CN113648232B - Stable composition carrying urea or derivatives thereof - Google Patents
Stable composition carrying urea or derivatives thereof Download PDFInfo
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- CN113648232B CN113648232B CN202110956699.9A CN202110956699A CN113648232B CN 113648232 B CN113648232 B CN 113648232B CN 202110956699 A CN202110956699 A CN 202110956699A CN 113648232 B CN113648232 B CN 113648232B
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- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 271
- 239000004202 carbamide Substances 0.000 title claims abstract description 261
- 239000000203 mixture Substances 0.000 title claims abstract description 136
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 40
- 125000002091 cationic group Chemical group 0.000 claims abstract description 31
- 239000004519 grease Substances 0.000 claims abstract description 31
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 25
- 239000008346 aqueous phase Substances 0.000 claims abstract description 13
- 150000003672 ureas Chemical class 0.000 claims abstract description 13
- REZZEXDLIUJMMS-UHFFFAOYSA-M dimethyldioctadecylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC REZZEXDLIUJMMS-UHFFFAOYSA-M 0.000 claims abstract description 11
- 239000004664 distearyldimethylammonium chloride (DHTDMAC) Substances 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 24
- NOPFSRXAKWQILS-UHFFFAOYSA-N docosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCO NOPFSRXAKWQILS-UHFFFAOYSA-N 0.000 claims description 22
- OULAJFUGPPVRBK-UHFFFAOYSA-N tetratriacontyl alcohol Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCO OULAJFUGPPVRBK-UHFFFAOYSA-N 0.000 claims description 22
- 229940082500 cetostearyl alcohol Drugs 0.000 claims description 18
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 18
- 229960000735 docosanol Drugs 0.000 claims description 11
- 229960000541 cetyl alcohol Drugs 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- BTFJIXJJCSYFAL-UHFFFAOYSA-N icosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCO BTFJIXJJCSYFAL-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 claims description 3
- 229940012831 stearyl alcohol Drugs 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 description 69
- 230000000087 stabilizing effect Effects 0.000 description 42
- 239000002537 cosmetic Substances 0.000 description 41
- 239000000839 emulsion Substances 0.000 description 41
- 239000012071 phase Substances 0.000 description 41
- 238000012360 testing method Methods 0.000 description 40
- 230000001804 emulsifying effect Effects 0.000 description 38
- 230000002829 reductive effect Effects 0.000 description 36
- 210000003491 skin Anatomy 0.000 description 35
- 230000003247 decreasing effect Effects 0.000 description 32
- 238000007792 addition Methods 0.000 description 29
- 239000003921 oil Substances 0.000 description 28
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 26
- 238000013329 compounding Methods 0.000 description 26
- 238000009472 formulation Methods 0.000 description 26
- 238000013112 stability test Methods 0.000 description 26
- 239000003093 cationic surfactant Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 21
- 238000002360 preparation method Methods 0.000 description 21
- 230000000694 effects Effects 0.000 description 19
- 239000002562 thickening agent Substances 0.000 description 18
- 239000003871 white petrolatum Substances 0.000 description 18
- 239000004094 surface-active agent Substances 0.000 description 14
- 239000004471 Glycine Substances 0.000 description 13
- DOOTYTYQINUNNV-UHFFFAOYSA-N Triethyl citrate Chemical compound CCOC(=O)CC(O)(C(=O)OCC)CC(=O)OCC DOOTYTYQINUNNV-UHFFFAOYSA-N 0.000 description 13
- 239000001069 triethyl citrate Substances 0.000 description 13
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 description 13
- 235000013769 triethyl citrate Nutrition 0.000 description 13
- 229920000642 polymer Polymers 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 230000032798 delamination Effects 0.000 description 10
- 238000004945 emulsification Methods 0.000 description 9
- 239000000693 micelle Substances 0.000 description 9
- 229920002553 poly(2-methacrylolyloxyethyltrimethylammonium chloride) polymer Polymers 0.000 description 9
- 239000000725 suspension Substances 0.000 description 9
- ARIWANIATODDMH-UHFFFAOYSA-N Lauric acid monoglyceride Natural products CCCCCCCCCCCC(=O)OCC(O)CO ARIWANIATODDMH-UHFFFAOYSA-N 0.000 description 8
- 239000004698 Polyethylene Substances 0.000 description 8
- 239000003925 fat Substances 0.000 description 8
- 238000000265 homogenisation Methods 0.000 description 8
- -1 zinc salts Chemical class 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 229920000223 polyglycerol Polymers 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 6
