CN114306112A - Anti-aging composition and preparation method thereof - Google Patents
Anti-aging composition and preparation method thereof Download PDFInfo
- Publication number
- CN114306112A CN114306112A CN202111620612.7A CN202111620612A CN114306112A CN 114306112 A CN114306112 A CN 114306112A CN 202111620612 A CN202111620612 A CN 202111620612A CN 114306112 A CN114306112 A CN 114306112A
- Authority
- CN
- China
- Prior art keywords
- parts
- extract
- deionized water
- weight
- crocus sativus
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 230000003712 anti-aging effect Effects 0.000 title claims abstract description 58
- 239000000203 mixture Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 22
- 239000000284 extract Substances 0.000 claims abstract description 98
- 235000015655 Crocus sativus Nutrition 0.000 claims abstract description 58
- 244000124209 Crocus sativus Species 0.000 claims abstract description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000008367 deionised water Substances 0.000 claims abstract description 56
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 56
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 55
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims abstract description 46
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims abstract description 38
- BIVBRWYINDPWKA-VLQRKCJKSA-L Glycyrrhizinate dipotassium Chemical compound [K+].[K+].O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@H]1CC[C@]2(C)[C@H]3C(=O)C=C4[C@@H]5C[C@](C)(CC[C@@]5(CC[C@@]4(C)[C@]3(C)CC[C@H]2C1(C)C)C)C(O)=O)C([O-])=O)[C@@H]1O[C@H](C([O-])=O)[C@@H](O)[C@H](O)[C@H]1O BIVBRWYINDPWKA-VLQRKCJKSA-L 0.000 claims abstract description 23
- 229920002385 Sodium hyaluronate Polymers 0.000 claims abstract description 23
- 229930003427 Vitamin E Natural products 0.000 claims abstract description 23
- SZYSLWCAWVWFLT-UTGHZIEOSA-N [(2s,3s,4s,5r)-3,4-dihydroxy-5-(hydroxymethyl)-2-[(2r,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxolan-2-yl]methyl octadecanoate Chemical compound O([C@@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@]1(COC(=O)CCCCCCCCCCCCCCCCC)O[C@H](CO)[C@@H](O)[C@@H]1O SZYSLWCAWVWFLT-UTGHZIEOSA-N 0.000 claims abstract description 23
- 229940101029 dipotassium glycyrrhizinate Drugs 0.000 claims abstract description 23
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229940010747 sodium hyaluronate Drugs 0.000 claims abstract description 23
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(2s,3s,4s,5r,6r)-6-[(2s,3r,4r,5s,6r)-3-acetamido-2-[(2s,3s,4r,5r,6r)-6-[(2r,3r,4r,5s,6r)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2- Chemical compound [Na+].CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 claims abstract description 23
- 229940046009 vitamin E Drugs 0.000 claims abstract description 23
- 235000019165 vitamin E Nutrition 0.000 claims abstract description 23
- 239000011709 vitamin E Substances 0.000 claims abstract description 23
- 235000019437 butane-1,3-diol Nutrition 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 94
- 239000000243 solution Substances 0.000 claims description 63
- 239000007788 liquid Substances 0.000 claims description 38
- 239000000843 powder Substances 0.000 claims description 33
- 238000001035 drying Methods 0.000 claims description 26
- 238000005406 washing Methods 0.000 claims description 20
- 238000011068 loading method Methods 0.000 claims description 19
- 235000011187 glycerol Nutrition 0.000 claims description 18
- 239000011347 resin Substances 0.000 claims description 17
- 229920005989 resin Polymers 0.000 claims description 17
- 238000001179 sorption measurement Methods 0.000 claims description 17
- 239000000706 filtrate Substances 0.000 claims description 16
- 241000037831 Polygonatum sibiricum Species 0.000 claims description 11
- 239000003480 eluent Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 238000000108 ultra-filtration Methods 0.000 claims description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 108090000526 Papain Proteins 0.000 claims description 8
- 239000004365 Protease Substances 0.000 claims description 8
- 102000004142 Trypsin Human genes 0.000 claims description 8
- 108090000631 Trypsin Proteins 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 229940055729 papain Drugs 0.000 claims description 8
- 235000019834 papain Nutrition 0.000 claims description 8
- 239000012588 trypsin Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- -1 fucoidin Chemical compound 0.000 claims description 5
- 239000008363 phosphate buffer Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 4
- 235000013974 saffron Nutrition 0.000 claims description 4
- 239000004248 saffron Substances 0.000 claims description 4
- 229940058015 1,3-butylene glycol Drugs 0.000 claims 1
- 229960005150 glycerol Drugs 0.000 claims 1
- 230000003110 anti-inflammatory effect Effects 0.000 abstract description 8
- 230000003020 moisturizing effect Effects 0.000 abstract description 8
- 241000756042 Polygonatum Species 0.000 abstract description 6
- 239000002537 cosmetic Substances 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 description 26
- 150000003254 radicals Chemical class 0.000 description 24
- 239000000523 sample Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 17
- 235000004237 Crocus Nutrition 0.000 description 15
- 241000596148 Crocus Species 0.000 description 15
- 230000000694 effects Effects 0.000 description 15
- 239000012488 sample solution Substances 0.000 description 12
- 230000002000 scavenging effect Effects 0.000 description 10
- 239000006228 supernatant Substances 0.000 description 8
- 235000003255 Carthamus tinctorius Nutrition 0.000 description 5
