CN112426381A - Marine biological active cosmetic - Google Patents
Marine biological active cosmetic Download PDFInfo
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- CN112426381A CN112426381A CN202110057008.1A CN202110057008A CN112426381A CN 112426381 A CN112426381 A CN 112426381A CN 202110057008 A CN202110057008 A CN 202110057008A CN 112426381 A CN112426381 A CN 112426381A
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- enzymolysis
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9706—Algae
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
Abstract
The invention relates to a marine biological activity cosmetic which is characterized by containing seaweed liquid, wherein the seaweed liquid is prepared according to the following steps: adding seaweed into water, and carrying out acidolysis and enzymolysis to obtain seaweed liquid, wherein the pH value of the acidolysis is 2-3; the enzyme is saccharifying enzyme and cellulase. The seaweed liquid extracted by the method has good water solubility and high water-soluble solid content. The method can be used for extracting the fresh seaweed, so that the green seaweed liquid with high solid content can be prepared, and the method has good effects of moistening and moisturizing and delaying senescence.
Description
Technical Field
The invention relates to a marine biological activity cosmetic.
Background
Since marine organisms live in severe environments with high humidity, high salt content and high cold, the marine organisms need to have strong repairing and water-retaining functions in order to adapt to the environment, so that the marine organisms have a good prospect in cosmetics. The seaweed has the advantages of low cost and easy obtainment, so the seaweed is widely applied to cosmetics, but the extraction method directly influences the use effect of the cosmetics.
At present, the method for chemically extracting the seaweed liquid is divided into an alkaline hydrolysis extraction mode, an acidolysis extraction mode or a combination extraction mode of the alkaline hydrolysis extraction mode and the acidolysis extraction mode, the prepared extracting solution is dark brown or black, the color is deepened along with the extension of the extraction time, the fragrance is emitted, and finally the solid content of water-soluble products in the extracting solution is low, so that part of effective substances are lost. The direct extraction of acid at low temperature can reduce the damage to effective components, but the seaweed gel is generated, the product fluidity is poor, the subsequent operation is not facilitated, the inconvenience is brought to producers and users, and the problem of low water-soluble solid content exists. In order to prevent the product from deteriorating in fluidity after acidolysis and facilitate production and use, alkali extraction is generally adopted first, and then acid extraction is adopted, however, due to the damage of the alkali extraction on the effective components of the seaweed, the prepared product is black even if acid extraction is adopted in the later period, and the water-soluble solid content is also low. For example, patent No. CN 1269339a discloses a technical scheme of alkaline hydrolysis followed by acid hydrolysis.
Although the damage to the effective substances of the seaweed can be reduced by adopting the enzyme extraction, the problems of incomplete extraction and low water-soluble solid content in the extract exist by adopting the enzyme extraction because the enzyme has specificity and different enzyme activity conditions are different.
At present, no method exists for extracting by acid, which does not destroy the effective components of seaweed, can enable the product to have good fluidity, can further improve the solid content of the extracting solution, and can ensure the stable quality of the finally prepared product.
Disclosure of Invention
The invention provides a marine biological activity cosmetic, which solves the technical problems that 1) the cosmetic has better effects of moistening and moisturizing and delaying senility; 2) the damage to the effective ingredients of the seaweed is reduced, so that the product has good fluidity; 3) further improving the water-soluble solid content in the seaweed extract and stabilizing the quality of the extracted seaweed liquid.
In order to solve the technical problems, the invention adopts the following technical scheme:
a marine bioactive cosmetic comprises seaweed liquid, which is prepared by the following steps:
1) acid hydrolysis: adding seaweed into water, and extracting under the condition that the pH value is 2-3 to obtain acidolysis solution;
2) enzymolysis: adjusting the pH value of the acidolysis solution to 4.2-6.5, adding enzyme, and carrying out enzymolysis to obtain an enzymolysis solution;
3) seaweed solution: the enzymolysis liquid obtained in the step 2) is seaweed liquid, or
Filtering the enzymolysis liquid to obtain filtrate, namely the seaweed liquid;
the enzyme is saccharifying enzyme and cellulase;
the mass ratio of the seaweed to the water in the step 1) is 1-2: 3-6;
the extraction conditions of step 1) are 5-30 ℃, the stirring speed is 65-100 r/min, and the time is 20-40 min;
the mass ratio of the seaweed to the enzyme is 10000: 0.1-5; the enzymolysis temperature is 26-62 ℃, and the enzymolysis time is 6-72 h.
