Composition of isobutylamido thiazolyl resorcinol as well as preparation method and application of composition
Through the combination and multi-step extraction technology of isobutylamide thiazolyl resorcinol and plant extracts, the problem of poor whitening effect of existing compositions is solved, and more effective tyrosinase inhibition and melanin are achieved. The generation slows down, significantly improving the whitening effect.
Patent Information
- Application Number
- CN202411077203.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-07
- Publication Date
- 2024-12-06
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The whitening effect of the existing compositions with isobutylamide thiazolyl resorcinol is not ideal, and it is difficult to effectively inhibit tyrosinase activity, resulting in poor slowing melanin production.
Isobutylamide thiazolyl resorcinol is combined with a variety of plant extracts, and the composition is prepared by anaerobic fermentation, enzymatic fermentation, ultrasonic extraction and supercritical extraction, etc., using Bifidobacter lactobacillus and titanium Enzymatic reactions such as glycozymes improve the whitening effect of the composition.
Through the combination and extraction technology, the whitening effect of the composition is significantly improved, which is better than the use of isobutylamide thiazolyl resorcinol alone, achieving more effective tyrosinase inhibition and slowing of melanin production.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of cosmetics, and in particular relates to an isobutylamide thiazolyl resorcinol composition, a preparation method and an application thereof. Background Art
[0002] In melanocytes, the tyrosine that originally existed in the cells will be converted into L-dopa through the action of tyrosinase, and L-dopa will be converted into L-dopaquinone through the catalytic action of tyrosinase again. Furthermore, L-dopaquinone will form melanin through a series of oxidation reactions. Among them, tyrosinase is the only enzyme that determines the melanin synthesis reaction process. Therefore, effectively inhibiting tyrosinase can effectively slow down the two oxidation processes of tyrosine turning into dopa and dopa turning into dopaquinone. Therefore, effectively inhibiting tyrosinase in melanocytes can promote the reduction of melanin production and achieve the effect of whitening.
[0003] Beiersdorf of Germany published three important whitening articles. They screened out an ingredient that has a good effect on inhibiting tyrosinase activity from 50,000 compounds - isobutylamidothiazolylresorcinol. However, the whitening effect of the composition with isobutylamidothiazolylresorcinol is not ideal. Summary of the invention
[0004] The purpose of the present invention is to provide an isobutylamide thiazolyl resorcinol composition and a preparation method and application thereof.
[0005] In order to achieve the above object, the present invention provides the following technical solutions: A method for preparing a composition of isobutylamidothiazolylresorcinol comprises the following steps: (1) Weigh the following raw materials in parts by weight: 5-10 parts of isobutylamidothiazolylresorcinol, 1-5 parts of agrimony, 3-8 parts of rhodiola rosea, 2-7 parts of cassia seed, 4-8 parts of pine nuts, 3-7 parts of golden buckwheat, 1-4 parts of mint, 2-6 parts of liquorice, 5-10 parts of valerian root, 1-4 parts of pomegranate seeds, 1-5 parts of custard apple, 2-8 parts of fresh perilla stems, 1-3 parts of black beans, 1-3 parts of Poria cocos, 2-5 parts of Polygala tenuifolia, and 3-7 parts of Polygonatum odoratum; (2) Mixing Agrimony Root, Rhodiola Rosea, Cassia Seed, and Platycladus Semen, and crushing through an 80-100 mesh sieve to obtain a first mixed powder, mixing 70-80 parts by weight of the first mixed powder with 220-250 parts by weight of purified water, and sterilizing to obtain a mixed liquid; adding 1 part by weight of Bifidobacterium lactis and the mixed liquid to a fermenter, and performing anaerobically fermentation for 4-6 days. After the fermentation is completed, sterilizing to obtain a fermentation system; centrifuging the fermentation system, and then filtering through a 0.22 μm membrane, taking the supernatant, and spray drying to obtain a first extract; (3) Mix golden buckwheat, mint and licorice, dry and grind to 80-100 mesh to obtain a second mixed powder; mix the second mixed powder with water, heat to 36-38°C, add xylanase for enzymolysis, inactivate the enzyme after the enzymolysis, cool to room temperature, and obtain an enzymolysis product; sonicate the enzymolysis product to obtain an extract; filter the extract using a 0.22 μm filter membrane, concentrate, and vacuum dry to obtain a second extract; (4) Mix valerian roots, pomegranate seeds, sugar apples, and fresh perilla stems, and grind them through an 80-100 mesh sieve to obtain a third mixed powder; mix the third mixed powder with an ethanol aqueous solution having a mass fraction of 70-75%, and perform ultrasonic extraction for 60-70 minutes at an ultrasonic frequency of 40-60 Hz to obtain an ultrasonic product; heat the ultrasonic product under reflux for 5-7 hours, and filter it using a 0.45 μm filter membrane to obtain a filtrate; treat the filtrate with a non-polar macroporous adsorption resin, collect the eluate, and concentrate and dry it to obtain a third extract; (5) mixing black beans, Poria cocos, Polygala tenuifolia and Polygonatum odoratum, and grinding the mixture through a 80-100 mesh sieve to obtain a fourth mixed powder; subjecting the third mixed powder to supercritical extraction to obtain a fourth extract; (6) The isobutylamide thiazolyl resorcinol, the first extract, the second extract, the third extract and the fourth extract are mixed evenly to obtain a composition of isobutylamide thiazolyl resorcinol.
