:7-7:3, preferably 6:4; And / or, the third homogenization process is performed at a speed of 6000-12000 rpm for a time of 1-10 min.

8. A bigel with an O1 / W / O2 microstructure prepared by the preparation method according to any one of claims 1-7.

9. The application of the dual gel with O1 / W / O2 microstructure as described in claim 8 in cheese texture simulation or co-delivery of hydrophilic / hydrophobic active substances.

10. A cheese-like texture material, characterized in that: The cheese-like texture material comprises the dual gel with an O1 / W / O2 microstructure as described in claim 8.

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