New cosmetic raw material mainly prepared from giant salamander oil and preparation process of new cosmetic raw material
Through the low-temperature process of biological enzymatic hydrolysis, centrifugal separation and molecular distillation, combined with special collagenase particles and gelatin-targeted enzymes, the problems of high-temperature damage and impurity contamination during giant salamander oil purification were solved, achieving efficient and safe extraction effects.
Patent Information
- Application Number
- CN202510859723.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-25
- Publication Date
- 2025-09-26
AI Technical Summary
The high-temperature treatment in the existing giant salamander oil purification process leads to the destruction of fatty acids and vitamins, and there is a risk of impurities and solvent residues, which affects product quality and safety.
The process of biological enzymatic hydrolysis, centrifugal separation, vacuum water washing and molecular distillation is adopted, combined with the use of special collagenase particles and bone gelatin targeted enzymes, and giant salamander oil is extracted through low-temperature treatment to avoid high-temperature degradation and impurity contamination.
The effective separation of fatty acids and vitamins in giant salamander oil was achieved, the extraction efficiency was improved, the quality and safety of the product were ensured, and high-temperature oxidation and impurity contamination were avoided.
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Figure CN120699706A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of animal fat extraction, in particular to a new cosmetic raw material mainly based on giant salamander oil and a preparation process thereof. Background Art
[0002] Wild giant salamanders require special protection. Currently, most giant salamander products on the market are derived from their offspring in captivity. The second generation of captive-bred giant salamanders and their offspring can be used for aquatic products and other resource development. Giant salamanders have extremely high economic value and are widely used in food, medicine, and health products. Their muscles contain over 70 naturally occurring active substances that can promote human metabolism and enhance immune function. Furthermore, organs such as the giant salamander's liver, mucus, skin, fat, and cartilage are also rich in a variety of bioactive substances, such as collagen, glycoproteins, bioactive peptides, metallothioneins, and bombesins.
[0003] Prior art methods for purifying giant salamander oil, a cosmetic raw material, primarily involve high-temperature steaming to extract fat from living individuals, refining or pressing to obtain crude oil, which is then decolorized and deodorized using activated carbon or clay, and finally subjected to high-temperature distillation or solvent extraction to obtain the target product. The high temperatures involved in this process can significantly damage the fat, produce trans fatty acids, and destroy vitamins. Furthermore, the risk of other impurities and solvents being introduced during the purification process is significant, making it difficult to ensure the quality and safety of the resulting giant salamander oil. Consequently, the present invention provides a new cosmetic raw material based on giant salamander oil and a preparation process thereof. Summary of the Invention
[0004] The purpose of the present invention is to provide a new cosmetic raw material based on giant salamander oil and a preparation process thereof, so as to solve the problems raised in the background technology.
[0005] To achieve the above object, the present invention provides the following technical solutions:
[0006] A process for preparing a new cosmetic raw material based on giant salamander oil comprises the following steps:
[0007] S1: obtaining raw material of giant salamander meat by slaughtering a living artificially cultivated giant salamander;
[0008] S2: Place the giant salamander meat raw material in a closed reactor, maintain at 55°C, add special collagenase granules, set the stirring speed to 80-100 rpm and process for 1-2 hours, then add protease, reduce the stirring speed to 50-80 rpm and process for 3-4 hours to obtain the enzymatic hydrolysis product;
[0009] S3: adding the enzymatic hydrolysis product to a centrifuge and subjecting it to high-speed centrifugation at 10,000-12,000 rpm to obtain crude oil;
[0010] S4: Wash the crude oil with water under vacuum at 95°C for 20-30 minutes, discard the waste water, and obtain refined crude oil;
[0011] S5: The refined crude oil is molecularly distilled at 110-140°C and 0.1-1Pa for 20-30 minutes to remove the first distillate, and then molecularly distilled at 140-170°C for 40-50 minutes to collect the second distillate, which is the new cosmetic raw material based on giant salamander oil.
[0012] Preferably, the dosage of the special collagenase granules is 0.5-1.2% of the mass of the giant salamander meat raw material, and the dosage of the protease is 0.8-1.2% of the mass of the giant salamander meat raw material.
[0013] Preferably, the method for preparing the special collagenase granules comprises the following steps:
[0014] Step 1: The main agent, auxiliary agent and stabilizer are mixed in a mass ratio of 7:2:1 to prepare a first premix;
[0015] Step 2: The first premix is put into the fluidized bed granulator, the coating liquid is sprayed at a rate of 20-25 ml / min, and the inlet air temperature is controlled at 40±2°C to obtain wet granules;
[0016] Step 3: The wet granules are passed through a 100-200 mesh vibrating sieve and then vacuum dried to a moisture content of ≤5% to obtain special collagenase granules.