[0006] Furthermore, the conditions for anaerobic fermentation are: pH 6.3-6.5, temperature 36-40°C.
[0007] Furthermore, the fermentation system was centrifuged at 8000-9000 rpm for 10-15 min.
[0008] Furthermore, the mass ratio of the second mixed powder to water is 1:11-14.
[0009] Furthermore, the added amount of xylanase accounts for 1-3% of the mass of the second mixed powder.
[0010] Furthermore, the ultrasonic conditions for the enzymatic hydrolysis product are: ultrasonic extraction for 1.2 to 1.5 h, and an ultrasonic frequency of 30 to 40 Hz.
[0011] Furthermore, the third mixed powder with a mass ratio of 1:8-10 and an ethanol aqueous solution with a mass fraction of 70-75% are mixed.
[0012] Furthermore, the conditions for supercritical extraction are: 35-45°C, 30-35MPa, CO 2 Extraction was performed for 80-100 min at a flow rate of 18-20 L / h.
[0013] Furthermore, the enzyme inactivation condition is: heating at 121°C for 15 min.
[0014] The invention provides an isobutylamidothiazolylresorcinol composition prepared by the preparation method.
[0015] The present invention also provides an application of an isobutylamidothiazolylresorcinol composition in the preparation of cosmetics.
[0016] Compared with the prior art, the advantages and beneficial effects of the present invention are as follows: the present invention compounds isobutylamide thiazolyl resorcinol with plant extracts, and extracts natural plant raw materials in groups, so that the components have a synergistic effect, and the inhibitory effect of mixed extraction can be avoided. The whitening effect of the composition of the present invention is better than that of using isobutylamide thiazolyl resorcinol alone. DETAILED DESCRIPTION
[0017] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0018] Example 1 This embodiment provides a method for preparing a composition of isobutylamidothiazolylresorcinol, comprising the following steps: (1) Weigh the following raw materials in parts by weight: 7 parts of isobutylamidothiazolylresorcinol, 3 parts of agrimony, 5 parts of rhodiola rosea, 4 parts of cassia seed, 6 parts of cypress seed, 5 parts of golden buckwheat, 2 parts of mint, 5 parts of liquorice, 8 parts of valerian root, 3 parts of pomegranate seed, 3 parts of custard apple, 5 parts of fresh perilla stem, 2 parts of black bean, 3 parts of Poria cocos, 4 parts of Polygala tenuifolia, and 6 parts of Polygonatum odoratum; (2) Mixing Herba Agrimoniae, Rhodiola Rosea, Semen Cassiae and Semen Platycladi, and grinding the mixture through an 80-mesh sieve to obtain a first mixed powder; mixing 70 parts by weight of the first mixed powder with 220 parts by weight of purified water, and sterilizing the mixture to obtain a mixed liquid; adding 1 part by weight of Bifidobacterium lactis and the mixed liquid to a fermenter, and performing anaerobically fermentation for 4 days; and sterilizing the mixture after the fermentation is completed to obtain a fermentation system; centrifuging the fermentation system, and then filtering the mixture through a 0.22 μm membrane, taking the supernatant, and spray drying the mixture to obtain a first extract; (3) Mix golden buckwheat, mint and licorice, dry and grind to 80 mesh, and obtain a second mixed powder; mix the second mixed powder with water, heat to 36°C, add xylanase for enzymolysis, inactivate the enzyme after the enzymolysis, cool to room temperature, and obtain an enzymolysis product; sonicate the enzymolysis product to obtain an extract; filter the extract using a 0.22 μm filter membrane, concentrate, and vacuum dry to obtain a second extract; (4) Mix valerian roots, pomegranate seeds, sugar apples, and fresh perilla stems, and grind them through an 80-mesh sieve to obtain a third mixed powder; mix the third mixed powder with a 70% by mass ethanol aqueous solution, and perform ultrasonic extraction for 60 minutes at an ultrasonic frequency of 40 Hz to obtain an ultrasonic product; heat the ultrasonic product under reflux for 5 hours, and filter it using a 0.45 μm filter membrane to obtain a filtrate; treat the filtrate with a non-polar macroporous adsorption resin, collect the eluate, and concentrate and dry it to obtain a third extract; (5) mixing black beans, Poria cocos, Polygala tenuifolia and Polygonatum odoratum, and grinding the mixture through an 80-mesh sieve to obtain a fourth mixed powder; subjecting the third mixed powder to supercritical extraction to obtain a fourth extract; (6) The isobutylamide thiazolyl resorcinol, the first extract, the second extract, the third extract and the fourth extract are mixed evenly to obtain a composition of isobutylamide thiazolyl resorcinol.
