Andrias oil active preparation and preparation method

Abstract

The application relates to the technical field of biological medicine and functional food, and particularly discloses an andrias oil active preparation and a preparation method. The andrias oil active preparation is a microcapsule granule preparation, which comprises a microcapsule core material and a microcapsule wall material; the microcapsule core material comprises the following components in parts by weight: andrias oil 30-50 parts, nervonic acid 5-10 parts, phosphatidylserine 3-8 parts, tea polyphenol palmitate 0.3-0.8 parts and food-grade titanium dioxide 0.05-0.2 parts; and the microcapsule wall material comprises the following components in parts by weight: beta-cyclodextrin 25-30 parts and sodium caseinate 10-15 parts. The application can significantly improve the phenomenon that the unsaturated fatty acids in the andrias oil in the microcapsule core material are easily oxidized, and finally, a high-stability andrias oil active preparation with a significantly prolonged oxidation induction period and suitable for long-term consumption by children is obtained.

Description

Technical Field

[0001] This application relates to the fields of biomedicine and functional food technology, and more specifically, it relates to an active preparation of giant salamander oil and its preparation method. Background Technology

[0002] The giant salamander (Andrias davidianus), commonly known as the Chinese giant salamander, is a rare natural resource with unique nutritional and medicinal value in its oil composition. Studies have shown that giant salamander oil, especially the fat from its tail and abdominal cavity, is rich in long-chain, highly unsaturated fatty acids. Its ω-3 fatty acid content, particularly docosahexaenoic acid (DHA) and eicosapentaenoic acid (EPA), is significantly higher than that of many traditional fish oil sources (such as salmon oil and tuna oil). Despite its excellent nutritional value, the industrial application of giant salamander oil has long faced a near-insurmountable technical obstacle—the inherent extreme instability of its molecules. This is mainly determined by its chemical structure: the DHA / EPA molecular chains each contain unsaturated double bonds. This highly unsaturated structure makes it chemically extremely reactive, readily undergoing complex auto-oxidation chain reactions under the catalysis of light, heat, oxygen, and trace metal ions. This process manifests itself in the following interconnected and serious problems: Rapid deterioration of sensory quality: In the early stages of oxidation, primary oxidation products (such as hydroperoxides) are colorless and odorless, but they decompose rapidly during storage or processing, producing a large number of low-molecular-weight secondary oxidation products, such as hexanal and nonenal. These substances have a strong, unpleasant rancid taste and pungent odor, resulting in extremely poor palatability of the final product and low consumer acceptance, especially unsuitable for children who are sensitive to flavors.

[0003] Irreversible inactivation of bioactive ingredients: The direct consequence of oxidation is the breakage of the chemical structure and alteration of functional groups in active molecules such as DHA / EPA. This not only causes them to lose their core biological functions such as anti-inflammation, but may also produce structurally similar but inactive or even interfering "pseudomolecules," rendering the product's efficacy meaningless and unable to achieve the claimed nutritional and health effects.

[0004] Potential safety concerns: Certain secondary byproducts of deep oxidation, such as 4-hydroxynonenal and malondialdehyde, have been shown to have cytotoxic and pro-inflammatory properties. If the degree of oxidation in the product is not properly controlled, long-term intake may pose potential health risks, which completely contradicts the original intention of functional foods to be "safe and beneficial" and does not meet the stringent safety standards for children's food.

[0005] Therefore, there is an urgent need to propose a solution to address the aforementioned technical problems. Summary of the Invention

[0006] To address the problem that unsaturated fatty acids in giant salamander oil are easily oxidized and rancid, this application provides a highly stable giant salamander oil active preparation with a significantly prolonged oxidation induction period, suitable for long-term consumption by children, and its preparation method.

[0007] In a first aspect, this application provides a giant salamander oil active formulation, which adopts the following technical solution: The active oil preparation of giant salamander is a microcapsule particle preparation, including microcapsule core material and microcapsule wall material; The microcapsule core material comprises the following components in parts by weight: 30-50 parts of giant salamander oil; 5-10 parts of nervonic acid; Phosphatidylserine 3-8 parts; Tea polyphenol palmitate 0.3-0.8 parts; Food-grade titanium dioxide, 0.05-0.2 parts; The microcapsule wall material comprises the following components in parts by weight: 25-30 parts of β-cyclodextrin; Sodium caseinate 10-15 parts.

[0008] By adopting the above technical solution, for the tea polyphenol palmitate and food-grade titanium dioxide in the microcapsule core material, the food-grade titanium dioxide physically blocks the occurrence of photo-oxidation reaction by reflecting and scattering ultraviolet rays; as a fat-soluble antioxidant, tea polyphenol palmitate can be evenly distributed in oils, directly quenching lipid free radicals and interrupting the oxidation chain reaction. Moreover, tea polyphenol palmitate also acts as a "passivating agent" or "isolation layer" for food-grade titanium dioxide at the interface, inhibiting the photocatalytic side effects of food-grade titanium dioxide, thereby allowing the physical light shielding advantage of food-grade titanium dioxide to be manifested, ultimately achieving synergistic antioxidation; at the same time, the combination of tea polyphenol palmitate and food-grade titanium dioxide is not a simple functional superposition, but rather constructs a three-dimensional antioxidation microenvironment of "internal and external synergy and spatiotemporal complementarity", thereby significantly prolonging the overall oxidation induction period.

