Hermetia illucens oil enzymolysis self-gel as well as preparation method and application thereof
By enzymatically hydrolyzing black soldier fly oil to generate a self-assembled three-dimensional network structure of monoglycerides, the safety and cost issues of exogenous gelling agents are solved, and the stability and applicability of oleogels are improved, making them suitable for functional foods, cosmetics and pharmaceuticals.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-22
- Publication Date
- 2026-03-17
AI Technical Summary
Existing oleogel technologies rely on exogenous gelling agents, which raises safety and regulatory approval issues, and their high cost limits commercialization. Black soldier fly oil has poor oxidative stability, and exogenous antioxidants are not safe enough.
By adding lipase and glycerol to black soldier fly oil, glycerol monoester is generated through enzymatic hydrolysis. The monoester is then used to self-assemble into a three-dimensional network structure, thus constructing a self-gelling system that does not rely on exogenous gelling agents.
The oleogels, which achieve high thermal and oxidative stability, are suitable for functional foods, cosmetics, and pharmaceuticals, reducing production costs.
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Figure CN121668079A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of gel preparation, in particular to a black soldier fly oil enzymatic self-gel and a preparation method and application thereof. BACKGROUND
[0002] Oil gel is a kind of semi-solid or solid material with three-dimensional network system formed by structuring liquid oil through gelator. It shows broad application prospects in food, medicine and cosmetics, etc. In the food industry, oil gel can be used as a healthy fat substitute to simulate the texture and mouthfeel of solid fat; in the medical field, its good biocompatibility makes it an excellent drug carrier; in cosmetics, it can combine the moisturizing property of oil and the stability of gel.
[0003] However, existing oil gel technology usually relies on adding exogenous gelators (such as natural wax, ethyl cellulose, monoglyceride, etc.) to build a three-dimensional network structure. These exogenous gelators face two major challenges: first, the safety and regulatory approval status of most gelators limit their application in food and medicine, cosmetics, etc.; second, the high production cost of high-quality gelators restricts the commercialization of oil gel technology.
[0004] Black soldier fly oil is a new type of sustainable oil rich in medium-chain fatty acids (especially lauric acid) and unsaturated fatty acids, with biological activities such as antibacterial and anti-inflammatory. However, its high content of unsaturated fatty acids is prone to oxidation, which leads to quality deterioration and shortens the shelf life, limiting its high-value application. In existing technology, the addition of synthetic or natural antioxidants can alleviate the oxidation problem, but there are potential health risks or limited effects; and if it is prepared into a traditional oil gel, it will also face the problems brought by the above-mentioned exogenous gelators. SUMMARY
[0005] In view of the technical problems in the background art, the present application provides a black soldier fly oil enzymatic self-gel and a preparation method and application thereof, aiming to solve the technical problems of poor oxidation stability of black soldier fly oil and insufficient safety of exogenous gelators and antioxidants.
[0006] In a first aspect, the present application provides a preparation method of a black soldier fly oil enzymatic self-gel, comprising the following steps: S1, adding lipase and glycerol to black soldier fly oil, homogenizing and stirring to obtain an emulsion; S2, incubating the emulsion at a constant temperature to obtain a black soldier fly oil enzymatic self-gel.
[0007] In a second aspect, the present application provides a black soldier fly oil enzymatic self-gel, which is prepared by the above method.
[0008] In a third aspect, the embodiments of the present application provide an application of the black soldier fly oil enzymatic self-gel in the field of functional food, cosmetics or pharmaceutical preparations.
[0009] Compared with the prior art, the beneficial effects of the present application include: The present application uses lipase to treat black soldier fly oil to increase the proportion of monoglyceride in the oil, and uses the gelation of monoglyceride itself to construct a self-gel system that does not depend on other gel agents and has excellent stability and microstructure. The obtained oil gel sample has high thermal stability, good oxidation stability, good oil retention rate and texture characteristics, and is suitable for use in functional food, cosmetics and pharmaceuticals.