[0019] The conditions for anaerobic fermentation are: pH 6.3, temperature 36°C.
[0020] The fermentation system was centrifuged at 8000 rpm for 10 min.
[0021] The mass ratio of the second mixed powder to water is 1:11.
[0022] The added amount of xylanase accounts for 1% of the mass of the second mixed powder.
[0023] The ultrasonic conditions for the enzymatic hydrolysis product were as follows: ultrasonic extraction for 1.2 h and an ultrasonic frequency of 30 Hz.
[0024] The third mixed powder in a mass ratio of 1:8 and an ethanol aqueous solution with a mass fraction of 70% are mixed.
[0025] The conditions for supercritical extraction are: 35°C, 30MPa, CO 2The extraction was carried out for 80 min at a flow rate of 18 L / h.
[0026] The conditions for inactivating the enzyme were: heating at 121°C for 15 min.
[0027] Example 2 This embodiment provides a method for preparing a composition of isobutylamidothiazolylresorcinol, comprising the following steps: (1) Weigh the following raw materials in parts by weight: 10 parts of isobutylamidothiazolylresorcinol, 1 part of Agrimoniae, 8 parts of Rhodiola rosea, 2 parts of Cassia seed, 8 parts of Platycladus orientalis, 7 parts of Fagopyrum sibiricum, 1 part of mint, 6 parts of Licorice root, 5 parts of Valerian root, 4 parts of Pomegranate seed, 1 part of Sugar Apple, 8 parts of Fresh Perilla stem, 1 part of Black Bean, 3 parts of Poria, 2 parts of Polygala tenuifolia, and 7 parts of Polygonatum odoratum; (2) Mixing Herba Agrimoniae, Rhodiola Rosea, Semen Cassiae and Semen Platycladi, and grinding the mixture through a 100-mesh sieve to obtain a first mixed powder; mixing 70 parts by weight of the first mixed powder with 250 parts by weight of purified water, and sterilizing the mixture to obtain a mixed liquid; adding 1 part by weight of Bifidobacterium lactis and the mixed liquid to a fermenter, and performing anaerobically fermentation for 4 days; and sterilizing the mixture after the fermentation is completed to obtain a fermentation system; centrifuging the fermentation system, and then filtering the mixture through a 0.22 μm membrane, taking the supernatant, and spray drying the mixture to obtain a first extract; (3) Mix golden buckwheat, mint and licorice, dry and grind to 100 mesh to obtain a second mixed powder; mix the second mixed powder with water, heat to 36°C, add xylanase for enzymolysis, inactivate the enzyme after the enzymolysis, cool to room temperature, and obtain an enzymolysis product; sonicate the enzymolysis product to obtain an extract; filter the extract using a 0.22 μm filter membrane, concentrate, and vacuum dry to obtain a second extract; (4) Mix valerian roots, pomegranate seeds, sugar apples, and fresh perilla stems, and grind them through a 100-mesh sieve to obtain a third mixed powder; mix the third mixed powder with a 70% by mass ethanol aqueous solution, and perform ultrasonic extraction for 60 minutes at an ultrasonic frequency of 60 Hz to obtain an ultrasonic product; heat the ultrasonic product under reflux for 7 hours, and filter it using a 0.45 μm filter membrane to obtain a filtrate; treat the filtrate with a non-polar macroporous adsorption resin, collect the eluate, and concentrate and dry it to obtain a third extract; (5) mixing black beans, Poria cocos, Polygala tenuifolia and Polygonatum odoratum, and grinding the mixture through a 100-mesh sieve to obtain a fourth mixed powder; subjecting the third mixed powder to supercritical extraction to obtain a fourth extract; (6) The isobutylamide thiazolyl resorcinol, the first extract, the second extract, the third extract and the fourth extract are mixed evenly to obtain a composition of isobutylamide thiazolyl resorcinol.
[0028] The conditions for anaerobic fermentation are: pH 6.3, temperature 40°C.
[0029] The fermentation system was centrifuged at 9000 rpm for 10 min.
[0030] The mass ratio of the second mixed powder to water is 1:11.
[0031] The added amount of xylanase is 3% of the mass of the second mixed powder.