[0009] In the microcapsule wall material, β-cyclodextrin serves as an inclusion material, and its hydrophobic cavities can encapsulate oil molecules, reducing their contact with oxygen. Sodium caseinate, as a high-quality emulsified protein, forms a continuous and dense film during spray drying, effectively blocking the penetration of oxygen and moisture. The combination of β-cyclodextrin and sodium caseinate can form a wall material structure that combines rigidity and flexibility with multi-level barriers, thereby significantly improving the phenomenon that unsaturated fatty acids in the giant salamander oil in the microcapsule core material are easily oxidized.

[0010] Therefore, in the above technical solution, tea polyphenol palmitate and food-grade titanium dioxide are used to construct an oil-phase antioxidant microenvironment in the microcapsule core material, and high-pressure homogenization microencapsulation is carried out in combination with β-cyclodextrin and sodium caseinate composite wall material to achieve interface barrier encapsulation. This constructs an internal and external dual stabilization mechanism of "antioxidant microenvironment + interface barrier encapsulation", which can ultimately obtain a highly stable giant salamander oil active preparation with a significantly extended oxidation induction period and suitable for long-term consumption by children.

[0011] Preferably, the weight ratio of the microcapsule core material to the microcapsule wall material is (1-1.5):1.

[0012] By adopting the above technical solution, it is ensured that each microcapsule can carry a sufficient dose of giant salamander oil, nervonic acid, and phosphatidylserine, maximizing the dose of active ingredients. It also ensures that the wall material can form a continuous and defect-free "shell", so that the microcapsule core material is completely and intactly encapsulated. Furthermore, it ensures that the optimal balance is achieved between the encapsulation rate and the oxidative stability of the raw materials, resulting in a giant salamander oil active formulation with better overall quality.

[0013] Preferably, the particle size of the microcapsule formulation is 5μm-10μm.

[0014] By adopting the above technical solution, particles of 5μm-10μm have a moderate specific surface area, which not only ensures emulsification efficiency, but also avoids the extremely high oxidation risk caused by the huge surface area due to excessively small particle size, as well as the relatively low release rate caused by excessively large particle size, which leads to a decrease in absorption efficiency. Thus, it ensures that the microcapsule particle formulation not only achieves efficient delivery and absorption of active ingredients, but also exhibits better antioxidant stability.

[0015] Preferably, the microcapsule core material further contains 0.5-1.5 parts by weight of functional additive A, which is composed of rosemary extract and vitamin E, and the weight ratio of rosemary extract to vitamin E is 1:(2-3).

[0016] By adopting the above technical solution, vitamin E will become a less active tocopherol free radical after scavenging free radicals, while rosemary extract (especially sarsaparilla acid) has a strong hydrogen donation capacity, which can quickly "restore" vitamin E back to its active state. The combination of the two establishes a "self-repairing" antioxidant microenvironment, which greatly improves the durability of the antioxidant network. Meanwhile, based on the application of the aforementioned rosemary extract and vitamin E as functional adjuvant A, when trace amounts of oxygen penetrate the wall material and enter the interface, the two combine and distribute on the edge of the oil droplets and the oil-water interface film, preferentially contacting and removing the infiltrated oxygen, which can greatly reduce the probability of oxygen penetrating into the core of the oil phase. Even if free radicals break through the interface and enter the interior of the oil phase, tea polyphenol palmitate, as a "second line of defense," immediately removes them. In this way, by positioning tea polyphenol palmitate in the main body of the oil phase, and distributing natural vitamin E and rosemary extract in the oil phase and interface region, a synergistic free radical quenching and chain blocking effect is formed, thereby constructing a hierarchical, specialized, and regenerable dynamic antioxidant network. This enriches the antioxidant microenvironment built by tea polyphenol palmitate and food-grade titanium dioxide, making the giant salamander oil active preparation exhibit better antioxidant stability.

[0017] Preferably, the weight ratio of the rosemary extract to vitamin E is 1:2.6.

[0018] By adopting the above technical solution, the regeneration cycle efficiency of vitamin E is maximized, and the functional adjuvant A can be combined with tea polyphenol palmitate to exert a better antioxidant effect, resulting in a high-quality giant salamander oil active preparation.

[0019] Preferably, the microcapsule wall material further contains 3-8 parts by weight of functional additive B, wherein the functional additive B is composed of chitosan and tannic acid, and the weight ratio of chitosan to tannic acid is (2-2.8):1.