- 244000020518 Carthamus tinctorius Species 0.000 description 5
- 230000007760 free radical scavenging Effects 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001599 crocus sativus l. flower extract Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000008055 phosphate buffer solution Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 229940076591 saffron extract Drugs 0.000 description 3
- 108010059892 Cellulase Proteins 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229940106157 cellulase Drugs 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 230000007850 degeneration Effects 0.000 description 2
- 238000002481 ethanol extraction Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- WSMYVTOQOOLQHP-UHFFFAOYSA-N Malondialdehyde Chemical compound O=CCC=O WSMYVTOQOOLQHP-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229940088598 enzyme Drugs 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 230000003859 lipid peroxidation Effects 0.000 description 1
- 229940118019 malondialdehyde Drugs 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- 150000007523 nucleic acids Chemical class 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000036542 oxidative stress Effects 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Landscapes
- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the technical field of cosmetics, and particularly discloses an anti-aging composition and a preparation method thereof, wherein the anti-aging composition comprises the following components in parts by weight: 0.05-0.3 part of dipotassium glycyrrhizinate, 0.2-0.6 part of sodium hyaluronate, 0.4-1 part of sucrose stearate, 1-3 parts of vitamin E, 1-5 parts of fucoidin, 2-5 parts of rhizoma polygonati extract, 3-7 parts of crocus sativus extract, 5-10 parts of glycerol, 4-12 parts of 1, 3-butanediol and 50-70 parts of deionized water. The anti-aging extract can effectively remove free radicals, so that a good anti-aging effect is achieved, the anti-aging, moisturizing and anti-inflammatory components based on dipotassium glycyrrhizinate, sodium hyaluronate, sucrose stearate, vitamin E and fucoidin can achieve good anti-aging, moisturizing and anti-inflammatory effects, and the anti-aging effect can be effectively improved by adding the active components of the polygonatum extract and the crocus sativus extract on the basis.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to an anti-aging composition and a preparation method thereof.
Background
Aging is a natural phenomenon in the life process and is the result of the combined action of various factors inside and outside the body. The essence of the natural degeneration is a gradual natural degeneration process of the structure and the function of cells, tissues, organs and the like of a living body under the stimulation of a plurality of factors inside and outside the living body along with the growth of the age.
The cells of the organism generate more active oxygen free radicals in the normal metabolic process, a proper amount of free radicals are beneficial to the effects of resisting inflammation, sterilizing and inhibiting tumors of the organism, and along with the occurrence of aging, the activity of endogenous antioxidant enzyme is reduced, the capacity of removing the free radicals is weakened, and the active oxygen free radicals are enabled to be generated. Active oxygen free radicals serving as strong oxidants can cause protein and nucleic acid denaturation and lipid peroxidation, the content of malondialdehyde serving as a metabolite is increased, and then oxidative stress is enhanced to damage cells and tissues, so that the skin is dry and loose, and aging is accelerated, so that how to eliminate the free radicals is an urgent technical problem to be solved.
Disclosure of Invention
The invention provides an anti-aging composition and a preparation method thereof, and the anti-aging extract can effectively remove free radicals, thereby achieving good anti-aging effect.
The invention adopts the following technical scheme for solving the technical problems:
an anti-aging composition comprising the following components: dipotassium glycyrrhizinate, sucrose stearate, vitamin E, fucoidin, rhizoma Polygonati extract and crocus sativus extract.
Preferably, the anti-aging composition further comprises sodium hyaluronate, glycerin, 1, 3-butanediol and deionized water.
Preferably, the anti-aging composition comprises the following components in parts by weight: 0.05-0.3 part of dipotassium glycyrrhizinate, 0.2-0.6 part of sodium hyaluronate, 0.4-1 part of sucrose stearate, 1-3 parts of vitamin E, 1-5 parts of fucoidin, 2-5 parts of rhizoma polygonati extract, 3-7 parts of crocus sativus extract, 5-10 parts of glycerol, 4-12 parts of 1, 3-butanediol and 50-70 parts of deionized water.
The inventor of the invention finds in a large number of researches that in the formula, good anti-aging, moisturizing and anti-inflammatory effects can be achieved by using dipotassium glycyrrhizinate, sodium hyaluronate, sucrose stearate, vitamin E and fucoidin as basic anti-aging, moisturizing and anti-inflammatory components, and the anti-aging effect can be effectively improved by adding the active components of rhizoma polygonati extract and crocus sativus extract on the basis.
Preferably, the anti-aging composition comprises the following components in parts by weight: 0.1-0.3 part of dipotassium glycyrrhizinate, 0.2-0.5 part of sodium hyaluronate, 0.4-0.8 part of sucrose stearate, 1-2.5 parts of vitamin E, 1-3 parts of fucoidin, 3-5 parts of rhizoma polygonati extract, 4-7 parts of crocus sativus extract, 6-10 parts of glycerol, 7-12 parts of 1, 3-butanediol and 60-70 parts of deionized water.