[0017] Preferably, the preparation method of the main agent is: mixing the gelatin targeting enzyme and the helicase in a mass ratio of (3-4): 1 to prepare an enzyme mixture, mixing the phospholipid and the bile salt in a mass ratio of 2: 1 to prepare an auxiliary agent, mixing the enzyme mixture and the auxiliary agent in a mass ratio of 6: (2-3), and rotary evaporating the resulting product at 35°C and a vacuum degree of -0.08MPa to remove the organic solvent to prepare the main agent.
[0018] Preferably, the preparation method of the gelatin-targeted enzyme comprises the following steps:
[0019] Step 1: Crush soybean meal into 60-80 mesh, add pure water to prepare a base solution with a solid content of 3-4%, and then add collagen-inducing peptide and dipotassium hydrogen phosphate to prepare a culture medium, wherein the mass of the collagen-inducing peptide accounts for 0.8-1% of the mass of the base solution, and the mass of the dipotassium hydrogen phosphate accounts for 0.1-0.3% of the mass of the base solution;
[0020] Step 2: Sterilize the culture medium at 121-123°C for 15-20 minutes, cool it to 36-38°C, and then inoculate Bacillus licheniformis at an inoculum volume of 5% of the culture medium volume. Ferment the culture medium at 37°C with aeration for 45-48 hours at a stirring speed of 100-150 rpm and an aeration volume of 1 vvm to obtain a crude enzyme extract.
[0021] Step 3: The crude enzyme extract was filtered through a plate and frame filter to obtain a filtrate, which was passed through an activated carbon adsorption column. The flowthrough was discarded and the adsorption column was eluted through a 0.1 mol / L phosphate buffer solution, and the eluate was collected. The activated carbon adsorption column had a diameter of 20 cm and a flow rate of 0.5 L / h. The phosphate buffer solution contained 0.5% trehalose.
[0022] Step 4: The eluate was concentrated to 18-22% of the original volume through a 10 kDa ultrafiltration membrane at an operating temperature of 25° C. to obtain a gelatin-targeted enzyme solution.
[0023] Preferably, the preparation method of the collagen-inducing peptide comprises the following steps:
[0024] Step a: crushing the tail bone of a cultured giant salamander into 100-150 mesh, mixing it with food-grade diatomaceous earth with a particle size of 150-200 mesh at a mass ratio of 1:3, spraying it with a suspension containing 5% coal-based activated carbon, and drying the resulting product at 55-65° C. to a moisture content of 5% to obtain an activated aggregate;
[0025] Step b: Mixing activated aggregate and deionized water in a mass ratio of 1:(9-11), adding papain, and hydrolyzing the resulting product at 55° C. for 4-5 hours to obtain a hydrolyzed slurry, wherein the mass of papain accounts for 0.5-0.7% of the total mass of the activated aggregate and deionized water;
[0026] Step c: The hydrolyzed slurry is inactivated at 95°C for 15-20 minutes, and then cooled to 25°C to obtain a hydrolyzate. The hydrolyzate is passed through a 5000 Gauss magnetic separator to remove metal impurities to obtain a magnetic separation liquid. The magnetic separation liquid is nanofiltered using a 500-1000Da ceramic membrane to obtain a peptide concentrate.
[0027] Step d: freeze-drying the peptide concentrate to obtain collagen-inducing peptide.
[0028] Preferably, the preparation method of the adjuvant is: mixing oyster shell powder and 0.5% zinc chloride solution in a mass ratio of 1:12, and spray drying to obtain an off-white powder, which is the adjuvant, wherein the particle size of the oyster shell powder is 5-10 μm, and the spray drying is set to an inlet temperature of 155-165°C and an outlet temperature of 75-85°C.
[0029] Preferably, the preparation method of the stabilizer is: crushing konjac glucomannan, fucoidan and sea buckthorn pectin to 150-200 mesh, mixing them evenly to obtain the stabilizer, wherein the mass ratio of konjac glucomannan, fucoidan and sea buckthorn pectin powder is 5:3:2.
[0030] Preferably, the coating solution is prepared by mixing an 8% gelatin aqueous solution and tea tree essential oil in a volume ratio of 19:1, adding 0.1% Tween-80 to the total weight of the mixture, and homogenizing and emulsifying at 8000 rpm for 10-12 minutes.
[0031] Compared with the prior art, the present invention has the following beneficial effects:
[0032] 1. This preparation process extracts giant salamander oil from living organisms. Through a special production method of biological enzymatic hydrolysis, centrifugal separation, vacuum water washing, and molecular distillation, the fat, fatty acids, and their derivatives in the giant salamander oil can be fully separated and purified, thereby ensuring that the fatty acids and vitamins in the giant salamander oil are not destroyed. No other substances are added throughout the process, avoiding high-temperature degradation and oxidation in traditional purification processes and contamination by other impurities, thereby ensuring the quality and safety of the giant salamander oil product.