The enzymolysis is divided into saccharification enzymolysis and cellulase enzymolysis; the saccharification enzymolysis and the cellulase enzymolysis are not carried out simultaneously;
the enzymolysis temperature of the saccharification enzymatic hydrolysis is 55-62 ℃, and the enzymolysis time is 6-24 h; enzyme deactivation is carried out after enzymolysis, wherein the enzyme deactivation temperature is 90-120 ℃, and the enzyme deactivation time is 2-5 min;
the enzymolysis temperature of the cellulase enzymolysis is 26-35 ℃, and the enzymolysis time is 6-48 h; and enzyme deactivation is carried out after enzymolysis, wherein the enzyme deactivation temperature is 90-120 ℃, and the enzyme deactivation time is 2-5 min.
The saccharification enzymatic hydrolysis is carried out according to the following steps:
and adjusting the pH value of the acidolysis solution to 4.0-4.5, adding saccharifying enzyme, and carrying out enzymolysis to obtain a saccharifying enzymolysis seaweed solution.
The cellulase enzymolysis is carried out according to the following steps:
and adjusting the pH value of the acidolysis solution to 5.5-6.5, adding cellulase, and carrying out enzymolysis to obtain cellulase-hydrolyzed seaweed solution.
The cellulase enzymolysis is carried out according to the following steps:
adjusting the pH value of the saccharification and enzymolysis seaweed liquid to 5.5-6.5, adding cellulase, and carrying out enzymolysis to obtain cellulase-hydrolyzed seaweed liquid, namely the seaweed liquid; or
Filtering the cellulose hydrolysate to obtain seaweed liquid.
The saccharification enzymatic hydrolysis is carried out according to the following steps:
adjusting the pH value of the cellulase enzymolysis liquid to 4.0-4.5, adding saccharifying enzyme for enzymolysis to obtain a saccharifying enzymolysis seaweed liquid, namely the seaweed liquid; or
Filtering the saccharified enzymatic hydrolysate to obtain the seaweed liquid.
The enzymolysis of the cellulase also comprises introducing nitrogen before the enzymolysis until the oxygen content in the saccharified enzymolysis liquid or the acidolysis liquid is lower than 0.2 mg/L;
the saccharification enzymatic hydrolysis also comprises introducing nitrogen before the enzymatic hydrolysis until the oxygen content in the saccharification enzymatic hydrolysis liquid or the acidolysis liquid is lower than 0.2 mg/L.
The invention has the following beneficial technical effects:
1. this application reduces the destruction of acid to the interior material of marine alga through low temperature acidolysis, simultaneously, through earlier stage acid treatment, obtains the acidolysis liquid, through later stage enzyme extraction, both can reduce the destruction to the marine alga composition, can make the extract have better mobility again, can also further improve water-soluble solid content in the marine alga extract.
2. According to the method, the seaweed is subjected to enzymolysis by adopting saccharifying enzyme and cellulase, and the enzymolysis is performed step by step, so that the water-soluble solid content in the seaweed liquid can be improved, wherein the saccharifying enzyme is used for hydrolyzing alpha-1, 4-and alpha-1, 6-glycosidic bonds, the cellulase is used for hydrolyzing 1, 4-beta glycosidic bonds, and the extraction rate of the seaweed polysaccharide can be improved under the combined action of the saccharifying enzyme and the cellulase.
3. This application can effectively prevent extract colour change, makes product quality more stable.
4. The moisturizing and anti-aging cream has good moisturizing and anti-aging effects.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
The marine biological activity skin cream comprises 7% of isopropyl palmitate, 4% of cetyl alcohol, 25% of seaweed liquid, 3% of propylene glycol, 0.2% of imidazolidinyl urea, 1.2% of triethanolamine and the balance of water, wherein the seaweed liquid is prepared according to the following steps:
1) acid hydrolysis: adding seaweed into water, and extracting under the condition that the pH value is 2.2 to obtain acidolysis solution;
2) enzymolysis: adjusting the pH value of the acidolysis solution to 6.0, adding enzyme, and carrying out enzymolysis to obtain an enzymolysis solution;
3) seaweed solution: inactivating enzyme of the enzymolysis solution at 95 deg.C for 3min, and filtering to obtain filtrate, i.e. Sargassum solution.
The enzyme is a mixture of saccharifying enzyme and cellulase according to the mass ratio of 1: 1; the seaweed is fresh Sargassum, and has water content of 80%.
The mass ratio of the seaweed and the water in the step 1) is 1: 3.
The extraction conditions of the step 1) are that the temperature is 15 ℃, the rotating speed is 65r/min, and the time is 30 min.