Preferably, the anti-aging composition comprises the following components in parts by weight: 0.2 part of dipotassium glycyrrhizinate, 0.4 part of sodium hyaluronate, 0.5 part of sucrose stearate, 2 parts of vitamin E, 2.5 parts of fucoidin, 4 parts of rhizoma polygonati extract, 5 parts of crocus sativus extract, 8 parts of glycerol, 10 parts of 1, 3-butanediol and 67.4 parts of deionized water.
Preferably, the preparation method of the crocus sativus extract comprises the following steps:
s1, cleaning crocus sativus, drying, and crushing to 20-100 meshes to obtain crocus sativus powder;
s2, adding crocus sativus powder into the enzymolysis liquid, heating to 55-70 ℃, and keeping for 1-4 hours to obtain a mixed liquid;
s3, centrifuging the mixed solution, taking supernate, and carrying out ultrafiltration on the supernate to obtain filtrate;
s4, adding the filtrate into deionized water, dispersing uniformly to obtain a sample loading solution, loading the sample loading solution onto D101 macroporous adsorption resin at a speed of 0.8-1.5 BV/H by using 0.6-1.2 BV/H, washing by using deionized water at a speed of 0.8-2 BV, washing by using 50-80 wt% of ethanol solution at a speed of 0.8-2 BV, collecting ethanol solution eluent, and drying to obtain the crocus sativus extract.
The inventor of the invention finds that the crocus extract which can obviously improve the free radical scavenging and anti-aging effects is obtained by cleaning, drying, crushing, enzymolysis, centrifugation, filtration and macroporous adsorption resin treatment of crocus.
The enzymolysis step adopts enzymolysis liquid consisting of cetyl trimethyl ammonium bromide, trypsin, papain, phosphate buffer solution and deionized water, can fully crush saffron cells, can better extract substances in saffron, and enables components for removing free radicals in the saffron to be dissolved out.
The macroporous adsorption resin treatment can effectively enrich the components with the effect of removing free radicals in the crocus sativus extract, and other components without the effect of removing the free radicals are eluted in the process.
Preferably, the ultrafiltration is an ultrafiltration membrane with the molecular weight cutoff of 50-100 KD.
Preferably, the weight ratio of the safflower powder to the enzymolysis liquid is 1: 2-6;
the enzymolysis liquid is prepared from 1-5 parts by weight of hexadecyl trimethyl ammonium bromide, 1-8 parts by weight of trypsin, 2-10 parts by weight of papain, 20-40 parts by weight of phosphate buffer and 40-80 parts by weight of deionized water.
Preferably, the preparation method of the polygonatum sibiricum extract comprises the following steps:
s11, drying rhizoma polygonati, and crushing to 20-100 meshes to obtain rhizoma polygonati powder;
s12, adding rhizoma polygonati powder into a 60-80% ethanol solution, performing reflux extraction for 2-4 times, extracting for 1-3 h each time, and combining to obtain an extracting solution, wherein the weight ratio of the rhizoma polygonati powder to the ethanol solution is 1: 3-8;
s13, adding the extracting solution into deionized water to obtain a sample loading solution, loading the sample loading solution onto AB-8 macroporous adsorption resin at a rate of 0.6-1.2 BV/H, washing with deionized water at a rate of 0.5-1.2 BV/H and 30-60 wt% ethanol solution at a rate of 0.5-2 BV, collecting ethanol solution eluent, and drying to obtain the sealwort extract.
The sealwort extract with good free radical scavenging effect is prepared by drying, crushing, ethanol extraction and macroporous adsorption resin application, and compared with the commercially available sealwort extract, the sealwort extract has better free radical scavenging effect.
The inventor finds that the crocus sativus extract and the polygonatum sibiricum extract prepared by the invention have remarkable synergistic effect in the aspect of scavenging free radicals.
The invention also provides a preparation method of the anti-aging composition, which is used for preparing the anti-aging composition and comprises the following steps: adding dipotassium glycyrrhizinate, sodium hyaluronate, sucrose stearate, vitamin E, fucoidin, glycerol and 1, 3-butanediol into deionized water, heating to 65-85 ℃, uniformly stirring, cooling to 35-45 ℃, adding a polygonatum sibiricum extract and a crocus sativus extract, and uniformly stirring to obtain the anti-aging composition.
The invention has the beneficial effects that: the anti-aging extract can effectively remove free radicals, so that a good anti-aging effect is achieved, the anti-aging, moisturizing and anti-inflammatory components based on dipotassium glycyrrhizinate, sodium hyaluronate, sucrose stearate, vitamin E and fucoidin are used for achieving the good anti-aging, moisturizing and anti-inflammatory effects, and the active components of the polygonatum extract and the crocus sativus extract are added on the basis, so that the anti-aging effect can be effectively improved, and the components are natural, non-irritant and have good safety.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the present invention, the parts are all parts by weight unless otherwise specified.
Example 1
An anti-aging composition comprises the following components in parts by weight: 0.2 part of dipotassium glycyrrhizinate, 0.4 part of sodium hyaluronate, 0.5 part of sucrose stearate, 2 parts of vitamin E, 2.5 parts of fucoidin, 4 parts of rhizoma polygonati extract, 5 parts of crocus sativus extract, 8 parts of glycerol, 10 parts of 1, 3-butanediol and 67.4 parts of deionized water.