[0033] 2. In the present invention, enzymatic hydrolysis is performed in advance by adding special collagenase particles, the collagen-targeting enzyme is activated by a special inducing peptide, the helicase and phospholipid bile salt complex destroys the triple helix structure, and the treated oyster shell powder provides an alkaline microenvironment. The mutual synergy can address the problem of collagen in giant salamander meat forming a gel substance that affects oil separation, thereby effectively improving the extraction efficiency of giant salamander oil. BRIEF DESCRIPTION OF THE DRAWINGS
[0034] Figure 1 The present invention is a flow chart of a new cosmetic raw material mainly based on giant salamander oil and its preparation process. DETAILED DESCRIPTION
[0035] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.
[0036] Example 1:
[0037] A process for preparing a new cosmetic raw material based on giant salamander oil comprises the following steps:
[0038] S1: obtaining raw material of giant salamander meat by slaughtering a living artificially cultivated giant salamander;
[0039] S2: Place the giant salamander meat raw material in a closed reactor, maintain at 55°C, add special collagenase granules, set the stirring speed to 80 rpm and process for 1 hour, then add protease, reduce the stirring speed to 50 rpm and process for 3 hours to obtain the enzymatic hydrolysis product;
[0040] S3: adding the enzymatic hydrolysate to a centrifuge and subjecting it to high-speed centrifugation at 10,000 rpm to obtain crude oil;
[0041] S4: The crude oil is washed with water under vacuum at 95°C for 20 min, and the waste water is discarded to obtain refined crude oil;
[0042] S5: The refined crude oil is molecularly distilled at 110°C and 0.1 Pa for 20 minutes to remove the first distillate, and then molecularly distilled at 140°C for 40 minutes to collect the second distillate, which is the new cosmetic raw material based on giant salamander oil.
[0043] The dosage of the special collagenase granules is 0.5% of the mass of the giant salamander meat raw material, and the dosage of the protease is 0.8% of the mass of the giant salamander meat raw material.
[0044] The method for preparing special collagenase granules comprises the following steps:
[0045] Step 1: The main agent, auxiliary agent and stabilizer are mixed in a mass ratio of 7:2:1 to prepare a first premix;
[0046] Step 2: The first premix is put into a fluidized bed granulator, the coating liquid is sprayed at a rate of 20 ml / min, and the inlet air temperature is controlled at 38°C to obtain wet granules;
[0047] Step 3: The wet granules are passed through a 100-mesh vibrating sieve and then vacuum-dried to a moisture content of ≤5% to obtain special collagenase granules.
[0048] The preparation method of the main agent is as follows: the gelatin-targeting enzyme and the helicase are mixed in a mass ratio of 3:1 to prepare an enzyme mixture, the phospholipid and the bile salt are mixed in a mass ratio of 2:1 to prepare an auxiliary agent, the enzyme mixture and the auxiliary agent are mixed in a mass ratio of 6:2, and the obtained product is rotary evaporated at 35° C. and a vacuum degree of -0.08 MPa to remove the organic solvent to prepare the main agent.
[0049] The preparation method of the gelatin-targeted enzyme comprises the following steps:
[0050] Step 1: Grind soybean meal into 60 mesh, add pure water to prepare a base solution with a solid content of 3%, and then add collagen-inducing peptide and dipotassium hydrogen phosphate to prepare a culture medium, wherein the mass of collagen-inducing peptide accounts for 0.8% of the mass of the base solution, and the mass of dipotassium hydrogen phosphate accounts for 0.1% of the mass of the base solution;
[0051] Step 2: The culture medium was sterilized at 121°C for 15 minutes, cooled to 36°C, and inoculated with Bacillus licheniformis at an inoculum size of 5% of the culture medium volume. The culture medium was then fermented at 37°C with aeration for 45 hours at a stirring speed of 100 rpm and an aeration volume of 1 vvm to obtain a crude enzyme extract.
[0052] Step 3: The crude enzyme extract was filtered through a plate and frame filter to obtain a filtrate, which was passed through an activated carbon adsorption column. The flowthrough was discarded and the adsorption column was eluted through a 0.1 mol / L phosphate buffer solution, and the eluate was collected. The activated carbon adsorption column had a diameter of 20 cm and a flow rate of 0.5 L / h. The phosphate buffer solution contained 0.5% trehalose.
[0053] Step 4: The eluate was concentrated to 18% of the original volume through a 10 kDa ultrafiltration membrane at an operating temperature of 25° C. to obtain a gelatin-targeted enzyme solution.