[0032] The ultrasonic conditions for the enzymatic hydrolysis product were as follows: ultrasonic extraction for 1.2 h and an ultrasonic frequency of 40 Hz.
[0033] The third mixed powder in a mass ratio of 1:8 and an ethanol aqueous solution with a mass fraction of 70% are mixed.
[0034] The conditions of supercritical extraction are: 45℃, 35MPa, CO 2 The extraction was carried out for 100 min at a flow rate of 18 L / h.
[0035] The conditions for inactivating the enzyme were: heating at 121°C for 15 min.
[0036] Comparative Example 1 The difference between this comparative example and Example 1 is that the amounts of Agrimoniae, Rhodiola rosea, Cassia seed and Platycladus orientalis seeds are different.
[0037] A method for preparing a composition of isobutylamidothiazolylresorcinol comprises the following steps: (1) Weigh the following raw materials in parts by weight: 7 parts of isobutylamidothiazolylresorcinol, 7 parts of agrimony, 1 part of rhodiola rosea, 9 parts of cassia seed, 1 part of cypress seed, 5 parts of golden buckwheat, 2 parts of mint, 5 parts of liquorice, 8 parts of valerian root, 3 parts of pomegranate seeds, 3 parts of custard apple, 5 parts of fresh perilla stems, 2 parts of black beans, 3 parts of Poria cocos, 4 parts of Polygala tenuifolia, and 6 parts of Polygonatum odoratum; (2) Mixing Herba Agrimoniae, Rhodiola Rosea, Semen Cassiae and Semen Platycladi, and grinding the mixture through an 80-mesh sieve to obtain a first mixed powder; mixing 70 parts by weight of the first mixed powder with 220 parts by weight of purified water, and sterilizing the mixture to obtain a mixed liquid; adding 1 part by weight of Bifidobacterium lactis and the mixed liquid to a fermenter, and performing anaerobically fermentation for 4 days; and sterilizing the mixture after the fermentation is completed to obtain a fermentation system; centrifuging the fermentation system, and then filtering the mixture through a 0.22 μm membrane, taking the supernatant, and spray drying the mixture to obtain a first extract; (3) Mix golden buckwheat, mint and licorice, dry and grind to 80 mesh, and obtain a second mixed powder; mix the second mixed powder with water, heat to 36°C, add xylanase for enzymolysis, inactivate the enzyme after the enzymolysis, cool to room temperature, and obtain an enzymolysis product; sonicate the enzymolysis product to obtain an extract; filter the extract using a 0.22 μm filter membrane, concentrate, and vacuum dry to obtain a second extract; (4) Mix valerian roots, pomegranate seeds, sugar apples, and fresh perilla stems, and grind them through an 80-mesh sieve to obtain a third mixed powder; mix the third mixed powder with a 70% by mass ethanol aqueous solution, and perform ultrasonic extraction for 60 minutes at an ultrasonic frequency of 40 Hz to obtain an ultrasonic product; heat the ultrasonic product under reflux for 5 hours, and filter it using a 0.45 μm filter membrane to obtain a filtrate; treat the filtrate with a non-polar macroporous adsorption resin, collect the eluate, and concentrate and dry it to obtain a third extract; (5) mixing black beans, Poria cocos, Polygala tenuifolia and Polygonatum odoratum, and grinding the mixture through an 80-mesh sieve to obtain a fourth mixed powder; subjecting the third mixed powder to supercritical extraction to obtain a fourth extract; (6) The isobutylamide thiazolyl resorcinol, the first extract, the second extract, the third extract and the fourth extract are mixed evenly to obtain a composition of isobutylamide thiazolyl resorcinol.
[0038] The conditions for anaerobic fermentation are: pH 6.3, temperature 36°C.
[0039] The fermentation system was centrifuged at 8000 rpm for 10 min.
[0040] The mass ratio of the second mixed powder to water is 1:11.
[0041] The added amount of xylanase accounts for 1% of the mass of the second mixed powder.
[0042] The ultrasonic conditions for the enzymatic hydrolysis product were as follows: ultrasonic extraction for 1.2 h and an ultrasonic frequency of 30 Hz.
[0043] The third mixed powder in a mass ratio of 1:8 and an ethanol aqueous solution with a mass fraction of 70% are mixed.
[0044] The conditions for supercritical extraction are: 35°C, 30MPa, CO 2 The extraction was carried out for 80 min at a flow rate of 18 L / h.
[0045] The conditions for inactivating the enzyme were: heating at 121°C for 15 min.