- 239000006071 cream Substances 0.000 description 6
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 description 6
- 230000003020 moisturizing effect Effects 0.000 description 6
- 235000014593 oils and fats Nutrition 0.000 description 6
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 6
- 229940083037 simethicone Drugs 0.000 description 6
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 6
- AMUTYVGRCVFCCD-UHFFFAOYSA-N 5,6-diaminopyridine-3-carboxylic acid Chemical compound NC1=CC(C(O)=O)=CN=C1N AMUTYVGRCVFCCD-UHFFFAOYSA-N 0.000 description 5
- 230000001174 ascending effect Effects 0.000 description 5
- 230000014509 gene expression Effects 0.000 description 5
- PXDJXZJSCPSGGI-UHFFFAOYSA-N hexadecanoic acid hexadecyl ester Natural products CCCCCCCCCCCCCCCCOC(=O)CCCCCCCCCCCCCCC PXDJXZJSCPSGGI-UHFFFAOYSA-N 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 235000019271 petrolatum Nutrition 0.000 description 5
- 239000000230 xanthan gum Substances 0.000 description 5
- 229920001285 xanthan gum Polymers 0.000 description 5
- 229940082509 xanthan gum Drugs 0.000 description 5
- 235000010493 xanthan gum Nutrition 0.000 description 5
- CLAHOZSYMRNIPY-UHFFFAOYSA-N 2-hydroxyethylurea Chemical group NC(=O)NCCO CLAHOZSYMRNIPY-UHFFFAOYSA-N 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000002552 dosage form Substances 0.000 description 4
- 230000037336 dry skin Effects 0.000 description 4
- 210000002615 epidermis Anatomy 0.000 description 4
- 230000001815 facial effect Effects 0.000 description 4
- 229940031575 hydroxyethyl urea Drugs 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 230000008591 skin barrier function Effects 0.000 description 4
- 235000010956 sodium stearoyl-2-lactylate Nutrition 0.000 description 4
- KNYAZNABVSEZDS-UHFFFAOYSA-M sodium;2-octadecanoyloxypropanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC(=O)OC(C)C([O-])=O KNYAZNABVSEZDS-UHFFFAOYSA-M 0.000 description 4
- 238000012430 stability testing Methods 0.000 description 4
- FLPJVCMIKUWSDR-UHFFFAOYSA-N 2-(4-formylphenoxy)acetamide Chemical compound NC(=O)COC1=CC=C(C=O)C=C1 FLPJVCMIKUWSDR-UHFFFAOYSA-N 0.000 description 3
- 125000000129 anionic group Chemical group 0.000 description 3
- 229940074979 cetyl palmitate Drugs 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 235000002316 solid fats Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000036962 time dependent Effects 0.000 description 3
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- WHMDKBIGKVEYHS-IYEMJOQQSA-L Zinc gluconate Chemical compound [Zn+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O WHMDKBIGKVEYHS-IYEMJOQQSA-L 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 201000008937 atopic dermatitis Diseases 0.000 description 2
- 208000010668 atopic eczema Diseases 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000008131 herbal destillate Substances 0.000 description 2
- 229940127554 medical product Drugs 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 230000003389 potentiating effect Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 229960000306 zinc gluconate Drugs 0.000 description 2
- 235000011478 zinc gluconate Nutrition 0.000 description 2
- 239000011670 zinc gluconate Substances 0.000 description 2
- ODNJVAVDJKOYFK-GRVYQHKQSA-L zinc;(9z,12z)-octadeca-9,12-dienoate Chemical compound [Zn+2].CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O.CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O ODNJVAVDJKOYFK-GRVYQHKQSA-L 0.000 description 2
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 1
- XYTHHAXRVHHXKO-JIUYZRCGSA-N 18-[(2r,3s,4r,5r)-4,5-dihydroxy-2-(hydroxymethyl)-6-methoxyoxan-3-yl]oxyoctadecanoic acid;ethanol Chemical compound CCO.COC1O[C@H](CO)[C@@H](OCCCCCCCCCCCCCCCCCC(O)=O)[C@H](O)[C@H]1O XYTHHAXRVHHXKO-JIUYZRCGSA-N 0.000 description 1
- 101710125298 Beta-defensin 2 Proteins 0.000 description 1
- 102100038326 Beta-defensin 4A Human genes 0.000 description 1
- 101710176951 Beta-defensin 4A Proteins 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 229920000832 Cutin Polymers 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 206010012434 Dermatitis allergic Diseases 0.000 description 1
- 206010012438 Dermatitis atopic Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 201000004681 Psoriasis Diseases 0.000 description 1
- 206010039793 Seborrhoeic dermatitis Diseases 0.000 description 1
- 206010051788 Sticky skin Diseases 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000008365 aqueous carrier Substances 0.000 description 1