[0020] By adopting the above technical solution, tannic acid is rich in phenolic hydroxyl groups, which can undergo multiple hydrogen bonding and Schiff base reactions with the amino groups on the chitosan molecular chain to form a three-dimensional network, which greatly enhances the mechanical strength of the wall material. Moreover, the polyphenolic structure of tannic acid not only provides antioxidant activity, but also fills the gaps between chitosan chains through hydrogen bonding and hydrophobic interactions, making the wall material more compact. Meanwhile, the chitosan-tannic acid complex forms a "nanofiber network" in the microcapsule wall material, significantly increasing the tortuous path of oxygen penetration. Tannic acid actively captures and consumes trace amounts of oxygen penetrating the wall material, achieving "intercepting along the way." Thus, it can be seen that functional additive B is not a simple wall material filler, but rather constructs a composite defense layer of "interfacial cross-linking densification + free radical chemical capture." From the two dimensions of diffusion kinetics and reaction thermodynamics, it pushes the oxidative stability of giant salamander oil to the extreme, significantly enhancing the effect of "interfacial barrier encapsulation." This upgrades the wall material from a simple "physical embedding layer" to an "intelligent dynamic barrier" with both mechanical density and chemical oxygen-consuming activity, thereby significantly extending the oxidation induction period. This effectively solves the problem of easy rancidity of unsaturated fatty acids, ultimately resulting in a higher quality giant salamander oil active formulation.

[0021] Preferably, the weight ratio of chitosan to tannic acid is 2.5:1.

[0022] By adopting the above technical solutions, an excess of tannic acid may lead to excessive local cross-linking, making the wall material brittle and prone to microcracks during spray drying; an excess of chitosan may result in some chain segments not being cross-linked, forming loose areas that become "short-circuit channels" for oxygen diffusion; and within the weight ratio of chitosan to tannic acid in the range of (2-2.8):1, a ratio of 2.5:1 can enable functional additive B to exert its corresponding effect better, constructing a solid time buffer for the internal "antioxidant microenvironment", so that the overall active preparation of giant salamander oil exhibits better antioxidant stability.

[0023] Preferably, the giant salamander oil is prepared by the following steps: S1. Take fat from the tail of artificially bred giant salamanders, crush it into granules of 2-3 mm, and obtain pre-treated fat tissue; S2. After mixing the pretreated adipose tissue obtained in step S1 with PBS buffer, add the complex enzyme, and then place it in a constant temperature water bath shaker. Set the temperature to 46-50℃ and the rotation speed to 130-180 rpm, and continue enzymatic hydrolysis for 1.5-2 hours. After the enzymatic hydrolysis is completed, raise the temperature to 90-95℃ and hold for 8-10 minutes to inactivate the enzyme, and obtain the mixture. S3. After centrifuging the mixture obtained in step S2, take the upper oil phase component and mix it with water at 50-60℃. After stirring, centrifuge again to remove the aqueous phase and water-soluble impurities. Then perform vacuum dehydration to obtain giant salamander oil. In step S2 above, the complex enzyme is composed of alkaline protease and flavor protease in a weight ratio of (1.8-2.2):1, and the amount of complex enzyme added is 0.5-1% of the weight of the pretreated adipose tissue.

[0024] By adopting the above technical solutions, the precise particle size control in S1 breaks down the fat cell wall, releases the lipid channels, and avoids excessive fragmentation that leads to the dissolution of a large amount of non-lipid impurities, thus reducing the burden of subsequent purification; in S2, the connection between lipids and membrane proteins is severed by a biological enzyme "scalpel" to achieve "cold extraction"; in S3, 50-60℃ warm water is used to remove water-soluble impurities (such as free fatty acids and fishy substances), and vacuum dehydration is used to completely remove water, the oxidation reaction medium. During the process, a complex enzyme composed of alkaline protease and flavor protease in a weight ratio of (1.8-2.2):1 is used, with the amount of the complex enzyme controlled at 0.5-1% of the weight of the pretreated adipose tissue. The alkaline protease leads the efficient cell wall disruption, while the flavor protease assists in removing bitterness, ensuring both efficient oil release and meeting the stringent flavor requirements of pediatric formulations. The temperature is precisely controlled at 46-50℃, at the enzyme's optimal activity temperature, ensuring enzyme activity while minimizing thermal oxidation. A rotation speed of 130-180 rpm utilizes gentle oscillation to promote enzyme-substrate contact, avoiding severe shear forces that could lead to oil emulsification or oxidation. Finally, rapid high-temperature instantaneous enzyme inactivation completely deactivates the enzyme while minimizing oxidative damage to the oil due to the extremely short time. Thus, the entire process is conducted at a temperature below 50℃ with a very short inactivation time, effectively preventing the thermal degradation and isomerization of polyunsaturated fatty acids. This provides highly active, low-oxidation-starting-point, and superior-flavored giant salamander oil for subsequent "antioxidant microenvironment construction + interface barrier encapsulation."

[0025] Preferably, in step S2, the complex enzyme is composed of alkaline protease and flavor protease in a weight ratio of 2:1, and the amount of complex enzyme added is 0.8% of the weight of the pretreated adipose tissue.

[0026] By adopting the above technical solution, the oil extracted at low temperature with 0.8% enzyme content has a low initial oxidation value, so that the "antioxidant microenvironment" of the microcapsules does not need to consume a large amount of antioxidants to repair the initial damage, and the "timing start point" of the oxidation induction period is significantly delayed; the 2:1 ratio avoids emulsifying impurities such as phospholipids and glycoproteins caused by excessive hydrolysis, so that the wall material of the subsequent microcapsules can form a denser interface film, resulting in better interface barrier encapsulation effect.