[0046] Comparative Example 2 The difference between this comparative example and Example 1 is that the amount of golden buckwheat, mint and licorice is different. A method for preparing a composition of isobutylamidothiazolylresorcinol comprises the following steps: (1) Weigh the following raw materials in parts by weight: 1 part of isobutylamidothiazolylresorcinol, 6 parts of agrimony, 8 parts of rhodiola rosea, 4 parts of cassia seed, 6 parts of cypress seed, 5 parts of golden buckwheat, 2 parts of mint, 5 parts of liquorice, 8 parts of valerian root, 3 parts of pomegranate seeds, 3 parts of custard apple, 5 parts of fresh perilla stems, 2 parts of black beans, 3 parts of Poria cocos, 4 parts of Polygala tenuifolia, and 6 parts of Polygonatum odoratum; (2) Mixing Herba Agrimoniae, Rhodiola Rosea, Semen Cassiae and Semen Platycladi, and grinding the mixture through an 80-mesh sieve to obtain a first mixed powder; mixing 70 parts by weight of the first mixed powder with 220 parts by weight of purified water, and sterilizing the mixture to obtain a mixed liquid; adding 1 part by weight of Bifidobacterium lactis and the mixed liquid to a fermenter, and performing anaerobically fermentation for 4 days; and sterilizing the mixture after the fermentation is completed to obtain a fermentation system; centrifuging the fermentation system, and then filtering the mixture through a 0.22 μm membrane, taking the supernatant, and spray drying the mixture to obtain a first extract; (3) Mix golden buckwheat, mint and licorice, dry and grind to 80 mesh, and obtain a second mixed powder; mix the second mixed powder with water, heat to 36°C, add xylanase for enzymolysis, inactivate the enzyme after the enzymolysis, cool to room temperature, and obtain an enzymolysis product; sonicate the enzymolysis product to obtain an extract; filter the extract using a 0.22 μm filter membrane, concentrate, and vacuum dry to obtain a second extract; (4) Mix valerian roots, pomegranate seeds, sugar apples, and fresh perilla stems, and grind them through an 80-mesh sieve to obtain a third mixed powder; mix the third mixed powder with a 70% by mass ethanol aqueous solution, and perform ultrasonic extraction for 60 minutes at an ultrasonic frequency of 40 Hz to obtain an ultrasonic product; heat the ultrasonic product under reflux for 5 hours, and filter it using a 0.45 μm filter membrane to obtain a filtrate; treat the filtrate with a non-polar macroporous adsorption resin, collect the eluate, and concentrate and dry it to obtain a third extract; (5) mixing black beans, Poria cocos, Polygala tenuifolia and Polygonatum odoratum, and grinding the mixture through an 80-mesh sieve to obtain a fourth mixed powder; subjecting the third mixed powder to supercritical extraction to obtain a fourth extract; (6) The isobutylamide thiazolyl resorcinol, the first extract, the second extract, the third extract and the fourth extract are mixed evenly to obtain a composition of isobutylamide thiazolyl resorcinol.
[0047] The conditions for anaerobic fermentation are: pH 6.3, temperature 36°C.
[0048] The fermentation system was centrifuged at 8000 rpm for 10 min.
[0049] The mass ratio of the second mixed powder to water is 1:11.
[0050] The added amount of xylanase accounts for 1% of the mass of the second mixed powder.
[0051] The ultrasonic conditions for the enzymatic hydrolysis product were as follows: ultrasonic extraction for 1.2 h and an ultrasonic frequency of 30 Hz.
[0052] The third mixed powder in a mass ratio of 1:8 and an ethanol aqueous solution with a mass fraction of 70% are mixed.
[0053] The conditions for supercritical extraction are: 35°C, 30MPa, CO 2The extraction was carried out for 80 min at a flow rate of 18 L / h.
[0054] The conditions for inactivating the enzyme were: heating at 121°C for 15 min.
[0055] Comparative Example 3 The difference between this comparative example and Example 1 is that the amounts of valerian root, pomegranate seed, custard apple and fresh perilla stem are different.