[0054] The preparation method of collagen-inducing peptide comprises the following steps:
[0055] Step a: grinding the tail bone of a cultured giant salamander into 100 mesh, mixing it with food-grade diatomaceous earth with a particle size of 150 mesh at a mass ratio of 1:3, spraying it with a suspension containing 5% coal-based activated carbon, and drying the resulting product at 55° C. to a moisture content of 5% to obtain an activated aggregate;
[0056] Step b: Mixing the activated aggregate and deionized water in a mass ratio of 1:9, adding papain, and hydrolyzing the resulting product at 55° C. for 4 hours to obtain a hydrolyzed slurry, wherein the mass of the papain accounts for 0.5% of the total mass of the activated aggregate and deionized water;
[0057] Step c: The hydrolysis slurry was inactivated at 95°C for 15 minutes, and then cooled to 25°C to obtain a hydrolyzate. The hydrolyzate was passed through a 5000 Gauss magnetic separator to remove metal impurities to obtain a magnetic separation solution. The magnetic separation solution was nanofiltered using a 500Da ceramic membrane to obtain a peptide concentrate.
[0058] Step d: freeze-drying the peptide concentrate to obtain collagen-inducing peptide.
[0059] The preparation method of the adjuvant is as follows: oyster shell powder and 0.5% zinc chloride solution are mixed in a mass ratio of 1:12, and then spray-dried to obtain an off-white powder, which is the adjuvant. The particle size of the oyster shell powder is 5 μm, and the spray drying is set at an inlet temperature of 155°C and an outlet temperature of 75°C.
[0060] The preparation method of the stabilizer is as follows: konjac glucomannan, fucoidan and sea buckthorn pectin are crushed into 150 meshes, and mixed evenly to obtain the stabilizer, wherein the mass ratio of konjac glucomannan, fucoidan and sea buckthorn pectin powder is 5:3:2.
[0061] The coating solution was prepared by mixing an 8% gelatin aqueous solution and tea tree essential oil in a volume ratio of 19:1, adding 0.1% Tween-80 to the total weight of the mixture, and homogenizing and emulsifying at 8000 rpm for 10 minutes.
[0062] Example 2:
[0063] A process for preparing a new cosmetic raw material based on giant salamander oil comprises the following steps:
[0064] S1: obtaining raw material of giant salamander meat by slaughtering a living artificially cultivated giant salamander;
[0065] S2: Place the giant salamander meat raw material in a closed reactor, maintain at 55°C, add special collagenase granules, set the stirring speed to 90 rpm and process for 1.5 hours, then add protease, reduce the stirring speed to 65 rpm and process for 3.5 hours to obtain the enzymatic hydrolysis product;
[0066] S3: adding the enzymatic hydrolysis product to a centrifuge and subjecting it to high-speed centrifugation at 11,000 rpm to obtain crude oil;
[0067] S4: The crude oil is washed with water under vacuum at 95°C for 25 min, and the waste water is discarded to obtain refined crude oil;
[0068] S5: The refined crude oil is molecularly distilled at 125°C and 0.5 Pa for 25 minutes to remove the first distillate, and then molecularly distilled at 155°C for 45 minutes to collect the second distillate, which is the new cosmetic raw material based on giant salamander oil.
[0069] The dosage of the special collagenase granules is 0.8% of the mass of the giant salamander meat raw material, and the dosage of the protease is 1% of the mass of the giant salamander meat raw material.
[0070] The method for preparing special collagenase granules comprises the following steps:
[0071] Step 1: The main agent, auxiliary agent and stabilizer are mixed in a mass ratio of 7:2:1 to prepare a first premix;
[0072] Step 2: The first premix is put into a fluidized bed granulator, the coating liquid is sprayed at a rate of 23 ml / min, and the inlet air temperature is controlled at 40°C to obtain wet granules;
[0073] Step 3: The wet granules are passed through a 150-mesh vibrating sieve and then vacuum-dried to a moisture content of ≤5% to obtain special collagenase granules.
[0074] The preparation method of the main agent is as follows: the gelatin-targeting enzyme and the helicase are mixed in a mass ratio of 3.5:1 to prepare an enzyme mixture, the phospholipid and the bile salt are mixed in a mass ratio of 2:1 to prepare an auxiliary agent, the enzyme mixture and the auxiliary agent are mixed in a mass ratio of 6:2.5, and the obtained product is rotary evaporated at 35° C. and a vacuum degree of -0.08 MPa to remove the organic solvent to prepare the main agent.
[0075] The preparation method of the gelatin-targeted enzyme comprises the following steps:
[0076] Step 1: Grind soybean meal into 70 mesh, add purified water to prepare a base solution with a solid content of 3.5%, and then add collagen-inducing peptide and dipotassium hydrogen phosphate to prepare a culture medium, wherein the mass of the collagen-inducing peptide accounts for 0.9% of the mass of the base solution, and the mass of the dipotassium hydrogen phosphate accounts for 0.2% of the mass of the base solution;
[0077] Step 2: The culture medium was sterilized at 121-123°C for 18 minutes, cooled to 37°C, and inoculated with Bacillus licheniformis at an inoculum size of 5% of the culture medium volume. The culture medium was then fermented at 37°C with aeration for 46 hours at a stirring speed of 130 rpm and an aeration volume of 1 vvm to obtain a crude enzyme extract.