The anti-aging, moisturizing and anti-inflammatory components based on dipotassium glycyrrhizinate, sodium hyaluronate, sucrose stearate, vitamin E and fucoidin can achieve good anti-aging, moisturizing and anti-inflammatory effects, and the anti-aging effect can be effectively improved by adding the active components of the polygonatum extract and the crocus sativus extract on the basis.
The preparation method of the crocus sativus extract comprises the following steps:
s1, cleaning crocus sativus, drying, and crushing to 50 meshes to obtain crocus sativus powder;
s2, adding crocus powder into the enzymolysis liquid, heating to 65 ℃ and keeping for 2h to obtain a mixed liquid; the weight ratio of the safflower powder to the enzymolysis liquid is 1: 4; the enzymolysis solution is prepared from 2 parts by weight of hexadecyl trimethyl ammonium bromide, 5 parts by weight of trypsin, 8 parts by weight of papain, 25 parts by weight of phosphate buffer (the pH value is 6.5) and 60 parts by weight of deionized water;
s3, centrifuging the mixed solution at 5000rpm for 10min, taking supernatant, and ultrafiltering the supernatant by using an ultrafiltration membrane with the molecular weight cutoff of 100KD to obtain filtrate;
s4, adding the filtrate into deionized water (the weight ratio of the filtrate to the deionized water is 1: 4), dispersing uniformly to obtain a sample liquid, loading the sample liquid on a D101 macroporous adsorption resin at the rate of 1BV/H, washing the sample liquid with deionized water for 1BV, washing the sample liquid with 70 wt% ethanol solution for 1.5BV, collecting ethanol solution eluent, and drying to obtain the crocus sativus extract.
The crocus extract which can obviously improve the free radical scavenging and the anti-aging performance is obtained by cleaning, drying, crushing, enzymolysis, centrifugation, filtration and macroporous adsorption resin.
The enzymolysis step adopts enzymolysis liquid consisting of cetyl trimethyl ammonium bromide, trypsin, papain, phosphate buffer solution and deionized water, so that crocus cells can be fully crushed, substances in crocus can be better extracted, and components for removing free radicals in crocus are dissolved out.
The macroporous adsorption resin treatment can effectively enrich the components with the effect of removing free radicals in the crocus sativus extract, and other components without the effect of removing the free radicals are eluted in the process.
The preparation method of the sealwort extract comprises the following steps:
s11, drying rhizoma Polygonati, and pulverizing to 80 mesh to obtain rhizoma Polygonati powder;
s12, adding rhizoma polygonati powder into a 70% ethanol solution, performing reflux extraction for 3 times, extracting for 2 hours each time, and mixing to obtain an extracting solution, wherein the weight ratio of the rhizoma polygonati powder to the ethanol solution is 1: 5;
s13, adding the extracting solution into deionized water (the weight ratio of the extracting solution to the deionized water is 1: 4) to obtain a sample solution, loading the sample solution on AB-8 macroporous adsorption resin at the rate of 1BV/H, washing the sample solution with deionized water for 1.2BV, washing the sample solution with 50 wt% of ethanol solution for 1.5BV, collecting the ethanol solution eluent, and drying to obtain the sealwort extract.
The sealwort extract with good free radical scavenging effect is prepared by drying, crushing, ethanol extraction and macroporous adsorption resin.
The preparation method of the anti-aging composition comprises the following steps: adding dipotassium glycyrrhizinate, sodium hyaluronate, sucrose stearate, vitamin E, fucoidin, glycerol and 1, 3-butanediol into deionized water, heating to 80 ℃, uniformly stirring, cooling to 40 ℃, adding the sealwort extract and the crocus sativus extract, and uniformly stirring to obtain the anti-aging composition.
Example 2
An anti-aging composition comprises the following components in parts by weight: 0.05 part of dipotassium glycyrrhizinate, 0.6 part of sodium hyaluronate, 0.4 part of sucrose stearate, 3 parts of vitamin E, 1 part of fucoidin, 5 parts of rhizoma polygonati extract, 3 parts of crocus sativus extract, 5 parts of glycerol, 12 parts of 1, 3-butanediol and 69.95 parts of deionized water.
The preparation method of the crocus sativus extract comprises the following steps:
s1, cleaning crocus sativus, drying, and crushing to 80 meshes to obtain crocus sativus powder;
s2, adding crocus powder into the enzymolysis liquid, heating to 60 ℃ and keeping for 3h to obtain a mixed liquid; the weight ratio of the safflower powder to the enzymolysis liquid is 1: 5, preparing the enzymolysis solution by 4 parts by weight of hexadecyl trimethyl ammonium bromide, 3 parts by weight of trypsin, 5 parts by weight of papain, 20 parts by weight of phosphate buffer solution and 68 parts by weight of deionized water;
s3, centrifuging the mixed solution at 5000rpm for 10min, taking supernatant, and ultrafiltering the supernatant by using an ultrafiltration membrane with the molecular weight cutoff of 100KD to obtain filtrate;
s4, adding the filtrate into deionized water (the weight ratio of the filtrate to the deionized water is 1: 4), dispersing uniformly to obtain a sample liquid, loading the sample liquid on a D101 macroporous adsorption resin at the rate of 1BV/H, washing the sample liquid with deionized water for 1BV, washing the sample liquid with 70 wt% ethanol solution for 1.5BV, collecting ethanol solution eluent, and drying to obtain the crocus sativus extract.