[0027] Secondly, this application provides a method for preparing an active preparation of giant salamander oil, using the following technical solution: The preparation method of the active oil preparation of the giant salamander includes the following steps: (1) Prepare raw materials containing giant salamander oil, nervonic acid, phosphatidylserine, tea polyphenol palmitate, food-grade titanium dioxide, β-cyclodextrin and sodium caseinate according to the formula; (2) After mixing the giant salamander oil, nervonic acid, phosphatidylserine, tea polyphenol palmitate and food-grade titanium dioxide in step (1), the mixture is subjected to shear emulsification treatment to obtain a microcapsule core material solution. (3) Mix the β-cyclodextrin and sodium caseinate from step (1) and dissolve them in deionized water to obtain a microcapsule wall material solution. Then add the microcapsule core material solution obtained in step (2) to the microcapsule wall material solution. After high-speed homogenization, spray dry and sieve to obtain the giant salamander oil active preparation.

[0028] By adopting the above technical solution, the three-step process is simple, and both high-speed homogenization and spray drying are mature industrial equipment with high yield, suitable for large-scale production, and can obtain high-quality and stable giant salamander oil active preparations.

[0029] In summary, this application has the following beneficial effects: 1. This application uses tea polyphenol palmitate and food-grade titanium dioxide to construct an oil-phase antioxidant microenvironment in the microcapsule core material, and combines β-cyclodextrin and sodium caseinate composite wall material for high-pressure homogenization microencapsulation to achieve interface barrier encapsulation, thus constructing an internal and external dual stabilization mechanism of "antioxidant microenvironment + interface barrier encapsulation", which can ultimately obtain a highly stable giant salamander oil active preparation with a significantly extended oxidation induction period, suitable for long-term consumption by children; 2. This application uses functional adjuvant A, composed of rosemary extract and vitamin E, in the microcapsule core material, and functional adjuvant B, composed of chitosan and tannic acid, in the microcapsule wall material. This not only enriches the antioxidant microenvironment built by tea polyphenol palmitate and food-grade titanium dioxide, but also significantly enhances the effect of "interface barrier encapsulation". This upgrades the wall material from a simple "physical embedding layer" to an "intelligent dynamic barrier" that combines mechanical density and chemical oxygen consumption activity, thereby enabling the giant salamander oil active formulation to exhibit better oxidation resistance and stability. Detailed Implementation

[0030] The present application will be further described in detail below with reference to preparation examples, embodiments and comparative examples.

[0031] Unless otherwise specified, all raw materials used in the preparation examples, embodiments and comparative examples of this application are commercially available.

[0032] Rosemary extract is food grade, CAS number: 84604-14-8; Chitosan is food grade, with CAS number 9012-76-4.

[0033] Preparation examples of raw materials and / or intermediates Preparation Example 1 A type of giant salamander oil is prepared by the following steps: S1. Take fat from the tail of artificially bred giant salamanders, crush it into granules of 2-3 mm, and obtain pre-treated fat tissue; S2. The pretreated adipose tissue obtained in step S1 was mixed with 0.05M PBS buffer (pH 7.2) at a ratio of 1g:3mL. The compound enzyme was added, and the mixture was placed in a constant temperature water bath shaker. The temperature was set at 48℃ and the rotation speed at 155rpm. The enzyme was continuously hydrolyzed for 1.75h. After the enzyme hydrolysis was completed, the temperature was raised to 92.5℃ and held for 9min to inactivate the enzyme, and the mixture was obtained. S3. After centrifuging the mixture obtained in step S2 (5000×g, 15min), take the upper oil phase component and mix it with an equal volume of water at 55℃. After stirring, centrifuge again (5000×g, 15min) to remove the aqueous phase and water-soluble impurities. Then, perform vacuum dehydration treatment (dehydration at 60℃ and -0.09MPa for 30min) to obtain giant salamander oil.

[0034] Note: In step S2 above, the complex enzyme is composed of alkaline protease and flavor protease in a weight ratio of 2:1, and the amount of complex enzyme added is 0.8% of the weight of the pretreated adipose tissue.

[0035] Preparation Example 2 A type of giant salamander oil, differing from Preparation Example 1, is prepared by the following steps: S1. Take fat from the tail of artificially bred giant salamanders, crush it into granules of 2-3 mm, and obtain pre-treated fat tissue; S2. The pretreated adipose tissue obtained in step S1 was mixed with 0.05M PBS buffer (pH 7.2) at a ratio of 1g:3mL. The compound enzyme was added, and the mixture was placed in a constant temperature water bath shaker. The temperature was set at 46℃ and the rotation speed at 80rpm. The mixture was continuously hydrolyzed for 1.5h. After the hydrolysis was completed, the temperature was raised to 90℃ and held for 10min to inactivate the enzyme, and the mixture was obtained. S3. After centrifuging the mixture obtained in step S2 (5000×g, 15min), take the upper oil phase component and mix it with an equal volume of 60℃ water, stir, and centrifuge again (5000×g, 15min) to remove the aqueous phase and water-soluble impurities. Then, perform vacuum dehydration treatment (dehydration at 60℃ and -0.09MPa for 30min) to obtain giant salamander oil.