[0078] Step 3: The crude enzyme extract was filtered through a plate and frame filter to obtain a filtrate, which was passed through an activated carbon adsorption column. The flowthrough was discarded and the adsorption column was eluted through a 0.1 mol / L phosphate buffer solution, and the eluate was collected. The activated carbon adsorption column had a diameter of 20 cm and a flow rate of 0.5 L / h. The phosphate buffer solution contained 0.5% trehalose.
[0079] Step 4: The eluate was concentrated to 20% of the original volume through a 10 kDa ultrafiltration membrane at an operating temperature of 25° C. to obtain a gelatin-targeted enzyme solution.
[0080] The preparation method of collagen-inducing peptide comprises the following steps:
[0081] Step a: grinding the tail bone of a cultured giant salamander into 130 mesh, mixing it with food-grade diatomaceous earth with a particle size of 180 mesh at a mass ratio of 1:3, spraying it with a suspension containing 5% coal-based activated carbon, and drying the resulting product at 60° C. to a moisture content of 5% to obtain an activated aggregate;
[0082] Step b: Mixing the activated aggregate and deionized water in a mass ratio of 1:10, adding papain, and hydrolyzing the resulting product at 55° C. for 4.5 hours to obtain a hydrolyzed slurry, wherein the mass of the papain accounts for 0.6% of the total mass of the activated aggregate and deionized water;
[0083] Step c: The hydrolysis slurry was inactivated at 95°C for 18 minutes, and then cooled to 25°C to obtain a hydrolyzate. The hydrolyzate was passed through a 5000 Gauss magnetic separator to remove metal impurities to obtain a magnetic separation solution. The magnetic separation solution was nanofiltered using an 800Da ceramic membrane to obtain a peptide concentrate.
[0084] Step d: freeze-drying the peptide concentrate to obtain collagen-inducing peptide.
[0085] The preparation method of the adjuvant is as follows: oyster shell powder and 0.5% zinc chloride solution are mixed in a mass ratio of 1:12, and then spray-dried to obtain an off-white powder, which is the adjuvant. The particle size of the oyster shell powder is 8 μm, and the spray drying is set at an inlet temperature of 160°C and an outlet temperature of 80°C.
[0086] The preparation method of the stabilizer is as follows: konjac glucomannan, fucoidan and sea buckthorn pectin are crushed into 180 meshes, and mixed evenly to obtain the stabilizer, wherein the mass ratio of konjac glucomannan, fucoidan and sea buckthorn pectin powder is 5:3:2.
[0087] The coating solution was prepared by mixing an 8% gelatin aqueous solution and tea tree essential oil in a volume ratio of 19:1, adding 0.1% Tween-80 to the total weight of the mixture, and homogenizing and emulsifying at 8000 rpm for 11 minutes.
[0088] Example 3:
[0089] A process for preparing a new cosmetic raw material based on giant salamander oil comprises the following steps:
[0090] S1: obtaining raw material of giant salamander meat by slaughtering a living artificially cultivated giant salamander;
[0091] S2: Place the giant salamander meat raw material in a closed reactor, maintain at 55°C, add special collagenase granules, set the stirring speed at 100 rpm and process for 2 hours, then add protease, reduce the stirring speed to 80 rpm and process for 4 hours to obtain the enzymatic hydrolysis product;
[0092] S3: adding the enzymatic hydrolysate to a centrifuge and subjecting it to high-speed centrifugation at 12,000 rpm to obtain crude oil;
[0093] S4: The crude oil is washed with water under vacuum at 95°C for 30 min, and the waste water is discarded to obtain refined crude oil;
[0094] S5: The refined crude oil is molecularly distilled at 140°C and 1 Pa for 30 minutes to remove the first distillate, and then molecularly distilled at 170°C for 50 minutes to collect the second distillate, which is the new cosmetic raw material based on giant salamander oil.
[0095] The dosage of the special collagenase granules is 1.2% of the mass of the giant salamander meat raw material, and the dosage of the protease is 1.2% of the mass of the giant salamander meat raw material.
[0096] The method for preparing special collagenase granules comprises the following steps:
[0097] Step 1: The main agent, auxiliary agent and stabilizer are mixed in a mass ratio of 7:2:1 to prepare a first premix;
[0098] Step 2: The first premix is put into a fluidized bed granulator, the coating liquid is sprayed at a rate of 25 ml / min, and the inlet air temperature is controlled at 42°C to obtain wet granules;
[0099] Step 3: The wet granules are passed through a 200-mesh vibrating sieve and then vacuum-dried to a moisture content of ≤5% to obtain special collagenase granules.