The mass ratio of the added enzyme to the kelp in the step 2) is 0.4:10000, wherein the activity of saccharifying enzyme is 50000U/g, the activity of cellulase is 100000U/g, the enzymolysis condition is that the enzymolysis temperature is 30 ℃, and the enzymolysis time is 24 hours.
And 3) filtering, wherein the mesh diameter of the filter screen is 400 meshes.
The steps relate to the seaweed mass ratio on a dry basis.
Example 2
The marine biological activity shampoo is composed of 15% of lauryl alcohol ether sulfate sodium salt, 4% of lauryl alcohol sulfate sodium salt, 6% of cocamidopropyl betaine, 10% of seaweed liquid, 3% of ethylene glycol stearate, 0.2% of methylisothiazolinone, 100.3% of polyquaternary ammonium salt, 1.2% of triethanolamine and the balance of water, wherein the seaweed liquid is prepared according to the following steps:
1) acid hydrolysis: adding seaweed into water, and extracting under the condition that the pH value is 2.2 to obtain acidolysis solution;
2) enzymolysis: adjusting the pH value of the acidolysis solution to 4.2, adding enzyme, and carrying out enzymolysis to obtain an enzymolysis solution;
3) seaweed solution: inactivating enzyme of the enzymolysis solution at 95 deg.C for 3min, and filtering to obtain filtrate, i.e. Sargassum solution.
The enzyme is a mixture of saccharifying enzyme and cellulase according to the mass ratio of 1: 1; the seaweed is fresh Sargassum, and has water content of 80%.
The mass ratio of the seaweed and the water in the step 1) is 1: 3.
The extraction conditions of the step 1) are that the temperature is 15 ℃, the rotating speed is 65r/min, and the time is 30 min.
The mass ratio of the added enzyme to the kelp in the step 2) is 0.4:10000, wherein the activity of saccharifying enzyme is 50000U/g, the activity of cellulase is 100000U/g, the enzymolysis condition is that the enzymolysis temperature is 60 ℃, and the enzymolysis time is 24 hours.
And 3) filtering, wherein the mesh diameter of the filter screen is 400 meshes.
The steps relate to the seaweed mass ratio on a dry basis.
Example 3
The skin cream with marine biological activity consists of 8% of isopropyl palmitate, 5% of cetyl alcohol, 3% of seaweed liquid, 4% of propylene glycol, 0.2% of imidazolidinyl urea, 1.1% of triethanolamine and the balance of water, wherein the seaweed liquid is prepared according to the following steps:
1) acid hydrolysis: adding seaweed into water, and extracting under the condition that the pH value is 2.2 to obtain acidolysis solution;
2) enzymolysis: adjusting pH of the acidolysis solution to 4.2, adding diastase, performing enzymolysis, and inactivating enzyme to obtain saccharified and enzymolyzed seaweed solution;
adjusting the pH value of the saccharification and enzymolysis seaweed solution to 6.0, adding cellulase for enzymolysis to obtain cellulase enzymolysis seaweed solution;
3) seaweed solution: inactivating enzyme of the cellulose enzymolysis Sargassum liquid at 95 deg.C for 3min, and filtering to obtain filtrate.
The mass ratio of the seaweed to the water in the step 1) is 1: 3; the seaweed is fresh Sargassum, and has water content of 80%.
The mass ratio of the seaweed and the water in the step 1) is 1: 3.
The extraction conditions of the step 1) are that the temperature is 15 ℃, the rotating speed is 65r/min, and the time is 30 min.
In the step 2), the mass ratio of the adding amount of the saccharifying enzyme to the kelp is 0.2:10000, the mass ratio of the adding amount of the cellulase to the kelp is 0.2:10000, wherein the activity of the saccharifying enzyme is 50000U/g, the activity of the cellulase is 100000U/g,
in the step 2), the enzymatic hydrolysis conditions of the saccharification enzyme are that the enzymatic hydrolysis temperature is 60 ℃ and the enzymatic hydrolysis time is 12 hours;
the enzymolysis condition of the cellulase is that the enzymolysis temperature is 30 ℃, and the enzymolysis time is 12 h.
And 3) filtering, wherein the mesh diameter of the filter screen is 400 meshes.
The steps relate to the seaweed mass ratio on a dry basis.