[0056] A method for preparing a composition of isobutylamidothiazolylresorcinol comprises the following steps: (1) Weigh the following raw materials in parts by weight: 7 parts of isobutylamidothiazolylresorcinol, 3 parts of agrimony, 5 parts of rhodiola rosea, 4 parts of cassia seed, 6 parts of cypress seed, 5 parts of golden buckwheat, 2 parts of mint, 5 parts of liquorice, 3 parts of valerian root, 8 parts of pomegranate seeds, 7 parts of custard apple, 1 part of fresh perilla stem, 2 parts of black beans, 3 parts of Poria cocos, 4 parts of Polygala tenuifolia, and 6 parts of Polygonatum odoratum; (2) Mixing Herba Agrimoniae, Rhodiola Rosea, Semen Cassiae and Semen Platycladi, and grinding the mixture through an 80-mesh sieve to obtain a first mixed powder; mixing 70 parts by weight of the first mixed powder with 220 parts by weight of purified water, and sterilizing the mixture to obtain a mixed liquid; adding 1 part by weight of Bifidobacterium lactis and the mixed liquid to a fermenter, and performing anaerobically fermentation for 4 days; and sterilizing the mixture after the fermentation is completed to obtain a fermentation system; centrifuging the fermentation system, and then filtering the mixture through a 0.22 μm membrane, taking the supernatant, and spray drying the mixture to obtain a first extract; (3) Mix golden buckwheat, mint and licorice, dry and grind to 80 mesh, and obtain a second mixed powder; mix the second mixed powder with water, heat to 36°C, add xylanase for enzymolysis, inactivate the enzyme after the enzymolysis, cool to room temperature, and obtain an enzymolysis product; sonicate the enzymolysis product to obtain an extract; filter the extract using a 0.22 μm filter membrane, concentrate, and vacuum dry to obtain a second extract; (4) Mix valerian roots, pomegranate seeds, sugar apples, and fresh perilla stems, and grind them through an 80-mesh sieve to obtain a third mixed powder; mix the third mixed powder with a 70% by mass ethanol aqueous solution, and perform ultrasonic extraction for 60 minutes at an ultrasonic frequency of 40 Hz to obtain an ultrasonic product; heat the ultrasonic product under reflux for 5 hours, and filter it using a 0.45 μm filter membrane to obtain a filtrate; treat the filtrate with a non-polar macroporous adsorption resin, collect the eluate, and concentrate and dry it to obtain a third extract; (5) mixing black beans, Poria cocos, Polygala tenuifolia and Polygonatum odoratum, and grinding the mixture through an 80-mesh sieve to obtain a fourth mixed powder; subjecting the third mixed powder to supercritical extraction to obtain a fourth extract; (6) The isobutylamide thiazolyl resorcinol, the first extract, the second extract, the third extract and the fourth extract are mixed evenly to obtain a composition of isobutylamide thiazolyl resorcinol.
[0057] The conditions for anaerobic fermentation are: pH 6.3, temperature 36°C.
[0058] The fermentation system was centrifuged at 8000 rpm for 10 min.
[0059] The mass ratio of the second mixed powder to water is 1:11.
[0060] The added amount of xylanase accounts for 1% of the mass of the second mixed powder.
[0061] The ultrasonic conditions for the enzymatic hydrolysis product were as follows: ultrasonic extraction for 1.2 h and an ultrasonic frequency of 30 Hz.
[0062] The third mixed powder in a mass ratio of 1:8 and an ethanol aqueous solution with a mass fraction of 70% are mixed.
[0063] The conditions for supercritical extraction are: 35°C, 30MPa, CO 2 The extraction was carried out for 80 min at a flow rate of 18 L / h.
[0064] The conditions for inactivating the enzyme were: heating at 121°C for 15 min.
[0065] Comparative Example 4 The difference between this comparative example and Example 1 is that the portions of black beans, Poria cocos, Polygala tenuifolia and Polygonatum odoratum are different.
[0066] A method for preparing a composition of isobutylamidothiazolylresorcinol comprises the following steps: (1) Weigh the following raw materials in parts by weight: 7 parts of isobutylamidothiazolylresorcinol, 3 parts of agrimony, 5 parts of rhodiola rosea, 4 parts of cassia seed, 6 parts of cypress seed, 5 parts of golden buckwheat, 2 parts of mint, 5 parts of liquorice, 8 parts of valerian root, 3 parts of pomegranate seed, 3 parts of custard apple, 5 parts of fresh perilla stem, 5 parts of black bean, 8 parts of Poria cocos, 1 part of Polygala tenuifolia, and 1 part of Polygonatum odoratum; (2) Mixing Herba Agrimoniae, Rhodiola Rosea, Semen Cassiae and Semen Platycladi, and grinding the mixture through an 80-mesh sieve to obtain a first mixed powder; mixing 70 parts by weight of the first mixed powder with 220 parts by weight of purified water, and sterilizing the mixture to obtain a mixed liquid; adding 1 part by weight of Bifidobacterium lactis and the mixed liquid to a fermenter, and performing anaerobically fermentation for 4 days; and sterilizing the mixture after the fermentation is completed to obtain a fermentation system; centrifuging the fermentation system, and then filtering the mixture through a 0.22 μm membrane, taking the supernatant, and spray drying the mixture to obtain a first extract; (3) Mix golden buckwheat, mint and licorice, dry and grind to 80 mesh, and obtain a second mixed powder; mix the second mixed powder with water, heat to 36°C, add xylanase for enzymolysis, inactivate the enzyme after the enzymolysis, cool to room temperature, and obtain an enzymolysis product; sonicate the enzymolysis product to obtain an extract; filter the extract using a 0.22 μm filter membrane, concentrate, and vacuum dry to obtain a second extract; (4) Mix valerian roots, pomegranate seeds, sugar apples, and fresh perilla stems, and grind them through an 80-mesh sieve to obtain a third mixed powder; mix the third mixed powder with a 70% by mass ethanol aqueous solution, and perform ultrasonic extraction for 60 minutes at an ultrasonic frequency of 40 Hz to obtain an ultrasonic product; heat the ultrasonic product under reflux for 5 hours, and filter it using a 0.45 μm filter membrane to obtain a filtrate; treat the filtrate with a non-polar macroporous adsorption resin, collect the eluate, and concentrate and dry it to obtain a third extract; (5) mixing black beans, Poria cocos, Polygala tenuifolia and Polygonatum odoratum, and grinding the mixture through an 80-mesh sieve to obtain a fourth mixed powder; subjecting the third mixed powder to supercritical extraction to obtain a fourth extract; (6) The isobutylamide thiazolyl resorcinol, the first extract, the second extract, the third extract and the fourth extract are mixed evenly to obtain a composition of isobutylamide thiazolyl resorcinol.