The preparation method of the sealwort extract comprises the following steps:
s11, drying rhizoma Polygonati, and pulverizing to 50 mesh to obtain rhizoma Polygonati powder;
s12, adding rhizoma polygonati powder into a 70% ethanol solution, performing reflux extraction for 3 times, extracting for 2 hours each time, and mixing to obtain an extracting solution, wherein the weight ratio of the rhizoma polygonati powder to the ethanol solution is 1: 5;
s13, adding the extracting solution into deionized water (the weight ratio of the extracting solution to the deionized water is 1: 4) to obtain a sample solution, loading the sample solution on AB-8 macroporous adsorption resin at the rate of 1BV/H, washing the sample solution with deionized water for 1.2BV, washing the sample solution with 50 wt% of ethanol solution for 1.5BV, collecting the ethanol solution eluent, and drying to obtain the sealwort extract.
The preparation method of the anti-aging composition comprises the following steps: adding dipotassium glycyrrhizinate, sodium hyaluronate, sucrose stearate, vitamin E, fucoidin, glycerol and 1, 3-butanediol into deionized water, heating to 80 ℃, uniformly stirring, cooling to 40 ℃, adding the sealwort extract and the crocus sativus extract, and uniformly stirring to obtain the anti-aging composition.
Example 3
An anti-aging composition comprises the following components in parts by weight: 0.3 part of dipotassium glycyrrhizinate, 0.2 part of sodium hyaluronate, 1 part of sucrose stearate, 1 part of vitamin E, 5 parts of fucoidin, 2 parts of rhizoma polygonati extract, 6 parts of crocus sativus extract, 10 parts of glycerol, 6 parts of 1, 3-butanediol and 68.5 parts of deionized water.
The preparation method of the crocus sativus extract comprises the following steps:
s1, cleaning crocus sativus, drying, and crushing to 60 meshes to obtain crocus sativus powder;
s2, adding crocus powder into the enzymolysis liquid, heating to 65 ℃ and keeping for 3h to obtain a mixed liquid; the weight ratio of the safflower powder to the enzymolysis liquid is 1: 4; the enzymolysis solution is prepared from 1 part by weight of hexadecyl trimethyl ammonium bromide, 8 parts by weight of trypsin, 2 parts by weight of papain, 40 parts by weight of phosphate buffer (the pH value is 6.5) and 49 parts by weight of deionized water;
s3, centrifuging the mixed solution at 5000rpm for 10min, taking supernatant, and ultrafiltering the supernatant by using an ultrafiltration membrane with the molecular weight cutoff of 100KD to obtain filtrate;
s4, adding the filtrate into deionized water (the weight ratio of the filtrate to the deionized water is 1: 4), dispersing uniformly to obtain a sample liquid, loading the sample liquid on a D101 macroporous adsorption resin at the rate of 1BV/H, washing the sample liquid with deionized water for 1BV, washing the sample liquid with 70 wt% ethanol solution for 1.5BV, collecting ethanol solution eluent, and drying to obtain the crocus sativus extract.
The preparation method of the sealwort extract comprises the following steps:
s11, drying rhizoma Polygonati, and pulverizing to 80 mesh to obtain rhizoma Polygonati powder;
s12, adding rhizoma polygonati powder into a 65% ethanol solution, extracting for 3 times under reflux, extracting for 2 hours each time, and mixing to obtain an extracting solution, wherein the weight ratio of the rhizoma polygonati powder to the ethanol solution is 1: 5;
s13, adding the extracting solution into deionized water (the weight ratio of the extracting solution to the deionized water is 1: 4) to obtain a sample solution, loading the sample solution on AB-8 macroporous adsorption resin at the rate of 1BV/H, washing the sample solution with deionized water for 1.2BV, washing the sample solution with 50 wt% of ethanol solution for 1.5BV, collecting the ethanol solution eluent, and drying to obtain the sealwort extract.
The preparation method of the anti-aging composition comprises the following steps: adding dipotassium glycyrrhizinate, sodium hyaluronate, sucrose stearate, vitamin E, fucoidin, glycerol and 1, 3-butanediol into deionized water, heating to 80 ℃, uniformly stirring, cooling to 40 ℃, adding the sealwort extract and the crocus sativus extract, and uniformly stirring to obtain the anti-aging composition.
Comparative example 1
Comparative example 1 is different from example 1 in that comparative example 1 replaces the polygonatum sibiricum extract with the same amount of saffron extract, and the rest is the same.
An anti-aging composition comprises the following components in parts by weight: 0.2 part of dipotassium glycyrrhizinate, 0.4 part of sodium hyaluronate, 0.5 part of sucrose stearate, 2 parts of vitamin E, 2.5 parts of fucoidin, 9 parts of crocus sativus extract, 8 parts of glycerol, 10 parts of 1, 3-butanediol and 67.4 parts of deionized water.