Example 4
The eye cream comprises 5% of cetyl alcohol, 6% of isopropyl palmitate, 5% of octadecanol, 0.4% of carbomer, 20% of seaweed liquid, 10% of butanediol, 0.2% of imidazolidinyl urea and the balance of water, wherein the seaweed liquid is prepared according to the following steps:
1) acid hydrolysis: adding seaweed into water, and extracting under the condition that the pH value is 2.2 to obtain acidolysis solution;
2) enzymolysis: adjusting pH of the acidolysis solution to 6.0, adding cellulase for enzymolysis, and inactivating enzyme to obtain cellulase-hydrolyzed seaweed solution;
adjusting the pH value of the cellulase-hydrolyzed seaweed solution to 4.2, adding saccharifying enzyme, and performing enzymolysis to obtain saccharified and enzymolyzed seaweed solution;
3) seaweed solution: inactivating enzyme of saccharified and enzymolyzed Sargassum liquid at 95 deg.C for 3min, and filtering to obtain filtrate.
The mass ratio of the seaweed to the water in the step 1) is 1: 3; the seaweed is fresh Sargassum, and has water content of 80%.
The mass ratio of the seaweed and the water in the step 1) is 1: 3.
The extraction conditions of the step 1) are that the temperature is 15 ℃, the rotating speed is 65r/min, and the time is 30 min.
In the step 2), the mass ratio of the adding amount of the saccharifying enzyme to the kelp is 0.2:10000, the mass ratio of the adding amount of the cellulase to the kelp is 0.2:10000, wherein the activity of the saccharifying enzyme is 50000U/g, the activity of the cellulase is 100000U/g,
in the step 2), the enzymatic hydrolysis conditions of the saccharification enzyme are that the enzymatic hydrolysis temperature is 60 ℃ and the enzymatic hydrolysis time is 12 hours;
the enzymolysis condition of the cellulase is that the enzymolysis temperature is 30 ℃, and the enzymolysis time is 12 h.
And 3) filtering, wherein the mesh diameter of the filter screen is 400 meshes.
The steps relate to the seaweed mass ratio on a dry basis.
Example 5
The marine biological active skin moisturizer is characterized by consisting of 9% of isopropyl palmitate, 3% of cetyl alcohol, 30% of seaweed liquid, 4% of propylene glycol, 0.2% of imidazolidinyl urea, 1.1% of triethanolamine and the balance of water, wherein the seaweed liquid is prepared according to the following steps:
the seaweed solution is prepared according to the following steps:
1) acid hydrolysis: adding seaweed into water, and extracting under the condition that the pH value is 2.2 to obtain acidolysis solution;
2) enzymolysis: adjusting the pH value of the acidolysis solution to 4.2, charging nitrogen until the oxygen content in the acidolysis solution is 0.1mg/L, adding saccharifying enzyme, carrying out enzymolysis under the protection of nitrogen, and inactivating enzyme to obtain saccharified and enzymolyzed seaweed liquid;
adjusting the pH value of the saccharification and enzymolysis seaweed solution to 6.0, adding cellulase, and carrying out enzymolysis under the protection of nitrogen to obtain cellulase enzymolysis seaweed solution;
3) seaweed solution: inactivating enzyme of the cellulose enzymolysis Sargassum liquid at 95 deg.C for 3min, and filtering to obtain filtrate.
The mass ratio of the seaweed to the water in the step 1) is 1: 3; the seaweed is fresh Sargassum, and has water content of 80%.
The mass ratio of the seaweed and the water in the step 1) is 1: 3.
The extraction conditions of the step 1) are that the temperature is 15 ℃, the rotating speed is 65r/min, and the time is 30 min.
In the step 2), the mass ratio of the adding amount of the saccharifying enzyme to the kelp is 0.2:10000, the mass ratio of the adding amount of the cellulase to the kelp is 0.2:10000, wherein the activity of the saccharifying enzyme is 50000U/g, the activity of the cellulase is 100000U/g,
in the step 2), the enzymatic hydrolysis conditions of the saccharification enzyme are that the enzymatic hydrolysis temperature is 60 ℃ and the enzymatic hydrolysis time is 12 hours;
the enzymolysis condition of the cellulase is that the enzymolysis temperature is 30 ℃, and the enzymolysis time is 12 h.
And 3) filtering, wherein the mesh diameter of the filter screen is 400 meshes.
The steps relate to the seaweed mass ratio on a dry basis.