- BQMNFPBUAQPINY-UHFFFAOYSA-N azane;2-methyl-2-(prop-2-enoylamino)propane-1-sulfonic acid Chemical compound [NH4+].[O-]S(=O)(=O)CC(C)(C)NC(=O)C=C BQMNFPBUAQPINY-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229940126214 compound 3 Drugs 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 230000012969 defense response to bacterium Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- GWTCIAGIKURVBJ-UHFFFAOYSA-L dipotassium;dodecyl phosphate Chemical compound [K+].[K+].CCCCCCCCCCCCOP([O-])([O-])=O GWTCIAGIKURVBJ-UHFFFAOYSA-L 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229910001651 emery Inorganic materials 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000009004 jinqing Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000005339 levitation Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000010534 mechanism of action 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
- 229940105132 myristate Drugs 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 231100000435 percutaneous penetration Toxicity 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 208000008742 seborrheic dermatitis Diseases 0.000 description 1
- 208000017520 skin disease Diseases 0.000 description 1
- 230000037394 skin elasticity Effects 0.000 description 1
- 230000036555 skin type Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- TUNFSRHWOTWDNC-UHFFFAOYSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/42—Amides
-
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/31—Hydrocarbons
-
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/342—Alcohols having more than seven atoms in an unbroken chain
-
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
-
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/41—Amines
- A61K8/416—Quaternary ammonium compounds
-
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
-
- 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
-
- 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
-
- 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
- A61Q19/007—Preparations for dry skin
-
- 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
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
Abstract
The present invention provides a stable composition for carrying urea or a derivative thereof, said composition comprising: (a) a grease; (b) A cationic emulsifier which is distearyl dimethyl ammonium chloride; (c) A long chain fatty alcohol having a carbon chain length of 16-22; (d) an aqueous phase; wherein the urea derivative is a hydroxyalkanoate of urea having 1-6 carbon atoms, wherein the weight ratio of the cationic emulsifier to the long chain fatty alcohol is 10:1 to 1:4, and the weight ratio of the cationic emulsifier to the supported urea or derivative thereof is 1:10 to 50:1.
Description
Technical Field
The invention relates to the field of cosmetics, in particular to a stable composition for bearing urea or derivatives thereof and application of the stable composition in cosmetics.
Background
Urea is one of the natural moisturizing factors of skin, and its effects of moisturizing, softening skin, promoting transdermal penetration, etc. have been widely reported in the literature. Literature "instrument and dermatologist evaluate the effect of glycerin and urea on dry skin of atopic dermatitis patients", skin study and technique, loden m, et al reported that the average value of skin capacitance values of 35 subjects after 30 days using moisturizing cream containing 4% urea increased from 35a.u. to 42a.u. (the higher the water content of the skin surface layer, the higher the capacitance value), the average value of skin moisture loss amount was from about 11 g/(m) 2 H) decrease to 8.5 g/(m) 2 H), the average value of the total dryness fraction is reduced from 3.2 to 0.8, the experimental results are obviously superior to those of a control group without urea, and the effects of moisturizing, softening and strengthening skin barrier of urea are proved by the statistical difference. The literature "effect of urea on human epidermis, skin", hellgren et al report that immersing dried epidermis in a 10% urea solution, after 90 hours of substantial equilibration, the water absorption of the epidermis approachesThe initial mass was 300% and the water absorption was approximately 3 times that of the sample immersed in distilled water. The increase in the water absorption of the dry skin results from the aqueous urea solution increasing the permeability of the epidermis. The literature "new effect of transdermal penetration enhancers on the percutaneous penetration of two zinc salts", science Technology and Engineering,2016;16:1671-1815 Chen Chuanxiu, jinqing, tan Ranran, the subject group studied the effect of urea on transdermal permeation of conjugated zinc linoleate and zinc gluconate, found that the cumulative permeation per unit time of conjugated zinc linoleate was 188.23 μg/cm by adding 2% urea to the stock 2 Rises to 388.04 mug/cm 2 The cumulative permeation per unit time of zinc gluconate is 682.26 mug/cm 2 Rises to 1020.49 mug/cm 2 And the permeation rate is still further improved with the increase of the urea content.