Comparative example 2
Comparative example 2 is different from example 1 in that comparative example 2 replaces the saffron extract with an equal amount of polygonatum extract, all the others being the same.
An anti-aging composition comprises the following components in parts by weight: 0.2 part of dipotassium glycyrrhizinate, 0.4 part of sodium hyaluronate, 0.5 part of sucrose stearate, 2 parts of vitamin E, 2.5 parts of fucoidin, 9 parts of sealwort extract, 8 parts of glycerol, 10 parts of 1, 3-butanediol and 67.4 parts of deionized water.
Comparative example 3
Comparative example 3 is different from example 1 in that the crocus sativus extract of comparative example 3 is prepared by the same method as example 1.
In the preparation method of the saffron extract, the cetyl trimethyl ammonium bromide, the trypsin and the papain are replaced by the same amount of cellulase
The preparation method of the crocus sativus extract comprises the following steps:
s1, cleaning crocus sativus, drying, and crushing to 50 meshes to obtain crocus sativus powder;
s2, adding crocus powder into the enzymolysis liquid, heating to 65 ℃ and keeping for 2h to obtain a mixed liquid; the weight ratio of the safflower powder to the enzymolysis liquid is 1: 4; the enzymolysis liquid is prepared by 15 parts by weight of cellulase, 25 parts by weight of phosphate buffer (pH is 6.5) and 60 parts by weight of deionized water;
s3, centrifuging the mixed solution at 5000rpm for 10min, taking supernatant, and ultrafiltering the supernatant by using an ultrafiltration membrane with the molecular weight cutoff of 100KD to obtain filtrate;
s4, adding the filtrate into deionized water (the weight ratio of the filtrate to the deionized water is 1: 4), dispersing uniformly to obtain a sample liquid, loading the sample liquid on a D101 macroporous adsorption resin at the rate of 1BV/H, washing the sample liquid with deionized water for 1BV, washing the sample liquid with 70 wt% ethanol solution for 1.5BV, collecting ethanol solution eluent, and drying to obtain the crocus sativus extract.
Comparative example 4
Comparative example 4 is different from example 1 in that comparative example 4 employs a commercially available polygonatum extract instead of the polygonatum extract, and the rest is the same.
The polygonatum sibiricum extract described in comparative example 4 was purchased from sienna corporation, biotechnology limited.
To further demonstrate the effect of the present invention, the following test methods were provided:
1. DPPH-clearance (conventional method): 20mg of DPPH (sigma) was weighed out accurately, the volume was fixed to a 250mL volumetric flask with absolute ethanol to obtain a DPPH solution with a concentration of 20mmol/L, and the compositions prepared in examples 1 to 3 and comparative examples 1 to 4 were diluted with distilled water to obtain test solutions. Respectively taking 2mL of test solution with different concentrations and 2mL of 20mmol/L DPPH solution, mixing uniformly, reacting for 30min, measuring the change of absorbance at the wavelength of 517nm, replacing a contrast solvent with absolute ethyl alcohol, and calculating the clearance according to the following formula.
The clearance (%) {1- [ (a 1-A3)/a 2] } × 100%.
Wherein A1 is the absorbance of a mixture of 2mL DPPH solution and 2mL of a composition of different concentrations; a3 is the absorbance of a mixed solution consisting of 2mL of compositions with different concentrations and 2mL of absolute ethyl alcohol; a2 is the absorbance of a mixture of 2mL of the solution of LDPPH and 2mL of absolute ethanol.
TABLE 1 test results
As can be seen from table 1, the anti-aging composition of the present invention has a good effect of scavenging free radicals, and can achieve a good anti-aging effect.
It can be seen from the comparison of examples 1 to 3 that the ratio of the different raw materials and the preparation parameters of the gold extract and the crocus sativus extract can affect the effect of scavenging free radicals, wherein example 1 is the best mode of execution and has the best effect of scavenging free radicals.
As can be seen from the comparison of example 1 and comparative examples 1-2, the crocus sativus extract and the polygonatum sibiricum extract have a remarkable synergistic effect in the aspect of scavenging free radicals.
As can be seen from comparison of example 1 and comparative example 3, the crocus extract of the present invention has a significant effect of scavenging free radicals, and the crocus extracts prepared by different preparation methods of the crocus extract have different effects of scavenging free radicals, and the crocus extract prepared by the preparation method of the present invention has a better effect of scavenging free radicals than the crocus extracts prepared by other methods.
Comparing example 1 with comparative example 4, it can be seen that the polygonatum sibiricum extract of the present invention can significantly improve the effect of scavenging free radicals, and the polygonatum sibiricum extract prepared by the present invention has better effect of scavenging free radicals than the commercially available polygonatum sibiricum extract.
In light of the foregoing description of preferred embodiments according to the invention, it is clear that many changes and modifications can be made by the person skilled in the art without departing from the scope of the invention. The technical scope of the present invention is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. An anti-aging composition, comprising the following components: dipotassium glycyrrhizinate, sucrose stearate, vitamin E, fucoidin, rhizoma Polygonati extract and crocus sativus extract.
2. The anti-aging composition according to claim 1, further comprising sodium hyaluronate, glycerin, 1, 3-butylene glycol, deionized water.