[0036] Preparation Example 3 A type of giant salamander oil, differing from Preparation Example 1, is prepared by the following steps: S1. Take fat from the tail of artificially bred giant salamanders, crush it into granules of 2-3 mm, and obtain pre-treated fat tissue; S2. The pretreated adipose tissue obtained in step S1 was mixed with 0.05M PBS buffer (pH 7.2) at a ratio of 1g:3mL. The compound enzyme was added, and the mixture was placed in a constant temperature water bath shaker. The temperature was set at 50℃ and the rotation speed at 130rpm. The enzyme was continuously hydrolyzed for 2h. After the enzyme hydrolysis was completed, the temperature was raised to 95℃ and held for 8min to inactivate the enzyme, and the mixture was obtained. S3. After centrifuging the mixture obtained in step S2 (5000×g, 15min), take the upper oil phase component and mix it with an equal volume of water at 50℃. After stirring, centrifuge again (5000×g, 15min) to remove the aqueous phase and water-soluble impurities. Then, perform vacuum dehydration treatment (dehydration at 60℃ and -0.09MPa for 30min) to obtain giant salamander oil.

[0037] Preparation Example 4 A type of giant salamander oil, which differs from Preparation Example 1 in that, in step S2 above, the complex enzyme is composed of alkaline protease and flavor protease in a weight ratio of 2:1, and the amount of complex enzyme added is 0.75% of the weight of the pretreated adipose tissue.

[0038] Preparation Example 5 A type of giant salamander oil, which differs from Preparation Example 1 in that, in step S2 above, the complex enzyme is composed of alkaline protease and flavor protease in a weight ratio of 1.8:1, and the amount of complex enzyme added is 0.5% of the weight of the pretreated adipose tissue.

[0039] Preparation Example 6 A type of giant salamander oil, which differs from Preparation Example 1 in that, in step S2 above, the complex enzyme is composed of alkaline protease and flavor protease in a weight ratio of 2.2:1, and the amount of complex enzyme added is 1% of the weight of the pretreated adipose tissue.

[0040] Preparation Example 7 A type of giant salamander oil, which differs from Preparation Example 1 in that the complex enzyme is composed of alkaline protease and flavor protease in a weight ratio of 1.7:1.

[0041] Preparation Example 8 A type of giant salamander oil, which differs from Preparation Example 1 in that the complex enzyme is composed of alkaline protease and flavor protease in a weight ratio of 2.3:1.

[0042] Preparation Example 9 A type of giant salamander oil, which differs from Preparation Example 1 in that it does not use flavor protease.

[0043] Preparation Example 10 A type of giant salamander oil differs from Preparation Example 1 in that the same giant salamander tail fat raw material is used, but instead of enzymatic hydrolysis, it is heated in a water bath at 85°C for 2 hours to melt, and then centrifuged to obtain the oil.

[0044] Example Example 1

[0045] The active oil formulation of the giant salamander is a microcapsule particulate formulation, comprising a microcapsule core material and a microcapsule wall material. The components and corresponding weight parts of the microcapsule core material are shown in Table 1, and the components and corresponding weight parts of the microcapsule wall material are shown in Table 2. It is prepared by the following steps: (1) Prepare raw materials containing giant salamander oil, nervonic acid, phosphatidylserine, tea polyphenol palmitate, food-grade titanium dioxide, β-cyclodextrin and sodium caseinate according to the formula; (2) The giant salamander oil, nervonic acid, phosphatidylserine, tea polyphenol palmitate and food-grade titanium dioxide in step (1) are mixed and heated to 40°C, and then sheared and emulsified at 3000 rpm for 15 min to obtain a microcapsule core material solution. (3) Mix the β-cyclodextrin and sodium caseinate from step (1) and dissolve them in deionized water at a ratio of 3g:10mL to obtain a microcapsule wall material solution. Then add the microcapsule core material solution obtained in step (2) to the microcapsule wall material solution. After high-speed homogenization at 12000rpm for 5min, spray dry (inlet air temperature 185℃, outlet air temperature 80℃). After sieving, obtain the giant salamander oil active preparation.

[0046] Note: In the above operations, the giant salamander oil was obtained from Preparation Example 1. The weight ratio of the microcapsule core material to the microcapsule wall material was 1.25:1. The particle size of the microcapsule formulation was 7.5 μm.

[0047] Example 2-3

[0048] The difference between the giant salamander oil active preparation and Example 1 is that the composition and corresponding weight parts of the microcapsule core material are shown in Table 1.

[0049] Table 1. Components and corresponding weight parts (parts / kg) of the microcapsule core material in Examples 1-3.

[0050] Examples 4-5

[0051] The difference between the giant salamander oil active preparation and Example 1 is that the composition and corresponding weight parts of the microcapsule wall material are shown in Table 2.

[0052] Table 2. Components and corresponding weight parts (parts / kg) of the microcapsule wall material in Examples 1 and 4-5.

[0053] Example 6

[0054] The difference between the giant salamander oil active formulation and Example 1 is that the weight ratio of the microcapsule core material to the microcapsule wall material is 1:1.

[0055] Example 7

[0056] The difference between the giant salamander oil active formulation and Example 1 is that the weight ratio of the microcapsule core material to the microcapsule wall material is 1.5:1.

[0057] Example 8

[0058] The difference between the giant salamander oil active formulation and Example 1 is that the microcapsule particle formulation has a particle size of 5 μm.