Example 6
The marine biological activity facial cleanser consists of 12% of lauryl alcohol ether sulfate sodium salt, 2% of bamboo salt, 3% of lauryl alcohol sulfate sodium salt, 5% of cocamidopropyl betaine, 15% of seaweed liquid, 3% of ethylene glycol stearate, 0.2% of methylisothiazolinone, 100.3% of polyquaternary ammonium salt, 1.2% of triethanolamine and the balance of water, wherein the seaweed liquid is prepared according to the following steps:
1) acid hydrolysis: adding seaweed into water, and extracting under the condition that the pH value is 2.2 to obtain acidolysis solution;
2) enzymolysis: adjusting the pH value of the acidolysis solution to 6.0, charging nitrogen until the oxygen content in the acidolysis solution is 0.1mg/L, adding cellulase, performing enzymolysis under the protection of nitrogen, and inactivating enzyme to obtain cellulase-hydrolyzed seaweed solution;
adjusting the pH value of the cellulase-hydrolyzed seaweed solution to 4.2, adding saccharifying enzyme, and carrying out enzymolysis under the protection of nitrogen to obtain a saccharified and enzymolyzed seaweed solution;
3) seaweed solution: inactivating enzyme of saccharified and enzymolyzed Sargassum liquid at 95 deg.C for 3min, and filtering to obtain filtrate.
The mass ratio of the seaweed to the water in the step 1) is 1: 3; the seaweed is fresh Sargassum, and has water content of 80%.
The mass ratio of the seaweed and the water in the step 1) is 1: 3.
The extraction conditions of the step 1) are that the temperature is 15 ℃, the rotating speed is 65r/min, and the time is 30 min.
In the step 2), the mass ratio of the adding amount of the saccharifying enzyme to the kelp is 0.2:10000, the mass ratio of the adding amount of the cellulase to the kelp is 0.2:10000, wherein the activity of the saccharifying enzyme is 50000U/g, the activity of the cellulase is 100000U/g,
in the step 2), the enzymatic hydrolysis conditions of the saccharification enzyme are that the enzymatic hydrolysis temperature is 60 ℃ and the enzymatic hydrolysis time is 12 hours;
the enzymolysis condition of the cellulase is that the enzymolysis temperature is 30 ℃, and the enzymolysis time is 12 h.
And 3) filtering, wherein the mesh diameter of the filter screen is 400 meshes.
The steps relate to the seaweed mass ratio on a dry basis.
Example 7
The marine bioactive cosmetic consists of 17 percent of lauryl alcohol ether sulfate sodium salt, 6 percent of lauryl alcohol sulfate sodium salt, 5 percent of cocamidopropyl betaine, 12 percent of seaweed liquid, 4 percent of ethylene glycol stearate, 0.2 percent of methylisothiazolinone, 100.3 percent of polyquaternary ammonium salt, 1.2 percent of triethanolamine and the balance of water, wherein the seaweed liquid is prepared according to the following steps:
1) acid hydrolysis: adding seaweed into water, and extracting under the condition that the pH value is 2.5 to obtain acidolysis solution;
2) enzymolysis: adjusting pH of the acidolysis solution to 5.8, adding cellulase for enzymolysis, and inactivating enzyme to obtain cellulase-hydrolyzed seaweed solution;
adjusting the pH value of the cellulase-hydrolyzed seaweed solution to 4.4, charging nitrogen until the oxygen content in the acidolysis solution is 0.05mg/L, adding saccharifying enzyme, and performing enzymolysis to obtain saccharified and enzymolyzed seaweed solution;
3) seaweed solution: inactivating enzyme of saccharified and enzymolyzed Sargassum liquid at 100 deg.C for 2min to obtain Sargassum liquid.
The mass ratio of the seaweed to the water in the step 1) is 1: 4; the seaweed is thallus laminariae.
The extraction conditions of the step 1) are that the temperature is 10 ℃, the rotating speed is 80r/min, and the time is 35 min.
In the step 2), the mass ratio of the adding amount of the saccharifying enzyme to the kelp is 0.1:10000, the mass ratio of the adding amount of the cellulase to the kelp is 0.3:10000, wherein the activity of the saccharifying enzyme is 100000U/g, the activity of the cellulase is 50000U/g,
in the step 2), the enzymatic hydrolysis conditions of the saccharification enzyme are that the enzymatic hydrolysis temperature is 56 ℃ and the enzymatic hydrolysis time is 8 hours;
the enzymolysis condition of the cellulase is that the enzymolysis temperature is 28 ℃, and the enzymolysis time is 24 hours.
Example 8
The marine bioactive cosmetic consists of 16 percent of lauryl alcohol ether sulfate sodium salt, 4 percent of lauryl alcohol sulfate sodium salt, 6 percent of cocamidopropyl betaine, 35 percent of seaweed liquid, 3 percent of ethylene glycol stearate, 0.2 percent of methylisothiazolinone, 100.3 percent of polyquaternary ammonium salt, 1.2 percent of triethanolamine and the balance of water, wherein the seaweed liquid is prepared according to the following steps:
1) acid hydrolysis: adding seaweed into water, and extracting under the condition that the pH value is 2.8 to obtain acidolysis solution;
2) enzymolysis: adjusting the pH value of the acidolysis solution to 4.5, charging nitrogen until the oxygen content in the acidolysis solution is 0.1mg/L, adding saccharifying enzyme, carrying out enzymolysis under the protection of nitrogen, and inactivating enzyme to obtain saccharified and enzymolyzed seaweed liquid;
adjusting the pH value of the saccharification and enzymolysis seaweed solution to 6.2, adding cellulase for enzymolysis to obtain cellulase enzymolysis seaweed solution;
3) seaweed solution: inactivating enzyme of the cellulose enzymolysis Sargassum liquid at 100 deg.C for 2min, and filtering to obtain filtrate.