[0067] The conditions for anaerobic fermentation are: pH 6.3, temperature 36°C.
[0068] The fermentation system was centrifuged at 8000 rpm for 10 min.
[0069] The mass ratio of the second mixed powder to water is 1:11.
[0070] The added amount of xylanase accounts for 1% of the mass of the second mixed powder.
[0071] The ultrasonic conditions for the enzymatic hydrolysis product were as follows: ultrasonic extraction for 1.2 h and an ultrasonic frequency of 30 Hz.
[0072] The third mixed powder in a mass ratio of 1:8 and an ethanol aqueous solution with a mass fraction of 70% are mixed.
[0073] The conditions for supercritical extraction are: 35°C, 30MPa, CO 2 The extraction was carried out for 80 min at a flow rate of 18 L / h.
[0074] The conditions for inactivating the enzyme were: heating at 121°C for 15 min.
[0075] Comparative Example 5 The difference between this comparative example and Example 1 is: A method for preparing a composition of isobutylamidothiazolylresorcinol comprises the following steps: (1) Weigh the following raw materials in parts by weight: 7 parts of isobutylamidothiazolylresorcinol, 3 parts of agrimony, 5 parts of rhodiola rosea, 4 parts of cassia seed, 6 parts of cypress seed, 5 parts of golden buckwheat, 2 parts of mint, 5 parts of liquorice, 8 parts of valerian root, 3 parts of pomegranate seed, 3 parts of custard apple, 5 parts of fresh perilla stem, 2 parts of black bean, 3 parts of Poria cocos, 4 parts of Polygala tenuifolia, and 6 parts of Polygonatum odoratum; (2) All raw materials except isobutylamidothiazolylresorcinol are mixed, crushed through an 80-mesh sieve to obtain a mixed powder, the mixed powder is mixed with a 70% by mass ethanol aqueous solution, and ultrasonic extraction is performed for 60 minutes at an ultrasonic frequency of 40 Hz to obtain an ultrasonic product; the ultrasonic product is heated to reflux for 5 hours, filtered using a 0.45 μm filter membrane to obtain a filtrate; the filtrate is treated with a non-polar macroporous adsorption resin, the eluate is collected, concentrated, and dried to obtain an extract; (3) The isobutylamide thiazolyl resorcinol and the extract are mixed evenly to obtain an isobutylamide thiazolyl resorcinol composition.
[0076] The mixed powder in a mass ratio of 1:8 was mixed with an ethanol aqueous solution with a mass fraction of 70%.
[0077] Performance Testing Test subjects: 80 volunteers (25-45 years old), divided into 8 groups, each group with 10 people, mixed the compositions of Examples 1-2 and Comparative Examples 1-5 with glycerol in a ratio of 1:10. The control group mixed isobutylamidothiazolylresorcinol with glycerol in a ratio of 1:10.
[0078] Test area: face (blank sample on the left, comparative example or example sample on the right).
[0079] Use twice a day, morning and evening, for 4 weeks.
[0080] Testing instrument: Finnish Delfin skin tester, model: Delfin Skin Color Catch.
[0081] Effect index: Determine the change in color brightness (ΔL ). The calculation formula is: ΔL =[L (4 weeks after the comparative example or embodiment was tested) L (Before the test begins)] [L (Blank case after 1 month of testing) L (before the blank test)], calculate ΔL for each group average value.
[0082] Table 1 Performance test results
[0083] The results show that the composition of Example 1-2 has an excellent whitening effect. The combination of isobutylamide thiazolyl resorcinol and plant extract has a synergistic effect, and the whitening effect is better than that of using isobutylamide thiazolyl resorcinol alone.