[0010] The above description is only a summary of the technical solutions of the present application. In order to more clearly understand the technical means of the present application, the following specific embodiments of the present application can be implemented according to the content of the specification, and in order to make the above and other purposes, characteristics and advantages of the present application more obvious and easy to understand, the following specific embodiments of the present application are described. BRIEF DESCRIPTION OF DRAWINGS
[0011] In order to more clearly illustrate the technical solutions of the present application, the following will briefly introduce the drawings used in the present application. Obviously, the drawings described below are only some embodiments of the present application, and those skilled in the art can also obtain other drawings according to these drawings without creating any creative labor.
[0012] Figure 1 The polarizing microscope scanning diagram of the black soldier fly oil of the present application.
[0013] Figure 2 The polarizing microscope scanning diagram of the gel prepared in Example 1 of the present application.
[0014] Figure 3 The polarizing microscope scanning diagram of the gel prepared in Example 2 of the present application.
[0015] Figure 4 The polarizing microscope scanning diagram of the gel prepared in Example 3 of the present application.
[0016] Figure 5 The oil retention rate detection results of Examples 1-3 of the present application.
[0017] Figure 6 The texture characteristic detection results of the gels prepared in Examples 1-3 and Comparative Examples 2-3 of the present application.
[0018] Figure 7 The oxidation stability detection results of the black soldier fly oil and the gel prepared in Example 3 of the present application. DETAILED DESCRIPTION
[0019] The technical solutions of the present application will be described in detail below with reference to the drawings. The following embodiments are only used to more clearly illustrate the technical solutions of the present application, and therefore only serve as examples, but cannot limit the protection scope of the present application.
[0020] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the present application belongs; the terms used herein are only for the purpose of describing specific embodiments of the present application, and are not intended to limit the present application; the terms "include" and "have" and any variations thereof in the specification and claims of the present application and the above description of drawings are intended to cover non-exclusive inclusion.
[0021] Existing oil gel technology usually relies on the addition of exogenous gelling agents (such as natural wax, ethyl cellulose, monoglyceride, etc.) to build a three-dimensional network structure. These exogenous gelling agents face two major challenges: first, the safety and regulatory approval status of most gelling factors limit their application in food and medicine, cosmetics and other fields; second, the high production cost of high-quality gelling agents restricts the commercialization and popularization of oil gel technology.
[0022] In order to solve the technical problems of poor oxidation stability of black soldier fly oil, and insufficient safety of exogenous gelling agents and antioxidants, the present application provides a black soldier fly oil enzymatic self-gel and a preparation method and application thereof. The present application uses lipase to treat black soldier fly oil to increase the proportion of monoglyceride in the oil, and uses the gelation of monoglyceride itself to build a self-gel system that does not rely on other gelling agents, has excellent stability and microstructure. The obtained oil gel sample has high thermal stability, good oxidation stability, good oil retention rate and texture characteristics, and is suitable for use in functional food, cosmetics and medicaments.
[0023] In a first aspect, the embodiments of the present application provide a preparation method of a black soldier fly oil enzymatic self-gel, comprising the following steps: S1, adding lipase and glycerol to black soldier fly oil, homogenizing and stirring to obtain an emulsion; S2, incubating the emulsion at a constant temperature to obtain a black soldier fly oil enzymatic self-gel.
[0024] Further, in some embodiments, the lipase is Burkholderia cepacia lipase (PS lipase).
[0025] In the technical solutions of the embodiments of the present application, the PS lipase enzymatically digests the black soldier fly oil at a specific reaction temperature and time, and the main component of the black soldier fly oil in a liquid state is triglyceride, which is converted into diglyceride and monoglyceride by the PS lipase.