Step 1), the mass ratio of the seaweed to the water is 1: 2; the seaweed is laver.
The extraction conditions of the step 1) are that the temperature is 25 ℃, the rotating speed is 65r/min, and the time is 20 min.
In the step 2), the mass ratio of the adding amount of the saccharifying enzyme to the kelp is 0.5:10000, the mass ratio of the adding amount of the cellulase to the kelp is 0.6:10000, wherein the activity of the saccharifying enzyme is 50000U/g, the activity of the cellulase is 50000U/g,
in the step 2), the enzymatic hydrolysis conditions of the saccharification enzyme are that the enzymatic hydrolysis temperature is 56 ℃ and the enzymatic hydrolysis time is 24 hours;
the enzymolysis condition of the cellulase is that the enzymolysis temperature is 32 ℃, and the enzymolysis time is 24 hours.
The beneficial effects of the present invention are further illustrated below in conjunction with experimental data:
test material
1.1 test site: the detection was made by Sanfeng (tobacco pipe) agriculture science and technology Co.
1.2 test detection: the seaweed solution contains water-soluble solid content, initial cytokinin content (the general names of isopentene adenine, zeatin, isopentene adenosine, trans-zeatin and gibberellin), final cytokinin content (the general names of isopentene adenine, zeatin, isopentene adenosine, trans-zeatin and gibberellin), initial seaweed polysaccharide content and final seaweed polysaccharide content, and the initial color and the final color are recorded, wherein the initial color is the color just produced, and the initial seaweed polysaccharide content is just produced; the content of inceptocytokinins (a general term for isopentenyladenine, zeatin, isopentenyladenosine, trans-zeatin and gibberellin) is as-produced; the final color is the color after being placed indoors in a 1L polyethylene bottle for 6 months, and the final cytokinin content (the general name of isopentene adenine, zeatin, isopentene adenosine, trans-zeatin and gibberellin) is the cytokinin content (the general name of isopentene adenine, zeatin, isopentene adenosine, trans-zeatin and gibberellin) after being placed indoors in a 1L polyethylene bottle for 6 months; the final algal polysaccharide content is the algal polysaccharide content after being placed indoors for 6 months in a 1L polyethylene bottle.
1.3 test materials: the preparation methods of the seaweed liquid prepared in the comparative example 1 (except that the seaweed liquid is not subjected to acid hydrolysis in the preparation process, the preparation methods are all the same as those in the example 3), the seaweed liquid prepared in the comparative example 2 (except that the enzyme used in the enzymolysis in the preparation process of the seaweed liquid only adopts cellulase, the preparation methods are all the same as those in the example 1), the seaweed liquid prepared in the comparative example 3 (except that the enzyme used in the enzymolysis in the preparation process of the seaweed liquid only adopts saccharifying enzyme, the preparation methods are all the same as those in the example 2), and the seaweed liquids prepared in the examples 1 to 6.
1.4 Experimental implementation: the solid content is determined according to the coating solid content determination method GB1725-79, the seaweed polysaccharide is detected by a sulfuric acid-phenol method, the cytokinin is detected by a liquid chromatography-mass spectrometry combined method, and the color change is observed by naked eyes.
The present application is consistent in other implementations except for differences in the respective processes.
1.5 Experimental phenomena: wherein the blank (acidolysis solution prepared in example 2) was seaweed gel, losing fluidity; the fluidity is restored after the enzyme treatment, and the fluidity is increased with the increase of the water-soluble solid content.
2 results and analysis
Water-soluble solid content, cytokinin content (a total name of isopentenyladenine, zeatin, isopentenyladenosine, trans-zeatin and gibberellin), final cytokinin content (a total name of isopentenyladenine, zeatin, isopentenyladenosine, trans-zeatin and gibberellin), algal polysaccharide content and algal polysaccharide content, and initial color and final color are shown in Table 1
TABLE 1
Note: the blank (acidolysis solution prepared in example 2) was prepared as alginate gel, which was not water-soluble, too viscous to filter and therefore not tested for solid content.