[0059] Example 9

[0060] The difference between the giant salamander oil active formulation and Example 1 is that the microcapsule particle formulation has a particle size of 10 μm.

[0061] Example 10

[0062] The giant salamander oil active preparation differs from that in Example 1 in that the giant salamander oil was obtained from Preparation Example 2.

[0063] Example 11

[0064] The giant salamander oil active preparation differs from that in Example 1 in that the giant salamander oil was obtained from Preparation Example 3.

[0065] Example 12

[0066] The giant salamander oil active preparation differs from that in Example 1 in that the giant salamander oil was obtained from Preparation Example 4.

[0067] Example 13

[0068] The giant salamander oil active preparation differs from that in Example 1 in that the giant salamander oil was obtained from Preparation Example 5.

[0069] Example 14

[0070] The giant salamander oil active preparation differs from that in Example 1 in that the giant salamander oil was obtained from Preparation Example 6.

[0071] Example 15

[0072] The giant salamander oil active preparation differs from that in Example 1 in that the giant salamander oil was obtained from Preparation Example 7.

[0073] Example 16

[0074] The giant salamander oil active preparation differs from that in Example 1 in that the giant salamander oil was obtained from Preparation Example 8.

[0075] Example 17

[0076] The giant salamander oil active preparation differs from that in Example 1 in that the giant salamander oil was obtained from Preparation Example 9.

[0077] Example 18

[0078] The giant salamander oil active preparation differs from that in Example 1 in that the giant salamander oil was obtained from Preparation Example 10.

[0079] Example 19

[0080] The difference between the giant salamander oil active preparation and Example 1 is that the microcapsule core material also contains 1 part by weight of functional adjuvant A, which is composed of rosemary extract and vitamin E in a weight ratio of 1:2.6, and is used together with the other components in the microcapsule core material.

[0081] Example 20

[0082] The difference between the giant salamander oil active preparation and Example 19 is that the amount of functional adjuvant A added is 0.5 parts by weight.

[0083] Example 21

[0084] The difference between the giant salamander oil active preparation and Example 19 is that the amount of functional adjuvant A added is 1.5 parts by weight.

[0085] Example 22

[0086] The giant salamander oil active preparation differs from that in Example 19 in that functional adjuvant A is composed of rosemary extract and vitamin E in a weight ratio of 1:2.

[0087] Example 23

[0088] The giant salamander oil active preparation differs from that in Example 19 in that functional adjuvant A is composed of rosemary extract and vitamin E in a weight ratio of 1:3.

[0089] Example 24

[0090] The giant salamander oil active preparation differs from that in Example 19 in that functional adjuvant A is composed of rosemary extract and vitamin E in a weight ratio of 1:2.5.

[0091] Example 25

[0092] The giant salamander oil active formulation differs from that in Example 19 in that rosemary extract is not used in the microcapsule core material.

[0093] Example 26

[0094] The giant salamander oil active preparation differs from that in Example 19 in that vitamin E is not used in the microcapsule core material.

[0095] Example 27

[0096] The difference between the giant salamander oil active preparation and Example 1 is that the microcapsule wall material also contains 5.5 parts by weight of functional additive B, which is composed of chitosan and tannic acid in a weight ratio of 2.5:1, and is used in combination with other components in the microcapsule wall material.

[0097] Example 28

[0098] The difference between the giant salamander oil active preparation and Example 27 is that the functional adjuvant B is added in 3 parts by weight.

[0099] Example 29

[0100] The difference between the giant salamander oil active preparation and Example 27 is that the functional adjuvant B is added in 8 parts by weight.

[0101] Example 30

[0102] The giant salamander oil active preparation differs from that in Example 27 in that functional adjuvant B is composed of chitosan and tannic acid in a weight ratio of 2:1.

[0103] Example 31

[0104] The giant salamander oil active preparation differs from that in Example 27 in that functional adjuvant B is composed of chitosan and tannic acid in a weight ratio of 2.8:1.

[0105] Example 32

[0106] The giant salamander oil active preparation differs from that in Example 27 in that functional adjuvant B is composed of chitosan and tannic acid in a weight ratio of 2.4:1.

[0107] Example 33

[0108] The giant salamander oil active formulation differs from that in Example 27 in that chitosan is not used in the microcapsule wall material.

[0109] Example 34

[0110] The giant salamander oil active formulation differs from that in Example 27 in that tannic acid is not used in the microcapsule wall material.

[0111] Comparative Example Comparative Example 1 The difference between the giant salamander oil active preparation and Example 1 is that tea polyphenol palmitate is not used in the microcapsule core material.

[0112] Comparative Example 2 The difference between the giant salamander oil active formulation and Example 1 is that food-grade titanium dioxide was not used in the microcapsule core material.

[0113] Comparative Example 3 The difference between the giant salamander oil active formulation and Example 1 is that food-grade titanium dioxide and tea polyphenol palmitate were not used in the microcapsule core material.

[0114] Comparative Example 4 The giant salamander oil active formulation differs from that in Example 19 in that food-grade titanium dioxide and tea polyphenol palmitate are not used in the microcapsule core material.