[0100] The preparation method of the main agent is as follows: the gelatin-targeting enzyme and the helicase are mixed in a mass ratio of 4:1 to prepare an enzyme mixture, the phospholipid and the bile salt are mixed in a mass ratio of 2:1 to prepare an auxiliary agent, the enzyme mixture and the auxiliary agent are mixed in a mass ratio of 6:3, and the obtained product is rotary evaporated at 35°C and a vacuum degree of -0.08MPa to remove the organic solvent to prepare the main agent.
[0101] The preparation method of the gelatin-targeted enzyme comprises the following steps:
[0102] Step 1: Grind soybean meal into 80 mesh, add pure water to prepare a base solution with a solid content of 4%, and then add collagen-inducing peptide and dipotassium hydrogen phosphate to prepare a culture medium, wherein the mass of collagen-inducing peptide accounts for 1% of the mass of the base solution, and the mass of dipotassium hydrogen phosphate accounts for 0.3% of the mass of the base solution;
[0103] Step 2: The culture medium was sterilized at 123°C for 20 minutes, cooled to 38°C, and inoculated with Bacillus licheniformis at an inoculum size of 5% of the culture medium volume. The culture medium was then fermented at 37°C for 48 hours with a stirring speed of 150 rpm and an aeration volume of 1 vvm to obtain a crude enzyme extract.
[0104] Step 3: The crude enzyme extract was filtered through a plate and frame filter to obtain a filtrate, which was passed through an activated carbon adsorption column. The flowthrough was discarded and the adsorption column was eluted through a 0.1 mol / L phosphate buffer solution, and the eluate was collected. The activated carbon adsorption column had a diameter of 20 cm and a flow rate of 0.5 L / h. The phosphate buffer solution contained 0.5% trehalose.
[0105] Step 4: The eluate was concentrated to 22% of the original volume through a 10 kDa ultrafiltration membrane at an operating temperature of 25° C. to obtain a gelatin-targeted enzyme solution.
[0106] The preparation method of collagen-inducing peptide comprises the following steps:
[0107] Step a: grinding the tail bone of a cultured giant salamander into 150 mesh, mixing it with food-grade diatomaceous earth with a particle size of 200 mesh at a mass ratio of 1:3, spraying it with a suspension containing 5% coal-based activated carbon, and drying the resulting product at 65° C. to a moisture content of 5% to obtain an activated aggregate;
[0108] Step b: Mixing the activated aggregate and deionized water in a mass ratio of 1:11, adding papain, and hydrolyzing the resulting product at 55° C. for 5 hours to obtain a hydrolyzed slurry, wherein the mass of the papain accounts for 0.7% of the total mass of the activated aggregate and deionized water;
[0109] Step c: The hydrolysis slurry was inactivated at 95°C for 20 minutes, and then cooled to 25°C to obtain a hydrolyzate. The hydrolyzate was passed through a 5000 Gauss magnetic separator to remove metal impurities to obtain a magnetic separation solution. The magnetic separation solution was nanofiltered using a 1000Da ceramic membrane to obtain a peptide concentrate.
[0110] Step d: freeze-drying the peptide concentrate to obtain collagen-inducing peptide.
[0111] The preparation method of the adjuvant is as follows: oyster shell powder and 0.5% zinc chloride solution are mixed in a mass ratio of 1:12, and then spray-dried to obtain an off-white powder, which is the adjuvant. The particle size of the oyster shell powder is 10 μm, and the spray drying is set at an inlet temperature of 165°C and an outlet temperature of 85°C.
[0112] The preparation method of the stabilizer is as follows: konjac glucomannan, fucoidan and sea buckthorn pectin are crushed into 200 meshes, and mixed evenly to obtain the stabilizer, wherein the mass ratio of konjac glucomannan, fucoidan and sea buckthorn pectin powder is 5:3:2.
[0113] The coating solution was prepared by mixing an 8% gelatin aqueous solution and tea tree essential oil in a volume ratio of 19:1, adding 0.1% Tween-80 to the total weight of the mixture, and homogenizing and emulsifying at 8000 rpm for 12 minutes.
[0114] Comparative Example 1: The difference between this comparative example and Examples 1-3 is that this comparative example does not contain special collagenase particles.
[0115] Comparative Example 2: The difference between this comparative example and Examples 1-3 is that in this comparative example, collagenase is used instead of the dedicated collagenase particles.
[0116] Comparative Example 3: The difference between this comparative example and Examples 1-3 is that this comparative example is prepared using a conventional high-temperature process.