As can be seen from the comparison of the blank in Table 1 (the acidolysis solution prepared in example 2) and the seaweed liquid prepared in example 2, the flowability of the product can be improved after the acidolysis solution is subjected to enzymolysis, and the solid content and the seaweed polysaccharide content in the extract can be improved; as can be seen from the comparison of the data of the seaweed liquid prepared in comparison 2 (except that the enzyme in the enzymolysis only adopts cellulase, and the other preparation methods are all consistent with those of example 1) in Table 1 with the seaweed liquid prepared in example 1, and comparison 3 (except that the enzyme in the enzymolysis only adopts saccharifying enzyme, and the other preparation methods are all consistent with those of example 2) with the seaweed liquid prepared in example 2, the solid content and polysaccharide content in the seaweed liquid can be remarkably improved by adopting the combined extraction of saccharifying enzyme and cellulase; as can be seen from the comparison of the data of comparative example 1 (except that no acid hydrolysis is performed, the preparation method is the same as that of example 3) and the seaweed liquid prepared in example 3 in Table 1, the seaweed liquid prepared in example 3 by the combined extraction of acid hydrolysis and enzymatic hydrolysis has a solid content increased by 12%, the seaweed polysaccharide increased by 4.4% and the cytokinin decreased by 0.6. mu.g/g, compared with comparative example 1 by the enzymatic hydrolysis only. As can be seen from the comparison of the data of the seaweed liquids prepared in example 1, example 2, example 3 and example 4, the effect of the extraction of example 3 and example 4 by using saccharifying enzyme and cellulase respectively is significantly better than that of the seaweed liquid prepared in example 1 and the seaweed liquid prepared in example 2 by using complex enzyme; as can be seen from the comparison of the data of the seaweed liquids prepared in the examples 3, 4, 5 and 6, the stability of the quality of the seaweed liquid can be obviously improved by introducing nitrogen for protection before enzymolysis.
Experiment two
Test material
1.1 test site: the detection was made by Sanfeng (tobacco pipe) agriculture science and technology Co.
1.2 test detection: free radical (DPPH) clearance (%) and water split loss (%).
1.3 test materials: the freshly prepared seaweed liquids of comparative example 1 (except that no acid hydrolysis was carried out, the preparation methods were the same as those in example 3), comparative example 2 (except that only cellulase was used as an enzyme in the enzymatic hydrolysis, and the preparation methods were the same as those in example 1), comparative example 3 (except that only glucoamylase was used as an enzyme in the enzymatic hydrolysis, and the preparation methods were the same as those in example 2), the freshly prepared seaweed liquids of examples 1 to 3, and the freshly prepared seaweed liquids of example 5 were allowed to stand for 6 months, and the seaweed liquids of example 3 (designated as final example 3) and example 5 (designated as final example 5) were adjusted to pH 7 with triethanolamine before the experiment.
1.4 Experimental implementation: DPPH clearance adopts a diphenylbitter acyl radical analysis method; the skin water loss tester Tewameter TM300 is characterized in that the mass ratio of a sample to be tested to ethanol is 1: 100.
The experimental temperature is 25 ℃; humidity is 40% -60%, and real-time dynamic monitoring is carried out.
The tested part can not be used for any product (cosmetics or external medicines) 2 days before testing, and can not contact water within 2 h. Before testing, the subjects needed to clean the inner sides of the forearms of both hands uniformly by wiping them clean with a clean facial tissue.
The part of the inner side of the forearm of the subject 5cm away from the base of the palm is an experimental part, and each experimental part is 9cm2The same arm marks 6 test areas, each 1.5cm apart.
The test should be rested for 30min in a standard room before official testing. The forearm is exposed and placed in a test state to keep relaxed.
The product application area and the blank control area should be randomly distributed in the left and right arm calibration areas to ensure that all product and blank area positions are statistically balanced.
Moisture content and water loss were measured in CM825 and TM300, respectively, and each zone was measured in duplicate 6 times, averaged, and recorded as a blank value.
The test sample is 2.0 +/-0.1 mg/cm2The amount of the coating is used for single coating, and a latex finger sleeve is usedThe test specimens were evenly coated in the test area.
The water content and water loss were measured for 1h, 2h, 3h and 4h of the applied samples using CM825 and TM300, respectively, 6 times, and averaged.
The number of test subjects per experimental treatment was 10, 90 total, between 20 and 30 years of age, combined randomly.
The present application is consistent in other implementations except for differences in the respective processes.