[0115] Comparative Example 5 The difference between the giant salamander oil active formulation and Example 1 is that sodium caseinate is not used in the microcapsule wall material.

[0116] Comparative Example 6 The giant salamander oil active formulation differs from that in Example 27 in that sodium caseinate is not used in the microcapsule wall material.

[0117] Comparative Example 7 The difference between the giant salamander oil active formulation and Example 1 is that food-grade titanium dioxide and tea polyphenol palmitate are not used in the microcapsule core material, and sodium caseinate is not used in the microcapsule wall material.

[0118] Performance testing Test samples: The giant salamander oil active preparations obtained in Examples 1-34 were selected as test samples 1-34, and the giant salamander oil active preparations obtained in Comparative Examples 1-7 were selected as control samples 1-7.

[0119] Test methods: (1) Peroxide value (POV) determination, referring to GB5009.227-2016 (determination of peroxide value in food), which reflects the accumulation of hydrogen peroxide.

[0120] (2) Anisamine value (AnV) determination, refer to GB / T24304-2009 (Determination of anisamine value of animal and vegetable oils), which reflects the generation of secondary oxidation products such as aldehydes (degree of rancidity).

[0121] The peroxide value (POV) of the giant salamander oil obtained in Preparation Examples 1-10 was determined as described above, and the test results are recorded in Table 3.

[0122] (3) Accelerated oxidation test: Use a forced convection constant temperature oven, set the temperature to 60℃, take the active preparation of giant salamander oil, put it into a 50mL brown glass wide-mouth bottle, the filling amount is 1 / 3 of the bottle volume; after accelerated oxidation for 90, the accelerated oxidation process is completed.

[0123] Microcapsule disruption and oil extraction: Accurately weigh 2.00 g of microcapsule powder, add 20 mL of n-hexane, and disrupt the cell walls using an ultrasonic cell disruptor (300 W, 3 s sonication, 5 s interval, total 5 min). Centrifuge at 4℃ and 8000 rpm for 10 min, and collect the supernatant (n-hexane phase), which is the extracted pure giant salamander oil. Repeat the extraction once, combine the supernatants, and concentrate to constant weight under nitrogen blowing at 40℃. DHA retention rate determination (GC method): Take 50 mg of extracted oil, add 1 mL of 0.5 mol / L NaOH-methanol solution and 2 mL of n-hexane, react in a water bath at 70 °C for 10 min to prepare fatty acid methyl esters; GC conditions: Chromatographic column: CP-Sil88 (100m × 0.25mm × 0.20μm) - This is crucial for the separation of DHA; Detector: FID, temperature 260℃; Temperature program: Initial 140℃ (hold for 5 min) → Increase to 240℃ at 4℃ / min (hold for 15 min); DHA retention rate (%) = (DHA peak area on day 90 / DHA peak area on day 0) × 100%.

[0124] After conducting the above accelerated oxidation test on test samples 1-34 and control samples 1-7, the test results are recorded in Table 4.

[0125] Table 3. Test results of the giant salamander oil obtained in Preparation Examples 1-10

[0126] Table 4. Test results of test samples 1-34 and control samples 1-7

[0127] Combining Preparation Examples 1-8 and 9-10 with Table 3, it can be seen that in the preparation of giant salamander oil, the combined use of alkaline protease and flavor protease has significant advantages over the use of alkaline protease alone and the traditional hot-melt method. It can provide giant salamander oil with high activity, low oxidation starting point and excellent flavor for the subsequent "antioxidant microenvironment construction + interface barrier encapsulation".

[0128] As can be seen from Examples 1 and Comparative Examples 1-3, 5, and 7, and Table 4, this application utilizes tea polyphenol palmitate and food-grade titanium dioxide to construct an oil-phase antioxidant microenvironment in the microcapsule core material. Combined with a composite wall material of β-cyclodextrin and sodium caseinate, high-pressure homogenization microencapsulation is used to achieve interface barrier encapsulation, which significantly improves DHA retention rate, indicating that the giant salamander oil active preparation product exhibits excellent antioxidant stability. The absence of tea polyphenol palmitate and food-grade titanium dioxide in the microcapsule core material, and the absence of sodium caseinate in the microcapsule wall material, both lead to a significant decrease in DHA retention rate, demonstrating their crucial role in antioxidant activity. Furthermore, adding only either tea polyphenol palmitate or food-grade titanium dioxide to the microcapsule core material, while improving the effect, is limited in magnitude, and the combined effect of the two is far less than that of their combination. Therefore, tea polyphenol palmitate and food-grade titanium dioxide can achieve a significant improvement effect of 1+1>2.

[0129] Combining Examples 1 and 19-24 with Table 4, it can be seen that using functional adjuvant A, composed of rosemary extract and vitamin E, in the microcapsule core material can further improve the DHA retention rate, indicating that the giant salamander oil active preparation can exhibit better antioxidant stability. Furthermore, combining Examples 25-26 with Table 4, it can be seen that while using either rosemary extract or vitamin E alone can improve the corresponding effect, the improvement is limited, and the sum of the improvement effects of using either alone is far less than that of the combination. Therefore, rosemary extract and vitamin E can bring a significant improvement effect of 1+1>2. Combining Comparative Examples 3-4 with Table 4, it can be seen that if the microcapsule core material lacks the use of tea polyphenol palmitate and food-grade titanium dioxide, the corresponding improvement effect brought by functional adjuvant A is greatly reduced. Therefore, functional adjuvant A can bring a synergistic effect on the antioxidant microenvironment constructed by tea polyphenol palmitate and food-grade titanium dioxide.