[0117] Performance test: The new cosmetic raw materials based on giant salamander oil prepared in Examples 1-3 and Comparative Examples 1-3 were subjected to performance tests, and the test data obtained are recorded in the following table:
[0118] Test items Trans fatty acid content (%) Vitamin A retention rate (%) Collagen residue (ppm) Example 1 Not detected 98.5 85 Example 2 Not detected 99.2 48 Example 3 Not detected 98.8 52 Comparative Example 1 0.08 97.6 1250 Comparative Example 2 0.06 98.1 680 Comparative Example 3 12.5 30.5 120
[0119] The conventional preparation process adopted in Comparative Example 3 is as follows: steaming giant salamander meat at 180°C for 4 hours, squeezing out crude oil, and then refining it by high-temperature distillation at 250°C;
[0120] In the performance test, the trans fatty acid content, vitamin A retention rate and collagen residue in the new cosmetic raw materials based on giant salamander oil prepared by the preparation processes in Examples 1-3 and Comparative Examples 1-3 were tested;
[0121] By analyzing the data in the comparison table, it can be seen that the new cosmetic raw materials based on giant salamander oil prepared in Examples 1-3 are superior to those in Comparative Examples 1-3 in all data;
[0122] This preparation process extracts giant salamander oil from living organisms. Through a special production method involving enzymatic hydrolysis, centrifugal separation, vacuum water washing, and molecular distillation, the fat, fatty acids, and their derivatives in the giant salamander oil are fully separated and purified, thereby ensuring that the fatty acids and vitamins in the giant salamander oil are not destroyed. No other substances are added throughout the process, avoiding high-temperature degradation and oxidation, as well as contamination by other impurities, in traditional purification processes, thus ensuring the quality and safety of the giant salamander oil product.
[0123] By adding special collagenase particles for pre-enzymatic hydrolysis, the collagen-targeted enzyme is activated by a special inducing peptide, the helicase and phospholipid bile salt complex destroys the triple helix structure, and the processed oyster shell powder provides an alkaline microenvironment. The mutual synergy can address the problem of collagen in giant salamander meat forming gel substances that affect oil separation, thereby effectively improving the extraction efficiency of giant salamander oil.
[0124] This shows that the fermented lactic acid bacteria camel milk powder formula provided by the present invention has a broader market prospect and is more suitable for promotion.
[0125] Throughout this specification, references to terms such as "one embodiment," "example," or "specific example" indicate that the specific features, structures, materials, or characteristics described in conjunction with that embodiment or example are included in at least one embodiment or example of the present invention. In this specification, schematic representations of these terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
[0126] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to the specific embodiments described. Obviously, many modifications and variations are possible based on the content of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.
Claims
1. A process for preparing a new raw material for cosmetics based on giant salamander oil, characterized in that: The following steps are involved: S1: obtaining raw material of giant salamander meat by slaughtering a living artificially cultivated giant salamander; S2: Place the giant salamander meat raw material in a closed reactor, maintain at 55°C, add special collagenase granules, set the stirring speed to 80-100 rpm and process for 1-2 hours, then add protease, reduce the stirring speed to 50-80 rpm and process for 3-4 hours to obtain the enzymatic hydrolysis product; S3: adding the enzymatic hydrolysis product to a centrifuge and subjecting it to high-speed centrifugation at 10,000-12,000 rpm to obtain crude oil; S4: Wash the crude oil with water under vacuum at 95°C for 20-30 minutes, discard the waste water, and obtain refined crude oil; S5: The refined crude oil is molecularly distilled at 110-140°C and 0.1-1Pa for 20-30 minutes to remove the first distillate, and then molecularly distilled at 140-170°C for 40-50 minutes to collect the second distillate, which is the new cosmetic raw material based on giant salamander oil.
2. The process for preparing the new raw material for cosmetics based on giant salamander oil according to claim 1, wherein: The dosage of the special collagenase particles is 0.5-1.2% of the mass of the giant salamander meat raw material, and the dosage of the protease is 0.8-1.2% of the mass of the giant salamander meat raw material.
3. The preparation process of the new raw material for cosmetics based on giant salamander oil according to claim 1, wherein: The method for preparing the special collagenase granules comprises the following steps: Step 1: The main agent, auxiliary agent and stabilizer are mixed in a mass ratio of 7:2:1 to prepare a first premix; Step 2: The first premix is put into the fluidized bed granulator, the coating liquid is sprayed at a rate of 20-25 ml / min, and the inlet air temperature is controlled at 40±2°C to obtain wet granules; Step 3: The wet granules are passed through a 100-200 mesh vibrating sieve and then vacuum dried to a moisture content of ≤5% to obtain special collagenase granules.