3. The anti-aging composition according to claim 2, comprising the following components in parts by weight: 0.05-0.3 part of dipotassium glycyrrhizinate, 0.2-0.6 part of sodium hyaluronate, 0.4-1 part of sucrose stearate, 1-3 parts of vitamin E, 1-5 parts of fucoidin, 2-5 parts of rhizoma polygonati extract, 3-7 parts of crocus sativus extract, 5-10 parts of glycerol, 4-12 parts of 1, 3-butanediol and 50-70 parts of deionized water.
4. The anti-aging composition according to claim 3, comprising the following components in parts by weight: 0.1-0.3 part of dipotassium glycyrrhizinate, 0.2-0.5 part of sodium hyaluronate, 0.4-0.8 part of sucrose stearate, 1-2.5 parts of vitamin E, 1-3 parts of fucoidin, 3-5 parts of rhizoma polygonati extract, 4-7 parts of crocus sativus extract, 6-10 parts of glycerol, 7-12 parts of 1, 3-butanediol and 60-70 parts of deionized water.
5. The anti-aging composition according to claim 3, comprising the following components in parts by weight: 0.2 part of dipotassium glycyrrhizinate, 0.4 part of sodium hyaluronate, 0.5 part of sucrose stearate, 2 parts of vitamin E, 2.5 parts of fucoidin, 4 parts of rhizoma polygonati extract, 5 parts of crocus sativus extract, 8 parts of glycerol, 10 parts of 1, 3-butanediol and 67.4 parts of deionized water.
6. The anti-aging composition according to claim 3, wherein the crocus sativus extract is prepared by:
s1, cleaning crocus sativus, drying, and crushing to 20-100 meshes to obtain crocus sativus powder;
s2, adding crocus sativus powder into the enzymolysis liquid, heating to 55-70 ℃, and keeping for 1-4 hours to obtain a mixed liquid;
s3, centrifuging the mixed solution, taking supernate, and carrying out ultrafiltration on the supernate to obtain filtrate;
s4, adding the filtrate into deionized water, dispersing uniformly to obtain a sample loading solution, loading the sample loading solution onto D101 macroporous adsorption resin at a speed of 0.8-1.5 BV/H by using 0.6-1.2 BV/H, washing by using deionized water at a speed of 0.8-2 BV, washing by using 50-80 wt% of ethanol solution at a speed of 0.8-2 BV, collecting ethanol solution eluent, and drying to obtain the crocus sativus extract.
7. The anti-aging composition according to claim 6, wherein the ultrafiltration is an ultrafiltration membrane with a molecular weight cut-off of 50-100 KD.
8. The anti-aging composition according to claim 6, wherein the weight ratio of the saffron powder to the enzymolysis solution is 1: 2-6;
the enzymolysis liquid is prepared from 1-5 parts by weight of hexadecyl trimethyl ammonium bromide, 1-8 parts by weight of trypsin, 2-10 parts by weight of papain, 20-40 parts by weight of phosphate buffer and 40-80 parts by weight of deionized water.
9. The anti-aging composition according to claim 3, wherein the Polygonatum sibiricum extract is prepared by:
s11, drying rhizoma polygonati, and crushing to 20-100 meshes to obtain rhizoma polygonati powder;
s12, adding rhizoma polygonati powder into a 60-80% ethanol solution, performing reflux extraction for 2-4 times, extracting for 1-3 h each time, and combining to obtain an extracting solution, wherein the weight ratio of the rhizoma polygonati powder to the ethanol solution is 1: 3-8;
s13, adding the extracting solution into deionized water to obtain a sample loading solution, loading the sample loading solution onto AB-8 macroporous adsorption resin at a rate of 0.6-1.2 BV/H, washing with deionized water at a rate of 0.5-1.2 BV/H and 30-60 wt% ethanol solution at a rate of 0.5-2 BV, collecting ethanol solution eluent, and drying to obtain the sealwort extract.