[0084] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.
Claims
1. A method for preparing a composition of isobutylamidothiazolylresorcinol, characterized in that: The following steps are included: (1) Weigh the following raw materials in parts by weight: 5-10 parts of isobutylamidothiazolylresorcinol, 1-5 parts of agrimony, 3-8 parts of rhodiola rosea, 2-7 parts of cassia seed, 4-8 parts of pine nuts, 3-7 parts of golden buckwheat, 1-4 parts of mint, 2-6 parts of liquorice, 5-10 parts of valerian root, 1-4 parts of pomegranate seeds, 1-5 parts of custard apple, 2-8 parts of fresh perilla stems, 1-3 parts of black beans, 1-3 parts of Poria cocos, 2-5 parts of Polygala tenuifolia, and 3-7 parts of Polygonatum odoratum; (2) Mixing Agrimony Root, Rhodiola Rosea, Cassia Seed, and Platycladus Semen, and crushing through an 80-100 mesh sieve to obtain a first mixed powder, mixing 70-80 parts by weight of the first mixed powder with 220-250 parts by weight of purified water, and sterilizing to obtain a mixed liquid; adding 1 part by weight of Bifidobacterium lactis and the mixed liquid to a fermenter, and performing anaerobically fermentation for 4-6 days. After the fermentation is completed, sterilizing to obtain a fermentation system; centrifuging the fermentation system, and then filtering through a 0.22 μm membrane, taking the supernatant, and spray drying to obtain a first extract; (3) Mix golden buckwheat, mint and licorice, dry and grind to 80-100 mesh to obtain a second mixed powder; mix the second mixed powder with water, heat to 36-38°C, add xylanase for enzymolysis, inactivate the enzyme after the enzymolysis, cool to room temperature, and obtain an enzymolysis product; sonicate the enzymolysis product to obtain an extract; The extract was filtered using a 0.22 μm filter membrane, concentrated, and vacuum dried to obtain a second extract; (4) Mixing valerian roots, pomegranate seeds, sugar apples, and fresh perilla stems, and crushing them through a 80-100 mesh sieve to obtain a third mixed powder; mixing the third mixed powder with a 70-75% by mass ethanol aqueous solution, and performing ultrasonic extraction for 60-70 minutes at an ultrasonic frequency of 40-60 Hz to obtain an ultrasonic product; The ultrasonic product is heated to reflux for 5-7 hours, and filtered using a 0.45 μm filter membrane to obtain a filtrate; the filtrate is treated with a non-polar macroporous adsorption resin, and the eluate is collected, concentrated, and dried to obtain a third extract; (5) mixing black beans, Poria cocos, Polygala tenuifolia and Polygonatum odoratum, and grinding the mixture through a 80-100 mesh sieve to obtain a fourth mixed powder; subjecting the third mixed powder to supercritical extraction to obtain a fourth extract; (6) The isobutylamide thiazolyl resorcinol, the first extract, the second extract, the third extract and the fourth extract are mixed evenly to obtain a composition of isobutylamide thiazolyl resorcinol.
2. The method for preparing the composition of isobutylamidothiazolylresorcinol according to claim 1, characterized in that: The conditions for anaerobic fermentation are: pH 6.3-6.5, temperature 36-40℃.
3. The method for preparing the composition of isobutylamidothiazolylresorcinol according to claim 1, characterized in that: The fermentation system was centrifuged at 8000-9000 rpm for 10-15 min.
4. The method for preparing the composition of isobutylamidothiazolylresorcinol according to claim 1, characterized in that: The mass ratio of the second mixed powder to water is 1:11-14.
5. The method for preparing the composition of isobutylamidothiazolylresorcinol according to claim 1, characterized in that: The added amount of xylanase is 1-3% of the mass of the second mixed powder.
6. The method for preparing the isobutylamidothiazolylresorcinol composition according to claim 1, characterized in that: The ultrasonic conditions for the enzymatic hydrolysis product were as follows: ultrasonic extraction for 1.2-1.5 h and an ultrasonic frequency of 30-40 Hz.
7. The method for preparing the isobutylamidothiazolylresorcinol composition according to claim 1, characterized in that: The third mixed powder in a mass ratio of 1:8-10 and an ethanol aqueous solution in a mass fraction of 70-75% are mixed.
8. The method for preparing the isobutylamidothiazolylresorcinol composition according to claim 1, characterized in that: The conditions of supercritical extraction are: extraction for 80-100 min at 35-45°C, 30-35 MPa, and a CO2 flow rate of 18-20 L / h.
9. A composition of isobutylamidothiazolylresorcinol prepared according to the preparation method of claims 1-8.
10. Use of the isobutylamidothiazolylresorcinol composition according to claim 9 in the preparation of cosmetics.