[0026] Triglycerides undergo a two-step controlled hydrolysis catalyzed by PS lipase: the lipase first attacks and cleaves the ester bond at the sn-1 or sn-3 position of the glycerol backbone, releasing a free fatty acid and generating diglyceride; subsequently, the enzyme continues to hydrolyze the remaining terminal ester bond of the diglyceride, releasing a second free fatty acid, ultimately mainly generating 2-monoglyceride. The enzymatic generation of monoglycerides eliminates the need for exogenous addition, saving costs.
[0027] When the content of monoglycerides exceeds 8%, monoglyceride molecules can self-assemble into a microscopic three-dimensional network structure in the oil. This structure effectively imprisons the liquid oil within it through surface tension and capillary action, thus exhibiting the macroscopic properties of a solid, namely an oil gel.
[0028] Furthermore, in some embodiments, the mass of the lipase is 2% to 4% of the mass of black soldier fly oil.
[0029] Furthermore, in some embodiments, the glycerol mass is 10% to 20% of the mass of black soldier fly oil.
[0030] In the technical solution of this application embodiment, adding glycerol to the raw materials can promote the conversion of triglycerides to monoglycerides and improve the conversion rate of monoglycerides.
[0031] Furthermore, in some embodiments, the homogenizing stirring speed is 6000~8000 r / min.
[0032] Furthermore, in some embodiments, the homogenization mixing time is 3 to 5 minutes.
[0033] Furthermore, in some embodiments, the isothermal incubation temperature is 20~25°C.
[0034] Furthermore, in some embodiments, the isothermal incubation time is 24-36 hours.
[0035] Secondly, embodiments of this application provide a black soldier fly oil enzymatic hydrolysis self-gel, which is prepared using the above method.
[0036] Thirdly, embodiments of this application provide an application of black soldier fly oil enzymatic hydrolysis self-gel in the fields of functional foods, cosmetics, or pharmaceutical preparations.
[0037] The following are some specific embodiments. It should be noted that the embodiments described below are exemplary and are only used to explain this application, and should not be construed as limiting this application. Where specific techniques or conditions are not specified in the embodiments, they shall be performed in accordance with the techniques or conditions described in the literature in this field or according to the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be obtained commercially.
[0038] I. Preparation Method Example 1 A method for preparing a self-gelled black soldier fly oil enzymatic hydrolysis product includes the following steps: After centrifuging black soldier fly oil at 8000 r / min for 20 min, take 10 g of the supernatant and add 1.0% PS lipase and 10% glycerol in sequence. Stir and homogenize at 8000 r / min for 3 min, and then react the emulsion at 25℃ for 24 h.
[0039] Example 2 A method for preparing a self-gelled black soldier fly oil enzymatic hydrolysis product includes the following steps: After centrifuging black soldier fly oil at 8000 r / min for 20 min, take 10 g of the supernatant and add 1.5% PS lipase and 10% glycerol in sequence. Stir and homogenize at 8000 r / min for 3 min, and then react the emulsion at 25℃ for 24 h.
[0040] Example 3 A method for preparing a self-gelled black soldier fly oil enzymatic hydrolysis product includes the following steps: After centrifuging black soldier fly oil at 8000 r / min for 20 min, take 10 g of the supernatant and add 2.0% PS lipase and 10% glycerol in sequence. Stir and homogenize at 8000 r / min for 3 min, and then react the emulsion at 25℃ for 24 h.
[0041] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that no glycerin was added.
[0042] Comparative Example 2 A method for preparing a self-gelled black soldier fly oil enzymatic hydrolysis product includes the following steps: After centrifuging black soldier fly oil at 8000 r / min for 20 min, take 10 g of the supernatant and add 2.5% PS lipase and 10% glycerol in sequence. Stir and homogenize at 8000 r / min for 3 min, and then react the emulsion at 25℃ for 24 h.