[0130] Combining Examples 1 and 27-32 with Table 4, it can be seen that the use of functional additive B, composed of chitosan and tannic acid, in the microcapsule wall material can further improve the DHA retention rate, indicating that the active preparation of giant salamander oil can exhibit better oxidative stability. Furthermore, combining Examples 33-34 with Table 4, it can be seen that while using either chitosan or tannic acid alone can improve the effect, the improvement is limited, and the combined effect of their individual additions is far less than that of their combination. Therefore, chitosan and tannic acid can bring a significant improvement effect of 1+1>2. Combining Comparative Examples 5-6 with Table 4, it can be seen that if sodium caseinate is missing from the microcapsule wall material, the improvement effect brought by functional additive B is greatly reduced. Therefore, functional additive B and sodium caseinate can synergistically combine to significantly improve the interfacial barrier encapsulation effect, resulting in better performance in oxidative stability.

[0131] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

Claims

1. A giant salamander oil active preparation, characterized in that, It is a microcapsule particle formulation, including microcapsule core material and microcapsule wall material; The microcapsule core material comprises the following components in parts by weight: 30-50 parts of giant salamander oil; 5-10 parts of nervonic acid; Phosphatidylserine 3-8 parts; Tea polyphenol palmitate 0.3-0.8 parts; Food-grade titanium dioxide, 0.05-0.2 parts; The microcapsule wall material comprises the following components in parts by weight: 25-30 parts of β-cyclodextrin; Sodium caseinate 10-15 parts; The microcapsule core material also contains 0.5-1.5 parts by weight of functional additive A, which is composed of rosemary extract and vitamin E, and the weight ratio of rosemary extract to vitamin E is 1:(2-3). The microcapsule wall material also contains 3-8 parts by weight of functional additive B, which is composed of chitosan and tannic acid, and the weight ratio of chitosan to tannic acid is (2-2.8):

1.

2. The giant salamander oil active preparation according to claim 1, characterized in that: The weight ratio of the microcapsule core material to the microcapsule wall material is (1-1.5):

1.

3. The giant salamander oil active preparation according to claim 1, characterized in that: The microcapsule particle formulation has a particle size of 5μm-10μm.

4. The giant salamander oil active preparation according to claim 1, characterized in that: The weight ratio of rosemary extract to vitamin E is 1:2.

6.

5. The giant salamander oil active preparation according to claim 1, characterized in that: The weight ratio of chitosan to tannic acid is 2.5:

1.

6. The giant salamander oil active preparation according to claim 1, characterized in that: The giant salamander oil is prepared through the following steps: S1. Take fat from the tail of artificially bred giant salamanders, crush it into granules of 2-3mm, and obtain pre-treated fat tissue; S2. After mixing the pretreated adipose tissue obtained in step S1 with PBS buffer, add the complex enzyme, and then place it in a constant temperature water bath shaker. Set the temperature to 46-50℃ and the rotation speed to 130-180 rpm, and continue enzymatic hydrolysis for 1.5-2 hours. After the enzymatic hydrolysis is completed, raise the temperature to 90-95℃ and hold for 8-10 minutes to inactivate the enzyme, and obtain the mixture. S3. After centrifuging the mixture obtained in step S2, take the upper oil phase component and mix it with water at 50-60℃. After stirring, centrifuge again to remove the aqueous phase and water-soluble impurities. Then perform vacuum dehydration to obtain giant salamander oil. In step S2 above, the complex enzyme is composed of alkaline protease and flavor protease in a weight ratio of (1.8-2.2):1, and the amount of complex enzyme added is 0.5-1% of the weight of the pretreated adipose tissue.

7. The giant salamander oil active preparation according to claim 6, characterized in that: In step S2, the complex enzyme is composed of alkaline protease and flavor protease in a weight ratio of 2:1, and the amount of complex enzyme added is 0.8% of the weight of the pretreated adipose tissue.

8. The method for preparing the giant salamander oil active preparation according to claim 1, characterized in that: Includes the following steps: (1) Prepare raw materials containing giant salamander oil, nervonic acid, phosphatidylserine, tea polyphenol palmitate, food-grade titanium dioxide, β-cyclodextrin, sodium caseinate, functional additive A and functional additive B according to the formula; (2) After mixing the giant salamander oil, nervonic acid, phosphatidylserine, tea polyphenol palmitate and food-grade titanium dioxide in step (1), the mixture is subjected to shear emulsification to obtain a microcapsule core material solution. Functional additive A is mixed with other components in the microcapsule core material for use. (3) Mix the β-cyclodextrin and sodium caseinate from step (1) and dissolve them in deionized water to obtain a microcapsule wall material solution. The functional additive B is mixed with other components in the microcapsule wall material and then the microcapsule core material solution obtained in step (2) is added to the microcapsule wall material solution. After high-speed homogenization, the solution is spray-dried and sieved to obtain the giant salamander oil active preparation.

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