10. A method for preparing an anti-aging composition according to any one of claims 1 to 9, comprising the steps of: adding dipotassium glycyrrhizinate, sodium hyaluronate, sucrose stearate, vitamin E, fucoidin, glycerol and 1, 3-butanediol into deionized water, heating to 65-85 ℃, uniformly stirring, cooling to 35-45 ℃, adding a polygonatum sibiricum extract and a crocus sativus extract, and uniformly stirring to obtain the anti-aging composition.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111620612.7A CN114306112B (en) | 2021-12-28 | 2021-12-28 | Anti-aging composition and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111620612.7A CN114306112B (en) | 2021-12-28 | 2021-12-28 | Anti-aging composition and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN114306112A true CN114306112A (en) | 2022-04-12 |
CN114306112B CN114306112B (en) | 2024-02-20 |
Family
ID=81014859
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202111620612.7A Active CN114306112B (en) | 2021-12-28 | 2021-12-28 | Anti-aging composition and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114306112B (en) |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102258638A (en) * | 2011-08-17 | 2011-11-30 | 林煌权 | Anti-aging plant extract composition and preparation method and application thereof |
KR20150002048A (en) * | 2013-06-28 | 2015-01-07 | 주식회사 코스메카코리아 | A composition for preventing wrinkle of skin and anti aging of skin |
CN107019653A (en) * | 2017-03-21 | 2017-08-08 | 广州雅纯化妆品制造有限公司 | A kind of anti-apolexis composition and preparation method thereof |
CN107913218A (en) * | 2017-11-20 | 2018-04-17 | 艾因特丽(苏州)生物科技有限公司 | A kind of compound elite preparation with senile-resistant efficacy and its preparation method and application |
CN110384622A (en) * | 2019-07-10 | 2019-10-29 | 青岛明月海藻生物健康科技集团有限公司 | A kind of seaweed moisturizing maintenance gel and preparation method thereof |
CN111329808A (en) * | 2020-04-03 | 2020-06-26 | 西安力邦医美科技有限公司 | Cosmetic composition with anti-glycosylation and anti-aging effects and application thereof |
CN112741789A (en) * | 2020-12-24 | 2021-05-04 | 广州尚品生物科技有限公司 | Anti-aging composition, preparation method and application |
CN113509422A (en) * | 2021-08-30 | 2021-10-19 | 苏湘怡 | Whitening, moisturizing and freckle removing cosmetic composition and preparation method thereof |
-
2021
- 2021-12-28 CN CN202111620612.7A patent/CN114306112B/en active Active
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102258638A (en) * | 2011-08-17 | 2011-11-30 | 林煌权 | Anti-aging plant extract composition and preparation method and application thereof |
KR20150002048A (en) * | 2013-06-28 | 2015-01-07 | 주식회사 코스메카코리아 | A composition for preventing wrinkle of skin and anti aging of skin |
CN107019653A (en) * | 2017-03-21 | 2017-08-08 | 广州雅纯化妆品制造有限公司 | A kind of anti-apolexis composition and preparation method thereof |
CN107913218A (en) * | 2017-11-20 | 2018-04-17 | 艾因特丽(苏州)生物科技有限公司 | A kind of compound elite preparation with senile-resistant efficacy and its preparation method and application |
CN110384622A (en) * | 2019-07-10 | 2019-10-29 | 青岛明月海藻生物健康科技集团有限公司 | A kind of seaweed moisturizing maintenance gel and preparation method thereof |
CN111329808A (en) * | 2020-04-03 | 2020-06-26 | 西安力邦医美科技有限公司 | Cosmetic composition with anti-glycosylation and anti-aging effects and application thereof |
CN112741789A (en) * | 2020-12-24 | 2021-05-04 | 广州尚品生物科技有限公司 | Anti-aging composition, preparation method and application |
CN113509422A (en) * | 2021-08-30 | 2021-10-19 | 苏湘怡 | Whitening, moisturizing and freckle removing cosmetic composition and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
CN114306112B (en) | 2024-02-20 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106955250B (en) | Method for preparing facial mask by using grape vinasse and facial mask obtained by method | |
CN110747234B (en) | Preparation method of sophora flower extract | |
CN106265254A (en) | The Tricholoma matsutake (lto et lmai) Singer extract and its preparation method and application of skin can be repaired by whitening skin and preserving moisture | |
Chen et al. | Preparation, characterization and anti-ageing activity of Gastrodia elata blume polysaccharide | |
CN107320357B (en) | Cosmetic containing polysaccharide | |
CN114306112A (en) | Anti-aging composition and preparation method thereof | |
CN110859788B (en) | Tanaka composition and preparation method and application thereof | |
CN115531430B (en) | Ginseng extract or ginseng extract, preparation method and application thereof | |
CN115414313B (en) | Anti-aging composition containing micrococcus lysate and preparation method thereof | |
CN111643392A (en) | Biological oligopeptide essence with multiple-effect whitening and anti-allergy effects and preparation method thereof | |
CN114591450B (en) | Pleurotus citrinopileatus polysaccharide PCP-3 with anti-photoaging effect, and preparation method and application thereof | |
CN106008618A (en) | Preparation method of salidroside | |
CN115677873A (en) | Tremella polysaccharide and application thereof in preparation of anti-aging composition | |
CN113208944A (en) | Skin care composition and skin care product with moisturizing effect | |
CN115505612A (en) | Ulva polysaccharide and preparation method and application thereof | |
CN112656829B (en) | Method for simultaneously extracting notoginsenoside, notoginsenones and notoginsen polysaccharide and application thereof | |
CN115531232A (en) | Preparation method and application of rose composite fermentation liquor rich in ellagic acid | |
CN115414289A (en) | Cordyceps flower cosmetics and preparation method thereof | |
CN106986950A (en) | A kind of method for integrated extraction of GL-B | |
CN107334671A (en) | A kind of skin-moisturizing, skin water containing pittosporum tobira flower essential oil and Honegsukle flower P.E | |
CN114028289A (en) | Preparation method and application of platycodon grandiflorum extract with relieving effect | |
CN113520888A (en) | Anti-aging composition containing fullerene and preparation method and application thereof | |
CN116693711B (en) | Polygonum multiflorum polysaccharide, extraction method and application thereof | |
CN115531259B (en) | Plant composition and preparation method and application thereof | |
CN103565698A (en) | Alpinia speciosa extract with anti-aging activity as well as preparation method and application of alpinia speciosa extract |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |