Preparation method and application of high-stability alligator oil

Abstract

The invention provides a preparation method and application of high-stability alligator oil, and the preparation method comprises the following steps: soaking fresh alligator oil in a malic acid aqueous solution, adding a mixed strain for fermentation, adding an algin aqueous solution and a chitin aqueous solution for centrifugation, decolorizing and deodorizing by using a supercritical CO2 extraction method, adding vitamin E and hydroxytyrosol, and performing vacuum sealing to obtain the high-stability alligator oil. The alligator oil finished product is obtained. The alligator oil prepared by the method disclosed by the invention has the advantages of no peculiar smell, higher stability, high purity, better quality, simple preparation process and good application prospect.

Description

Technical Field

[0001] The present invention relates to the field of crocodile oil preparation, and specifically relates to a preparation method and application of highly stable crocodile oil. Background Art

[0002] Crocodile oil is rich in unsaturated fatty acids such as linoleic acid. These unsaturated fatty acids have good moisturizing and hydrating properties, can form a protective film on the skin surface to prevent the loss of skin moisture, and can also penetrate into the stratum corneum of the skin to improve the dry state of the skin. Crocodile oil also contains some bioactive substances such as vitamin A and squalene, which have antioxidant and cell repair promoting effects and can enhance the vitality of skin cells. Currently, there are the following problems in the preparation of crocodile oil. First, crocodile oil is rich in unsaturated fatty acids such as oleic acid and linoleic acid, and the double bonds in its molecules are easily oxidized by oxygen to generate products such as peroxides and aldehydes, resulting in oil rancidity, color change and peculiar smell. Second, insufficiently refined crocodile oil may contain moisture, protein or enzyme residues, and these impurities will promote hydrolysis reactions to generate free fatty acids or microbial growth, accelerating deterioration. Third, if crocodile oil contains medium-chain fatty acids such as lauric acid, its hydrolysis rate may be faster, and the increase in acid value leads to a decrease in stability. Crocodile oil may contain components such as phospholipids and sterols, which may react with other substances during storage, affecting homogeneity. Poor stability will cause the crocodile oil product to have a "rancid smell", which is similar to the smell of expired lard or peanut oil, affecting the quality of the product and the user experience. Summary of the Invention

[0003] Based on the existing technology, the technical problem to be solved by the present invention is to provide a preparation method and application of highly stable crocodile oil to solve the above problems.

[0004] The technical solution of the present invention:

[0005] The preparation of a highly stable crocodile oil includes the following steps:

[0006] S1. Crush fresh crocodile fat to obtain crushed crocodile fat, soak it in an aqueous solution of malic acid, steam cook it, and cool it to obtain a mixed solution;

[0007] S2. Add Leuconostoc mesenteroides, Lactobacillus rhamnosus, Lactobacillus acidophilus, Bifidobacterium longum and Bifidobacterium breve to the mixed solution for fermentation, and stir to obtain a fermentation broth;

[0008] S3. Inactivate the fermentation broth, add an aqueous solution of alginic acid and an aqueous solution of chitin to the inactivated fermentation broth for centrifugation, and use supercritical CO2 extraction to decolorize and deodorize to obtain centrifuged crocodile oil;

[0009] S4. Add vitamin E and hydroxytyrosol to the centrifuged alligator oil, stir, and seal it under vacuum to obtain the finished alligator oil product.

[0010] Further, in step S1, the crushed alligator oil grease is crushed to a diameter of 1 - 2 mm; the soaking time is 20 - 25 min.

[0011] Further, in step S1, the steam cooking temperature is 90 - 100 °C, the cooking time is 15 - 20 min; the cooling temperature is 10 - 20 °C.

[0012] Further, in step S1, the mass concentration of the malic acid aqueous solution is 7% - 10%, and the mass ratio of the crushed alligator oil grease to the malic acid aqueous solution is 1:0.5 - 0.8.

[0013] Further, in step S2, the mass ratio of Lactobacillus leichmannii, Lactobacillus rhamnosus, Lactobacillus acidophilus, Bifidobacterium longum and Bifidobacterium breve is 1.5 - 2.0:0.8 - 1.0:3.0 - 4.5:2.0 - 3.5:1.0 - 1.5.

[0014] Further, in step S2, the fermentation pH value is 5.0 - 5.5, the temperature is 25 °C - 35 °C, and the stirring time is 15 - 20 min.

[0015] Further, in step S3, the volume concentration of the alginic acid aqueous solution is 80 - 110 mg / L, and the volume concentration of the chitin aqueous solution is 120 - 140 mg / L.

[0016] Further, in step S3, the number of inactivations of the fermentation broth is 2 - 3 times, the inactivation time for each time is 10 - 15 min, and the number of centrifugations is 2 - 4 times; for the supercritical CO2 extraction method, the separation pressure is 20 - 25 MPa, and the separation temperature is 35 - 45 °C.

[0017] Further, in step S4, the addition amount of vitamin E and hydroxytyrosol is 1% - 5% of the centrifuged alligator oil, and the mass ratio of vitamin E to hydroxytyrosol is 1:0.5 - 1.

[0018] Compared with the prior art, the beneficial effects of the present invention are:

[0019] (1) In the method of the present invention, adding malic acid for cooking, adding composite microorganisms for fermentation, and then adding alginic acid aqueous solution and chitin aqueous solution for centrifugation. The combination of these steps accelerates the dissolution of unsaturated fatty acid impurities in the alligator oil, reduces the content of free fatty acids, and improves the purity of the alligator oil.

[0020] (2) Vitamin E and hydroxytyrosol are added to the crocodile oil prepared by the method of the present invention, which increases the antioxidant property of the crocodile oil, reduces the content of free fatty acids, and improves the stability of the product. Detailed implementation manners

[0021] To better understand the technical content of the present invention and describe the technical solution clearly and completely, specific embodiments are provided below to further illustrate the present invention. The following are only some embodiments of the present invention.

[0022] The materials, reagents, etc. used in the embodiments of the present invention can be obtained from commercial channels without special instructions.

[0023] In the raw material components adopted in this embodiment, Lactobacillus reuteri is purchased from Shandong Hezhong Kangyuan Biotechnology Co., Ltd., food grade, with an effective viable count of more than 50 billion CFU / g; Lactobacillus rhamnosus is purchased from Shanghai Yuanye Biotechnology Co., Ltd., food grade, with a viable count of more than 13 billion CFU / g; Lactobacillus acidophilus is purchased from... food grade, Bifidobacterium longum is purchased from Shandong Jiacheng Biotechnology Co., Ltd., food grade, product model: PG-LAS107, effective substance content: 10 billion cfu / g; Bifidobacterium breve is purchased from Tai'an Jiangzhou Biotechnology Co., Ltd., food grade, product number CB-2019673, effective ingredient content 99%, viable count 10 billion CFU / g.

[0024] Example 1

[0025] The preparation of a highly stable crocodile oil includes the following steps:

[0026] Step (1): Crush fresh crocodile oil into flakes with a diameter of 1 mm to obtain crushed crocodile oil, soak it in an aqueous solution of malic acid with a mass concentration of 7% for 20 min, where the mass ratio of crushed crocodile oil to the aqueous solution of malic acid is 1:0.5. Then, steam-cook it at 90 °C for 15 - 20 min, and after cooling to 10 °C, obtain a mixed solution;

[0027] Step (2): Add the mixed solution to Lactobacillus reuteri, Lactobacillus rhamnosus, Lactobacillus acidophilus, Bifidobacterium longum, and Bifidobacterium breve with a mass ratio of 1.5:0.8:3:2:1 for fermentation. The fermentation pH value is 5.0, the temperature is 25 °C, and stir for 15 min to obtain a fermentation broth;

[0028] Step (3): Inactivate the fermentation broth twice, with each inactivation time of 10 min. Add an aqueous solution of alginic acid with a volume concentration of 80 mg / L and an aqueous solution of chitin with a volume concentration of 120 mg / L to the inactivated fermentation broth, centrifuge twice, take the supernatant and centrifuge twice again, and separate by supercritical CO2 extraction method, with a pressure of 20 MPa and a separation temperature of 35 °C to obtain centrifuged crocodile oil;

[0029] Step (4): Add vitamin E and hydroxytyrosol to the centrifuged alligator oil. The addition amounts of vitamin E and hydroxytyrosol are 1% of the centrifuged alligator oil, and the mass ratio of vitamin E to hydroxytyrosol is 1:0.5. Stir and seal in a vacuum to obtain the finished alligator oil product.

[0030] Example 2

[0031] Step (1): Crush the fresh alligator fat into flakes with a diameter of 2 mm to obtain crushed alligator fat. Soak it in an aqueous solution of malic acid with a mass concentration of 10% for 25 min, where the mass ratio of the crushed alligator fat to the aqueous solution of malic acid is 1:0.8. Then, steam-cook it at 100 °C for 20 min. After cooling to 20 °C, obtain a mixed solution.

[0032] Step (2): Add the mixed solution to Lactobacillus leichmannii, Lactobacillus rhamnosus, Lactobacillus acidophilus, Bifidobacterium longum, and Bifidobacterium breve with a mass ratio of 2:1:4.5:3.5:1 for fermentation. The fermentation pH value is 5.5, the temperature is 35 °C, and stir for 20 min to obtain a fermentation broth.

[0033] Step (3): Inactivate the fermentation broth twice, with each inactivation time being 15 min. Add an aqueous solution of alginic acid with a volume concentration of 110 mg / L and an aqueous solution of chitin with a volume concentration of 140 mg / L to the inactivated fermentation broth. Centrifuge 4 times, take the supernatant and centrifuge 4 more times, and separate by the supercritical CO2 extraction method. The pressure is 25 MPa, and the separation temperature is 45 °C to obtain centrifuged alligator oil.

[0034] Step (4): Add vitamin E and hydroxytyrosol to the centrifuged alligator oil. The addition amounts of vitamin E and hydroxytyrosol are 5% of the centrifuged alligator oil, and the mass ratio of vitamin E to hydroxytyrosol is 1:1. Stir and seal in a vacuum to obtain the finished alligator oil product.

[0035] Example 3

[0036] Step (1): Crush the fresh alligator fat into flakes with a diameter of 1.5 mm to obtain crushed alligator fat. Soak it in an aqueous solution of malic acid with a mass concentration of 8% for 25 min, where the mass ratio of the crushed alligator fat to the aqueous solution of malic acid is 1:0.6. Then, steam-cook it at 90 °C for 20 min. After cooling to 15 °C, obtain a mixed solution.

[0037] Step (2): Add the mixed solution to Lactobacillus leichmannii, Lactobacillus rhamnosus, Lactobacillus acidophilus, Bifidobacterium longum, and Bifidobacterium breve with a mass ratio of 2:1:3:2.5:1 for fermentation. The fermentation pH value is 5.5, the temperature is 30 °C, and stir for 18 min to obtain a fermentation broth.

[0038] Step (3): Inactivate the fermentation broth twice, with each inactivation lasting for 12 minutes. After inactivation, add an aqueous solution of alginic acid with a volume concentration of 100 mg / L and an aqueous solution of chitin with a volume concentration of 130 mg / L to the fermentation broth, centrifuge three times, take the supernatant and centrifuge three more times, and then separate by supercritical CO2 extraction at a pressure of 23 MPa and a separation temperature of 40 °C to obtain centrifuged crocodile oil;

[0039] Step (4): Add vitamin E and hydroxytyrosol to the centrifuged crocodile oil. The addition amounts of vitamin E and hydroxytyrosol are 3% of the centrifuged crocodile oil, and the mass ratio of vitamin E to hydroxytyrosol is 1:0.8. Stir and seal in a vacuum to obtain the finished crocodile oil product.

[0040] Comparative Example 1

[0041] The difference between Comparative Example 1 and Example 3 is that in step (1), the step of soaking in the aqueous malic acid solution is removed, and other methods and steps are the same as those in Example 3.

[0042] Comparative Example 2

[0043] The difference between Comparative Example 2 and Example 3 is that in step (2), the fermentation step is removed, and other methods and steps are the same as those in Example 3.

[0044] Comparative Example 3

[0045] The difference between Comparative Example 3 and Example 3 is that in step (3), the addition of the aqueous alginic acid solution and the aqueous chitin solution to the fermentation broth is removed, and other methods and steps are the same as those in Example 3.

[0046] Comparative Example 4

[0047] The difference between Comparative Example 4 and Example 3 is that in step (4), vitamin E and hydroxytyrosol are not added, and other methods and steps are the same as those in Example 3.

[0048] Control:

[0049] Commercially available crocodile oil, produced by Shanxi Lanyuan Biotechnology Co., Ltd., with an active substance content of 99%.

[0050] Properties:

[0051] The appearance and properties of the product of the present invention: at room temperature of 10 - 25 °C, it is a light orange oily liquid, without precipitation, impurities, or peculiar smell, is easily soluble in organic solvents such as acetone, ether, petroleum ether, and n-hexane, is insoluble in water, and no solid fat precipitates. Among the fatty acids of crocodile oil prepared in Examples 1 - 3 of this method, palmitic acid accounts for 16.5%, palmitoleic acid accounts for 5.9%, and stearic acid accounts for 4.1%. See Table 1 for details.

[0052] Table 1 Crocodile oil property table

[0053]

[0054]

[0055] Experiment:

[0056] Select the crocodile oil prepared in Examples 1-3, the crocodile oil prepared by the methods of Comparative Examples 1-4, and the commercially available control crocodile oil. The acid value was determined by the cold solvent indicator titration method in GB 5009.229-2016 "Determination of Acid Value in Foods"; the peroxide value was determined by the titration method in GB 5009.227-2016 "Determination of Peroxide Value in Foods" (stored for 15 days at a temperature of 40 °C). The lead, arsenic, and mercury contents were determined, and the methods in "GB 5009.12-2017 National Food Safety Standard Determination of Lead in Foods", "GB 5009.11-2024 National Food Safety Standard Determination of Total Arsenic and Inorganic Arsenic in Foods", and "GB 5009.17-2021 Determination of Total Mercury and Organic Mercury in Foods" were referred to for the determination, and the determination results are shown in Table 2.

[0057] Table 2 Statistical Table of Detection Indicators

[0058]

[0059] The peroxide value (POV) can reflect the oxidation degree of crocodile oil and is an important indicator for evaluating the quality of crocodile oil. At high temperatures, the oxidation of crocodile oil produces primary oxides such as hydroperoxides, which will further oxidize over time, and the crocodile oil lipid chain breaks to form secondary oxidation products such as short-chain aldehydes, ketones, acids, and short-chain hydrocarbons, resulting in an increase in POV. The acid value (AV), a measurement standard for free carboxylic acid groups in an oil, is closely related to the amount of free fatty acids contained. The higher the AV value, the higher the oxidation degree of the crocodile oil. The test results show that the oil yield of the crocodile oil prepared by the method of the present invention is between 85.3% and 87.0%, the peroxide value and acid value are reduced, and the lead, arsenic, and mercury contents are not detected in the crocodile oil prepared by the method of the present invention.

[0060] The test results show that the oil yield of the crocodile oil prepared according to Examples 1-3 can reach 85.3%-87%, without precipitation, impurities, and peculiar smell, no solid fat is separated out, and it does not contain heavy metals such as lead, arsenic, and mercury. It has a high oil yield and reliable and safe quality. Comparative Examples 1-4 changed the raw material components, including removing the step of soaking in malic acid aqueous solution, removing the fermentation step, removing the addition of alginic acid aqueous solution and chitin aqueous solution to the fermentation broth, and not adding vitamin E and hydroxytyrosol, and none of them achieved the technical effect of improving the stability of crocodile oil in the present invention, indicating that the combination of the raw materials and steps of the method of the present invention has a good application effect of improving the stability of crocodile oil.

[0061] The above are only exemplary embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A preparation method of highly stable crocodile oil, characterized in that, It includes the following steps: S1. Crush fresh crocodile fat to obtain crushed crocodile fat, soak it in an aqueous malic acid solution, steam it, and cool it to obtain a mixed solution; S2. Add Lactobacillus leichmannii, Lactobacillus rhamnosus, Lactobacillus acidophilus, Bifidobacterium longum, and Bifidobacterium breve to the mixed solution for fermentation, and stir to obtain a fermentation broth; S3. Inactivate the fermentation broth, add an aqueous alginic acid solution and an aqueous chitin solution to the inactivated fermentation broth for centrifugation, and use the supercritical CO2 extraction method to decolorize and deodorize to obtain centrifuged crocodile oil; S4. Add vitamin E and hydroxytyrosol to the centrifuged crocodile oil, stir, and seal it under vacuum to obtain the finished crocodile oil.

2. The preparation method of a highly stable crocodile oil according to claim 1, characterized in that In step S1, the crushed crocodile fat is crushed to a diameter of 1-2 mm; the soaking time is 20-25 min.

3. The preparation method of a highly stable crocodile oil according to claim 1, wherein, In step S1, the steam cooking temperature is 90°C - 100°C, and the cooking time is 15-20 min; the cooling temperature is 10°C - 20°C.

4. The preparation method of a highly stable crocodile oil as described in claim 1, characterized in that, In step S1, the mass concentration of the aqueous malic acid solution is 7% - 10%, and the mass ratio of the crushed crocodile fat to the aqueous malic acid solution is 1:0.5 - 0.

8.

5. The preparation method of a highly stable crocodile oil as described in claim 1, characterized in that, In step S2, the mass ratio of Lactobacillus leichmannii, Lactobacillus rhamnosus, Lactobacillus acidophilus, Bifidobacterium longum, and Bifidobacterium breve is 1.5 - 2.0:0.8 - 1.0:3.0 - 4.5:2.0 - 3.5:1.0 - 1.

5.

6. The preparation method of a highly stable crocodile oil as described in claim 1, characterized in that, In step S2, the fermentation pH value is 5.0 - 5.5, the temperature is 25°C - 35°C, and the stirring time is 15 - 20 min.

7. The preparation method of a highly stable crocodile oil according to claim 1, characterized in that, In step S3, the volume concentration of the aqueous alginic acid solution is 80 - 110 mg / L, and the volume concentration of the aqueous chitin solution is 120 - 140 mg / L.

8. The preparation method of a highly stable crocodile oil as described in claim 1, characterized in that, In step S3, the number of times of inactivating the fermentation broth is 2 - 3 times, the inactivating time for each time is 10 - 15 min, and the number of centrifugation times is 2 - 4 times; for the supercritical CO2 extraction method, the separation pressure is 20 - 25 MPa, and the separation temperature is 35 - 45°C.

9. The preparation method of a highly stable crocodile oil as described in claim 1, characterized in that, In step S4, the addition amount of vitamin E and hydroxytyrosol is 1% - 5% of the centrifuged crocodile oil, and the mass ratio of vitamin E to hydroxytyrosol is 1:0.5 - 1.

10. Use of the crocodile oil according to any one of claims 1-9 in the field of preparing drugs or cosmetics.

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