4. The process for preparing the new raw material for cosmetics based on giant salamander oil according to claim 3, wherein: The preparation method of the main agent comprises: mixing a gelatin-targeting enzyme and a helicase in a mass ratio of (3-4):1 to prepare an enzyme mixture, mixing a phospholipid and a bile salt in a mass ratio of 2:1 to prepare an auxiliary agent, mixing the enzyme mixture and the auxiliary agent in a mass ratio of 6:(2-3), and rotary evaporating the resulting product at 35°C and a vacuum degree of -0.08MPa to remove the organic solvent to prepare the main agent.
5. The process for preparing the new raw material for cosmetics based on giant salamander oil according to claim 4, wherein: The preparation method of the bone gelatin targeted enzyme comprises the following steps: Step 1: Crush soybean meal into 60-80 mesh, add pure water to prepare a base solution with a solid content of 3-4%, and then add collagen-inducing peptide and dipotassium hydrogen phosphate to prepare a culture medium, wherein the mass of the collagen-inducing peptide accounts for 0.8-1% of the mass of the base solution, and the mass of the dipotassium hydrogen phosphate accounts for 0.1-0.3% of the mass of the base solution; Step 2: Sterilize the culture medium at 121-123°C for 15-20 minutes, cool it to 36-38°C, and then inoculate Bacillus licheniformis at an inoculum volume of 5% of the culture medium volume. Ferment the culture medium at 37°C with aeration for 45-48 hours at a stirring speed of 100-150 rpm and an aeration volume of 1 vvm to obtain a crude enzyme extract. Step 3: The crude enzyme extract was filtered through a plate and frame filter to obtain a filtrate, which was passed through an activated carbon adsorption column. The flowthrough was discarded and the adsorption column was eluted through a 0.1 mol / L phosphate buffer solution, and the eluate was collected. The activated carbon adsorption column had a diameter of 20 cm and a flow rate of 0.5 L / h. The phosphate buffer solution contained 0.5% trehalose. Step 4: The eluate was concentrated to 18-22% of the original volume through a 10 kDa ultrafiltration membrane at an operating temperature of 25° C. to obtain a gelatin-targeted enzyme solution.
6. The process for preparing the new raw material for cosmetics based on giant salamander oil according to claim 5, characterized in that: The preparation method of the collagen-inducing peptide comprises the following steps: Step a: crushing the tail bone of a cultured giant salamander into 100-150 mesh, mixing it with food-grade diatomaceous earth with a particle size of 150-200 mesh at a mass ratio of 1:3, spraying it with a suspension containing 5% coal-based activated carbon, and drying the resulting product at 55-65° C. to a moisture content of 5% to obtain an activated aggregate; Step b: Mixing activated aggregate and deionized water in a mass ratio of 1:(9-11), adding papain, and hydrolyzing the resulting product at 55° C. for 4-5 hours to obtain a hydrolyzed slurry, wherein the mass of papain accounts for 0.5-0.7% of the total mass of the activated aggregate and deionized water; Step c: The hydrolyzed slurry is inactivated at 95°C for 15-20 minutes, and then cooled to 25°C to obtain a hydrolyzate. The hydrolyzate is passed through a 5000 Gauss magnetic separator to remove metal impurities to obtain a magnetic separation liquid. The magnetic separation liquid is nanofiltered using a 500-1000Da ceramic membrane to obtain a peptide concentrate. Step d: freeze-drying the peptide concentrate to obtain collagen-inducing peptide.
7. The process for preparing the new raw material for cosmetics based on giant salamander oil according to claim 3, wherein: The preparation method of the adjuvant is as follows: oyster shell powder and 0.5% zinc chloride solution are mixed in a mass ratio of 1:12, and spray-dried to obtain an off-white powder, which is the adjuvant. The particle size of the oyster shell powder is 5-10 μm, and the spray drying is set at an inlet temperature of 155-165° C. and an outlet temperature of 75-85° C.
8. The process for preparing the new raw material for cosmetics based on giant salamander oil according to claim 3, wherein: The preparation method of the stabilizer comprises the following steps: crushing konjac glucomannan, fucoidan and sea buckthorn pectin to 150-200 meshes, and uniformly mixing to obtain the stabilizer, wherein the mass ratio of konjac glucomannan, fucoidan and sea buckthorn pectin powder is 5:3:
2.
9. The process for preparing the new raw material for cosmetics based on giant salamander oil according to claim 3, wherein: The coating solution is prepared by mixing an 8% gelatin aqueous solution and tea tree essential oil in a volume ratio of 19:1, adding 0.1% Tween-80 of the total weight of the mixture, and homogenizing and emulsifying at 8000 rpm for 10-12 minutes.
10. A new cosmetic raw material based on giant salamander oil, characterized in that: The product is prepared by the preparation process of the new cosmetic raw material mainly based on giant salamander oil according to any one of claims 1 to 9.