[0043] Comparative Example 3 A method for preparing a self-gelled black soldier fly oil enzymatic hydrolysis product includes the following steps: After centrifuging black soldier fly oil at 8000 r / min for 20 min, take 10 g of the supernatant and add 3.0% PS lipase and 10% glycerol in sequence. Stir and homogenize at 8000 r / min for 3 min, and then react the emulsion at 25℃ for 24 h.
[0044] II. Testing Methods 1. Oil retention rate test method: Place the oleogel sample (b) into a centrifuge tube (a) and centrifuge. Invert the tube for 30 min to remove the precipitated oil. Weigh the remaining sample and the mass of the centrifuge tube (c) and calculate the oil retention rate. Oil retention rate (%) = (ca / b) × 100.
[0045] 2. Textural properties testing method: Take an appropriate amount of oleogloss sample and measure its hardness, chewiness, and adhesiveness using a texture analyzer.
[0046] 3. Oxidative stability test method: Weigh 2.0 g of powdered sample (accurate to 0.001 g) into a 50 mL centrifuge tube, add 20 mL of isooctane-isopropanol mixed solvent, vortex for 5 min, sonicate at 40℃ for 15 min (power 300 W), then centrifuge at 4000 rpm for 10 min, and take the supernatant for later use.
[0047] Peroxide value determination: Transfer the supernatant to a 250 mL Erlenmeyer flask and add 10 mL of glacial acetic acid (ensure the system is acidic). Add 1 mL of saturated potassium iodide solution, immediately cover with plastic wrap, shake in the dark for 30 s, and then let stand at room temperature in the dark for 3 min (strictly control the time). Add 100 mL of distilled water and titrate with 0.01 M sodium thiosulfate until a pale yellow color is obtained. Add 1 mL of starch indicator and continue titrating until the blue color disappears (no color return within 30 seconds). Blank experiment: Treat the solvent system without the sample using the same method.
[0048] POV= 100 (g / 100g) Where V is the volume of sodium thiosulfate standard solution consumed by the sample (mL), V0 is the volume of sodium thiosulfate standard solution consumed by the blank test (mL), C is the concentration of sodium thiosulfate standard solution (mol / L), and m is the sample mass (g).
[0049] 4. Thermal stability testing method: The melting and crystallization behavior of the oleogel oil sample was determined using a differential scanning calorimeter. 15–20 mg of the oleogel oil sample was weighed and placed in an aluminum pan, which was then sealed. An empty aluminum pan was used as a reference. The parameters were set as follows: the temperature was lowered to -10°C and held for 2 minutes; then the sealed aluminum pan was heated to 100°C at a heating rate of 10°C / min and held for 2 minutes; finally, the temperature was lowered to -10°C at a cooling rate of -10°C / min.
[0050] III. Analysis of Test Results for Each Embodiment and Comparative Example (1) The black soldier fly oil and the gels prepared in Examples 1-3 were observed using a polarizing microscope to obtain... Figures 1-4 .from Figure 1As can be seen, pure black soldier fly oil exhibits a completely dark field under a polarized light field. This is because liquid oil is an isotropic fluid and does not exhibit birefringence of light, indicating that no ordered crystal structure has yet formed inside it. Figures 2-4 A dense, continuous three-dimensional crystalline network structure was formed within the gel, successfully immobilizing the liquid oil. In Examples 1-3, the monoglyceride content was 8%, 10%, and 12%, respectively. Figures 2-4 The three-dimensional mesh structure in it is becoming increasingly dense.
[0051] (2) The oil retention rate of the gels prepared in Examples 1-3 was measured, and the results are shown in the figure. Figure 5 .from Figure 5 As can be seen, the oil retention rate of the gel gradually increases with the increase of monoglyceride content.
[0052] (3) The textural properties of the gels prepared in Examples 1-3 and Comparative Examples 2-3 were tested, and the test results are shown in the figure. Figure 6 The monoglyceride content in Comparative Examples 2 and 3 was 14% and 16%, respectively. No glycerol was added in Comparative Example 1, resulting in poor gel formation and making it impossible to obtain textural property data.
