Camellia oil containing nano squalene and preparation method thereof

Abstract

The invention provides camellia oil containing nano squalene and a preparation method thereof, and relates to the technical field of food processing, in particular to camellia oil containing nano squalene. According to the scheme, a high-pressure homogeneous emulsification technology and a lipid-surfactant synergistic stabilization mechanism are adopted; the preparation method comprises the following steps: firstly, beeswax (solid lipid), camellia oil and rice oil (liquid lipid) are fused at high temperature to form a uniform oil phase; the interfacial tension is reduced through high-speed stirring, in the high-pressure homogenizing process, lipid liquid drops are broken to nanoscale through mechanical shearing force and the hole effect, and soybean lecithin molecules rapidly wrap new liquid drops to prevent aggregation. And finally, quickly cooling to recrystallize and solidify the beewax, wherein a crystalline region of the beewax can enhance the rigidity of emulsion droplets, lock a nano structure and uniformly disperse squalene to obtain the nano functional camellia oil. Solid lipid of the nano-carrier can form a physical barrier, the contact rate of squalene and oxygen is reduced, the oxidation rate is reduced, and the preparation method is simple in process, high in operability and suitable for large-scale mass production.

Description

Technical Field

[0001] This invention relates to the field of food processing technology, and in particular to a camellia oil containing nano-squalene and its preparation method. Background Technology

[0002] Camellia seed oil, also known as tea tree oil, oriental olive oil, tea oil, and tea seed oil, is a fatty oil extracted from the seeds of the Camellia oleifera Abel., a species belonging to the genus Camellia in the family Theaceae. As a high-quality health-promoting plant fat extracted from Camellia seeds, camellia oil is a natural plant oil, renowned as "longevity oil" and "king of oils." According to modern Traditional Chinese Medicine, camellia oil is neutral in nature and can lower cholesterol, plasma fibrinogen, and blood sugar levels. Regular consumption has significant therapeutic effects on hypertension, cardiovascular disease, cerebrovascular disease, and obesity. Furthermore, applying camellia oil to the skin can have certain cosmetic and skincare benefits.

[0003] Camellia oil is rich in antioxidant active ingredients, among which squalene is a naturally occurring active substance that can enhance superoxide dismutase activity, boost immunity, promote blood circulation, activate cells for anti-oxidation, combat fatigue, reduce inflammation and kill bacteria, and repair cells. However, prolonged exposure to high temperatures and sunlight can accelerate oxidation of camellia oil, leading to a decrease in its content. In particular, the refining process, such as deodorization and decolorization, may destroy squalene.

[0004] Nanocarriers are widely used in the pharmaceutical and food industries due to their advantages such as small size, large specific surface area, and ability to achieve sustained release and targeted release. However, there are few research reports on how to use this innovative technology to maximize the retention of squalene content. Summary of the Invention

[0005] Objectives of the Invention: Firstly, this invention proposes a method for preparing camellia oil containing nano-squalene. Using camellia oil itself as a liquid lipid component, solid lipids, emulsifiers, and active ingredients are added. High-pressure homogenization directly forms a nano-carrier, resulting in camellia oil with a high squalene content, high oxidative stability, and excellent quality. The process is simple, highly operable, and suitable for large-scale production. Secondly, this application provides a camellia oil containing nano-squalene, which has a high squalene content and high oxidative stability and quality.

[0006] Technical solution:

[0007] In a first aspect, this application provides a camellia oil containing nano-squalene, comprising a liquid lipid and nano-solid particles dispersed in the liquid lipid, wherein the liquid lipid comprises camellia oil, and the nano-solid particles comprise squalene, solid lipids encapsulating squalene, and a surfactant; the solid lipid comprises any one or a combination of several of beeswax, carnauba wax, palmitic acid, and stearic acid; and the surfactant comprises any one or a combination of several of soybean lecithin, egg yolk lecithin, monoglyceride fatty acid ester, diglyceride fatty acid ester, diacetyl tartaric acid monoglyceride, sucrose fatty acid ester, Span surfactants, and Tween surfactants.

[0008] Optionally, the mass ratio of camellia oil to nano solid particles is 85-88:1-50, and the mass ratio of solid lipids, surfactants and squalene is 1-20:1-20:1-20.

[0009] Optionally, the mass ratio of camellia oil to nano solid particles is 85-88:1-20, and the mass ratio of solid lipids, surfactants and squalene is 1-10:1-10:1-10.

[0010] Preferably, the mass ratio of camellia oil to nano solid particles is 85-88:6-25, and the mass ratio of solid lipids, surfactants and squalene is 3-8:1-5:2-5.

[0011] More preferably, the mass ratio of camellia oil to nano solid particles is 85-88:7-16, and the mass ratio of solid lipids, surfactants and squalene is 3-8:2-3:2-5.

[0012] More preferably, the mass ratio of camellia oil to nano solid particles is 85-88:7-10, and the mass ratio of solid lipids, surfactants and squalene is 3-4:2-3:2-3.

[0013] More preferably, the solid lipid includes any one or a combination of several of beeswax, carnauba wax, lecithin, and sucrose esters.

[0014] Furthermore, the solid lipid is beeswax, and the surfactant is soybean lecithin.

[0015] Furthermore, the liquid lipid also includes vitamin E, and the mass ratio of vitamin E to camellia oil is 0.05-0.35:85-90.

[0016] Furthermore, the liquid lipid also includes vitamin E, and the mass ratio of vitamin E to camellia oil is 0.1-0.2:85-90.

[0017] Furthermore, the liquid lipid also includes rice bran oil, and the mass ratio of rice bran oil to camellia oil is 4-5:85-90.

[0018] Rice bran oil, as a liquid lipid, can be used directly as a carrier for active ingredients and is also rich in squalene, which can synergistically enhance their effects.

[0019] Secondly, this application provides a method for preparing camellia oil containing nano-squalene:

[0020] A method for preparing camellia oil containing nano-squalene includes the following preparation steps:

[0021] 1) Melting: Solid lipids and liquid lipids are mixed in a certain proportion and heated to a temperature higher than the melting point of the solid lipids to melt them;

[0022] 2) Emulsification: Add surfactants and squalene and stir at high speed to form a primary emulsion;

[0023] 3) High-pressure homogenization: Nanoemulsions are formed through high-pressure homogenization;

[0024] 4) Cooling and solidification: Rapid cooling or ice bath cooling is used to obtain camellia oil containing nano-squalene by cooling it below the melting point of solid lipids.

[0025] Further, in step 1), the temperature is heated to 75-85°C; in step 3), the high-pressure homogenization condition is 150-200 bar; and the average particle size of the nanoemulsion is 80-300 nm.

[0026] Furthermore, the cooling and solidification conditions described in step 4) are as follows: using an ice bath to rapidly reduce the temperature from the homogeneous temperature to a low temperature of 0-4℃; or using a circulating cooling system with a temperature drop rate of 20-30℃ / minute; and controlling the cooling time within 5 minutes.

[0027] Beneficial effects: 1. The high-pressure homogenization emulsification technology and lipid-surfactant synergistic stabilization mechanism in this scheme: First, beeswax (solid lipid) melts with camellia oil and rice bran oil (liquid lipid) at high temperature to form a homogeneous oil phase; after adding surfactant and squalene, the interfacial tension is reduced by high-speed stirring. During the high-pressure homogenization process, mechanical shear force and cavitation effect break the lipid droplets into nanoscale. Soy lecithin molecules, as surfactants, quickly encapsulate the newly formed droplets to prevent aggregation. Finally, rapid cooling causes the beeswax to recrystallize and solidify. The crystalline region of beeswax can enhance the rigidity of the emulsion droplets, lock the nanostructure, and uniformly disperse the squalene in the nano-functional camellia oil. The solid lipid of the nanocarrier can form a physical barrier, reducing the contact rate between squalene and oxygen, and reducing the oxidation rate. Moreover, the preparation method of this invention is simple, highly operable, and suitable for large-scale mass production.

[0028] 2. The optimal mass ratio of solid lipids, surfactants and squalene is selected to ensure that the squalene in camellia oil containing nano-squalene has a high encapsulation rate, stability and antioxidant properties.

[0029] 3. Furthermore, the addition of nano-sized vitamin E and rice bran oil can synergistically enhance antioxidant properties, encapsulation rate, and stability; the nano-carrier can simultaneously encapsulate polyphenols, synergistically improving the sensory flavor of tea oil. At the same time, the nano-carrier can increase light transmittance, resolving the cloudiness issue of tea oil. Detailed Implementation

[0030] To make the technical solution of the present invention clearer, the present invention will be further described in detail below with reference to specific embodiments.

[0031] Example 1

[0032] A method for preparing camellia oil containing nano-squalene, using raw materials as shown in Table 1, includes the following preparation steps:

[0033] 1) Melting: Mix solid lipids (beeswax) and liquid lipids (camellia oil) in a certain proportion and heat to 80°C above the melting point of the lipids.

[0034] 2) Emulsification: Add surfactant (soy lecithin) and squalene, and stir at high speed to form a primary emulsion.

[0035] 3) High-pressure homogenization: At the same temperature, the mixture is cyclically processed 4 times by a high-pressure homogenizer (180 bar) to form a nanoemulsion.

[0036] 4) Cooling and solidification: Rapid cooling is achieved by using a circulating cooling system to quickly reduce the temperature from the homogeneous temperature to a low temperature of 0-4℃. The temperature drop rate is 25℃ / minute, and the cooling time is controlled within 5 minutes. After cooling, camellia oil containing nano-squalene is obtained.

[0037] Examples 2 to 5

[0038] A method for preparing camellia oil containing nano-squalene differs from Example 1 in that the raw materials and preparation process settings are different, as detailed in Table 1.

[0039] Table 1. List of raw materials and preparation process settings used in the methods of Examples 1 to 5

[0040]

[0041] Example 6

[0042] A method for preparing camellia oil containing nano-squalene differs from Example 1 in that stearic acid is used to replace beeswax in equal amounts in the solid lipid.

[0043] Examples 7 to 11

[0044] A method for preparing camellia oil containing nano-squalene differs from Example 1 in that the liquid lipid further includes vitamin E and / or rice bran oil, as detailed in Table 2.

[0045] Table 2. List of Vitamin E and Rice Bran Oil Used in the Methods of Examples 1 and 7 to 11

[0046]

[0047] Comparative Example 1

[0048] The preparation of a functional camellia oil containing nano-squalene differs from the nano-squalene preparation method in Example 1 in that no solid lipid beeswax is added.

[0049] Comparative Example 2

[0050] The preparation of a functional camellia oil containing nano-squalene differs from the nano-squalene preparation method in Example 1 in that soybean lecithin is not added.

[0051] Comparative Example 3

[0052] The preparation of a functional camellia oil containing nano-squalene differs from the nano-squalene preparation method in Example 1 in that no squalene is added.

[0053] Performance testing

[0054] The free squalene content was determined by ultrafiltration centrifugation, the encapsulation efficiency (>85%) was calculated, and the peroxide value and acid value were tested. The test results are shown in Table 3.

[0055] 1. Encapsulation efficiency: The free squalene content was determined using ultrafiltration centrifugation. The sample solution was diluted and placed in ultrafiltration centrifuge tubes, centrifuged (4000 r / min, 20-30 min), and the filtrate (containing free squalene) was collected. The concentration of free squalene in the filtrate was analyzed by HPLC (C18 column, acetonitrile-isopropanol mobile phase, 215 nm detection), and the content was calculated using a standard curve. Total squalene content calculation: The total content was directly measured after demulsification. The encapsulation efficiency calculation formula is as follows:

[0056] EE% = (1 - free squalene / total squalene) * 100.

[0057] 2. Peroxide value (POV) test: in accordance with GB 5009.227-2023 "National Food Safety Standard - Determination of Peroxide Value in Food".

[0058] 3. Acid value determination: in accordance with GB 5009.229-2016 "National Food Safety Standard - Determination of Acid Value in Food".

[0059] Table 3. Performance test results of camellia oil obtained using the methods of Examples 1-11 and Comparative Examples 1-3

[0060]

[0061] Compared with Example 1, Example 4 uses a smaller amount of soybean lecithin; compared with Example 1, Example 5 uses a larger amount of soybean lecithin. Excessive soybean lecithin can easily form reverse micelles or multilayer structures, leading to increased system viscosity, reduced physical stability of the nanoemulsion, and wider particle size distribution. When soybean lecithin is insufficient, the synergistic effect between soybean lecithin and solid lipids deteriorates, the emulsion particles are prone to aggregation, resulting in increased particle size, loss of nano-properties, and decreased transparency and stability.

[0062] Compared to Example 1, in Example 6, stearic acid replaced beeswax in an equal amount, resulting in a decrease in the encapsulation rate of squalene. The unsaturated double bonds in squalene were easily oxidized to form peroxides, leading to an increase in the peroxide value. This may be because stearic acid has a high melting point, and the interfacial film formed in conjunction with lecithin is too rigid, potentially hindering droplet deformation. Additionally, the carboxyl groups of stearic acid can bind to the phosphate groups of lecithin, reducing emulsification efficiency.

[0063] The results of Examples 1 and 7-11 show that rice bran oil can be directly used as a carrier for active ingredients. It is rich in squalene and can synergistically enhance the effects of squalene. Vitamin E, as an antioxidant, synergistically increases antioxidant capacity with squalene, preventing the oxidative degradation of the nanocarrier. Rice bran oil has strong antioxidant capacity, and its synergistic effect with vitamin E...

[0064] It further enhances the free radical scavenging ability, delays the oxidative rancidity of camellia oil and squalene, and improves the physical stability of the emulsion. On the other hand, the hydrophobic segments of the nano-sized vitamin E small molecule lipids can be well embedded in lipid phases such as camellia oil, rice bran oil and beeswax, which can better protect the squalene in the nano-emulsion droplets from oxidative degradation.

[0065] However, when the vitamin E content is too high, the free radical intermediates generated during the self-oxidation process accumulate and trigger new oxidation chain reactions. Therefore, excessive vitamin E may transform from an antioxidant to a pro-oxidant under the high temperature conditions of processing, accelerating lipid oxidation. High concentrations of vitamin E may interfere with the emulsification of soybean lecithin, leading to the aggregation of nanodroplets or an increase in particle size.

[0066] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention. Therefore, the scope of protection of this patent should be determined by the appended claims.

Claims

1. A camellia oil containing nano-squalene, characterized in that, The invention comprises liquid lipids and nano-solid particles dispersed in the liquid lipids. The liquid lipids include camellia oil, and the nano-solid particles include squalene, solid lipids encapsulated with squalene, and surfactants. The solid lipids include any one or a combination of several of beeswax, carnauba wax, palmitic acid, and stearic acid. The surfactants include any one or a combination of several of soybean lecithin, egg yolk lecithin, monoglyceride fatty acid esters, diglyceride fatty acid esters, diacetyl tartaric acid monoglyceride, sucrose fatty acid esters, Span surfactants, and Tween surfactants.

2. The camellia oil containing nano-squalene according to claim 1, characterized in that, The mass ratio of camellia oil to nano solid particles is 85-88:6-25, and the mass ratio of solid lipids, surfactants and squalene is 3-8:1-5:2-5.

3. The camellia oil containing nano-squalene according to claim 2, characterized in that, The mass ratio of camellia oil to nano solid particles is 85-88:7-16, and the mass ratio of solid lipids, surfactants and squalene is 3-8:2-3:2-5.

4. The camellia oil containing nano-squalene according to claim 3, characterized in that, The solid lipid is beeswax, and the surfactant is soybean lecithin.

5. A camellia oil containing nano-squalene according to any one of claims 1-4, characterized in that, The liquid lipid also includes vitamin E, and the mass ratio of vitamin E to camellia oil is 0.05-0.35:85-90.

6. A camellia oil containing nano-squalene according to any one of claims 5, characterized in that, The liquid lipid also includes vitamin E, and the mass ratio of vitamin E to camellia oil is 0.1-0.2:85-90.

7. A camellia oil containing nano-squalene according to any one of claims 1-4, 6, characterized in that, The liquid lipid also includes rice bran oil, and the mass ratio of rice bran oil to camellia oil is 4-5:85-90.

8. A method for preparing camellia oil according to any one of claims 1-7, characterized in that, The preparation steps include the following: 1) Melting: Solid lipids and liquid lipids are mixed in a certain proportion and heated to a temperature higher than the melting point of the solid lipids to melt them; 2) Emulsification: Add surfactants and squalene and stir at high speed to form a primary emulsion; 3) High-pressure homogenization: Nanoemulsions are formed through high-pressure homogenization; 4) Cooling and solidification: Rapid cooling or ice bath cooling is used to obtain camellia oil containing nano-squalene by cooling it below the melting point of solid lipids.

9. The method for preparing camellia oil according to claim 8, characterized in that, In step 1), the temperature is heated to 75-85℃; in step 3), the high-pressure homogenization conditions are 150-200 bar; the average particle size of the nanoemulsion is 80-300 nm.

10. The method for preparing camellia oil according to claim 8 or 9, characterized in that, The cooling and solidification conditions described in step 4) are as follows: use an ice bath to rapidly reduce the temperature from the homogeneous temperature to a low temperature of 0-4℃; or use a circulating cooling system with a temperature drop rate of 20-30℃ / minute; and control the cooling time within 5 minutes.

Images