2 results and analysis
The results of the radical (DPPH) clearance (%), water content (%) and water loss (%) measurements are shown in Table 2
TABLE 2
As can be seen from the comparison of the data in Table 2, the DPPH clearance rate has better effect along with the increase of the solid content in the seaweed liquid, and as can be seen from the comparison of the effect of the embodiment 3 and the final embodiment 3, the phenomenon of effect degradation, namely unstable quality, exists after the embodiment 3 which is not flushed with the nitrogen protection for a long time, and as can be seen from the data of the embodiment 5 and the final embodiment 5, the quality of the seaweed liquid is more stable after the seaweed liquid is flushed with the nitrogen protection, and the effect is more stable, namely the effect of the seaweed liquid is stabilized by flushing the nitrogen before enzymolysis.
Claims (7)
1. A marine bioactive cosmetic is characterized by comprising seaweed liquid, wherein the seaweed liquid is prepared according to the following steps:
1) acid hydrolysis: adding seaweed into water, and extracting under the condition that the pH value is 2-3 to obtain acidolysis solution;
2) enzymolysis: adjusting the pH value of the acidolysis solution to 4.2-6.5, adding enzyme, and carrying out enzymolysis to obtain an enzymolysis solution;
3) seaweed solution: the enzymolysis liquid obtained in the step 2) is seaweed liquid, or
Filtering the enzymolysis liquid to obtain filtrate, namely the seaweed liquid;
the enzyme is saccharifying enzyme and cellulase;
the mass ratio of the seaweed to the water in the step 1) is 1-2: 3-6;
the extraction conditions of step 1) are 5-30 ℃, the stirring speed is 65-100 r/min, and the time is 20-40 min;
the mass ratio of the seaweed to the enzyme is 10000: 0.1-5; the enzymolysis temperature is 26-62 ℃, and the enzymolysis time is 6-72 h.
2. The marine bioactive cosmetic of claim 1 wherein said enzymatic hydrolysis is divided into carbohydrase enzymatic hydrolysis and cellulase enzymatic hydrolysis; the saccharification enzymolysis and the cellulase enzymolysis are not carried out simultaneously;
the enzymolysis temperature of the saccharification enzymatic hydrolysis is 55-62 ℃, and the enzymolysis time is 6-24 h; enzyme deactivation is carried out after enzymolysis, wherein the enzyme deactivation temperature is 90-120 ℃, and the enzyme deactivation time is 2-5 min;
the enzymolysis temperature of the cellulase enzymolysis is 26-35 ℃, and the enzymolysis time is 6-48 h; and enzyme deactivation is carried out after enzymolysis, wherein the enzyme deactivation temperature is 90-120 ℃, and the enzyme deactivation time is 2-5 min.
3. The marine bioactive cosmetic of claim 2 wherein said glycolytic enzymatic hydrolysis is performed according to the following steps:
and adjusting the pH value of the acidolysis solution to 4.0-4.5, adding saccharifying enzyme, and carrying out enzymolysis to obtain a saccharifying enzymolysis seaweed solution.
4. The marine bioactive cosmetic of claim 2 wherein the cellulase enzymatic hydrolysis is carried out according to the following steps:
and adjusting the pH value of the acidolysis solution to 5.5-6.5, adding cellulase, and carrying out enzymolysis to obtain cellulase-hydrolyzed seaweed solution.
5. The marine bioactive cosmetic of claim 3 wherein the cellulase enzymatic hydrolysis is carried out according to the following steps:
adjusting the pH value of the saccharification and enzymolysis seaweed liquid to 5.5-6.5, adding cellulase, and carrying out enzymolysis to obtain cellulase-hydrolyzed seaweed liquid, namely the seaweed liquid; or
Filtering the cellulose hydrolysate to obtain seaweed liquid.
6. The marine bioactive cosmetic of claim 4 wherein said glycolytic enzymatic hydrolysis is performed according to the following steps:
adjusting the pH value of the cellulase enzymolysis liquid to 4.0-4.5, adding saccharifying enzyme for enzymolysis to obtain a saccharifying enzymolysis seaweed liquid, namely the seaweed liquid; or
Filtering the saccharified enzymatic hydrolysate to obtain the seaweed liquid.
7. The marine bioactive cosmetic of any of claims 4, 5, 6, wherein the enzymatic hydrolysis of cellulase further comprises introducing nitrogen gas before enzymatic hydrolysis until the oxygen content in saccharified enzymatic hydrolysate or acidolyzed solution is less than 0.2 mg/L;
the saccharification enzymatic hydrolysis also comprises introducing nitrogen before the enzymatic hydrolysis until the oxygen content in the saccharification enzymatic hydrolysis liquid or the acidolysis liquid is lower than 0.2 mg/L.
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