[0053] from Figure 6 As can be seen, the hardness, chewiness, and adhesiveness of the gel increase with the increase of monoglyceride content. However, excessively hard oil gels have poor spreadability and are unsuitable for cosmetic use, and the required enzyme amount increases, leading to higher costs. A hardness >300 makes it difficult to spread, a chewiness >150 results in a less light feel on the skin, and an adhesiveness of 100-200 indicates strong adhesion, intended for prolonged adhesion to the skin or application site, potentially accompanied by a noticeable stickiness. An adhesiveness >200 is generally considered too sticky, resulting in a poor user experience, difficulty in even application, or interference with subsequent makeup application. Therefore, selecting the preparation parameters in Examples 1-3 yields gels with suitable performance.
[0054] (4) The thermal stability of the gels prepared in Examples 1 to 3 was tested, and the test results are shown in Table 1 below.
[0055] Table 1. Results of thermal stability testing of gels prepared in Examples 1-3
[0056] As can be seen from Table 1, the thermal stability of the gel increases with the increase of the proportion of monoglyceride.
[0057] (5) The oxidative stability of black soldier fly oil and the gel prepared in Example 3 was tested, and the results are as follows: Figure 7As shown, the solid network formed in the self-gel of black soldier fly oil after enzymatic hydrolysis segments and fixes the liquid oil in a micron-sized space, significantly reducing the fluidity of the oil and the diffusion rate of oxygen, thereby slowing down the initiation and transmission of oxidation chain reactions. Simultaneously, this network structure effectively restricts the movement of pro-oxidative components (such as metal ions and free radicals) and physically blocks external oxidizing factors such as light and heat, thus greatly improving the oxidative stability of black soldier fly oil.
[0058] It should be noted that this application is not limited to the above-described embodiments. The above embodiments are merely examples, and any embodiments with the same structure and function as the technical concept within the scope of this application are included in the technical scope of this application. Furthermore, various modifications that can be conceived by those skilled in the art to the embodiments, and other ways of constructing by combining some of the constituent elements of the embodiments, without departing from the spirit of this application, are also included in the scope of this application.
Claims
1. A method of preparing a black soldier fly oil enzymatic self-gel, characterized in that, It comprises the following steps: S1, adding lipase and glycerol into black soldier fly oil, homogenously stirring to obtain an emulsion; S2, culturing the emulsion at constant temperature to obtain black soldier fly oil enzymatic self-gel.
2. The method of claim 1, wherein the black soldier fly oil enzymatic self-gel is prepared by the steps of: The lipase is Burkholderia cepacia lipase.
3. The method of claim 1, wherein the black soldier fly oil enzymatic self-gel is prepared by the steps of: The mass of the lipase is 2%-4% of the mass of the black soldier fly oil.
4. The method of claim 1, wherein the black soldier fly oil enzymatic self-gel is prepared by the steps of: The mass of the glycerol is 10%-20% of the mass of the black soldier fly oil.
5. The method of claim 1, wherein the black soldier fly oil enzymatic self-gel is prepared by the steps of: The rotating speed of the homogenously stirring is 6000-8000 r / min.
6. The method of claim 1, wherein the black soldier fly oil enzymatic self-gel is prepared by the steps of: The homogenously stirring time is 3-5 min.
7. The method of claim 1, wherein the black soldier fly oil enzymatic self-gel is prepared by the steps of: The constant temperature is 20-25 ℃.
8. The method of claim 1, wherein the black soldier fly oil enzymatic self-gel is prepared by the steps of: The constant temperature culturing time is 24-36 h.
9. A black soldier fly oil enzymatic self-gel, characterized in that, The preparation method is prepared according to any one of claims 1-8.
10. The use of the black soldier fly oil enzymatic self-gel according to claim 9 in the field of functional food, cosmetics or pharmaceutical preparations.