Recent studies have revealed more in depth the efficacy of urea in caring for the skin. For example, the literature "urea uptake enhances human barrier function and antibacterial defense by regulating epidermal gene expression", journal of dermatological research Susanne g. -b., (2012) 132,1561-1572 reports that urea can enhance the expression of skin barrier-related genes AMP, LL-37 and β -defensin-2, and detailed studies on the mechanism of action of urea to regulate gene expression, enhance skin barrier and antibacterial activity have been made. According to the results of the study, the authors believe that urea is not only a metabolite of the body but also acts as a regulator of small molecules with the effect of modifying the expression of genes associated with the skin barrier. Furthermore, urea and skin: a famous molecular review summarizes urea as a medicine for treating skin diseases such as psoriasis, allergic dermatitis, eczema, seborrheic dermatitis and the like.
However, the practical use of urea with potent skin care efficacy in cosmetics or dermatological products presents a number of challenges. One of them is that urea hydrolysis produces stronger alkalinity and ionization, and has high requirements on the bearing capacity of the cosmetic formula matrix. For example, 12 Shanghai household United states Co., ltd were found after testing of the sold emulsion formulations (viscosity 1000 mPas to 20000 mPas, each formulation using different emulsifiers and thickeners), wherein 11 formulations were significantly reduced in viscosity during the high temperature stability test after compounding the urea and urea+glycine+triethyl citrate compositions, and had stability problems such as delamination, demulsification, etc., which could not meet the requirements of national regulations for cosmetic stability. After further testing of the emulsifiers and thickeners involved in the 12 above formulations, it was found that most of the samples were not stable during the high temperature time course of the test after compounding with urea (test example 1).
Because urea has strict requirements on the bearing capacity of a formula system, most of the bearing capacity of the formula sold in cosmetics on the market cannot meet the requirements of compound urea, so that the urea with strong efficacy, good safety and low price has very low use rate in the existing cosmetics products (according to the search result of Mintel based on the global market in 2020, the proportion of cosmetics containing urea is only 2.8%). Furthermore, most of the urea cosmetics added at present are only added in a trace amount to stabilize the pH value of the formulation, and the addition amount is far lower than the urea efficacy addition amount reported in the above documents.
Therefore, the development of a formulation base capable of stably supporting urea or its derivatives, or a composition comprising urea or its derivatives, is of great importance for facilitating the use of urea and its derivatives in cosmetics.
Disclosure of Invention
In one aspect, the present invention provides a stable composition for carrying urea or a derivative thereof, the composition comprising:
(a) Grease;
(b) A cationic emulsifier which is distearyl dimethyl ammonium chloride;
(c) A long chain fatty alcohol having a carbon chain length of 16-22;
(d) An aqueous phase;
wherein the urea derivative is a hydroxyalkanoate with carbon number of 1-6 of urea,
Wherein the weight ratio of the cationic emulsifier to the long chain fatty alcohol is 10:1 to 1:4, and the weight ratio of the cationic emulsifier to the supported urea or derivative thereof is 1:10 to 50:1.
In a preferred embodiment, the grease in the composition is selected from: a non-polar solid fat; a non-polar liquid fat; polar liquid grease; polar solid grease; silicone oil; or mixtures thereof. In a preferred embodiment, the composition comprises 0.1 to 20% by weight of grease.
In a preferred embodiment, the composition comprises 2.5 to 10 wt% cationic surfactant.
In a preferred embodiment, the long chain fatty alcohol in the composition is selected from: cetyl alcohol, cetostearyl alcohol, stearyl alcohol, arachidyl alcohol, behenyl alcohol, or mixtures thereof. In a preferred embodiment, the composition comprises 0.1 to 10% by weight of long chain fatty alcohols.
In a preferred embodiment, the composition comprises more than 1% by weight of urea or a derivative thereof.
In a preferred embodiment, the composition comprises more than 50% by weight of the aqueous phase.
In a preferred embodiment, the weight ratio of cationic emulsifier to long chain fatty alcohol in the composition is from 10:1 to 1:2 and the weight ratio of cationic emulsifier to supported urea or derivative thereof is from 1:2 to 10:1.
In another aspect, the present invention also provides a skin external preparation comprising the stable composition of the present invention.
Detailed Description
The present invention unexpectedly found a stable composition that can carry urea or derivatives thereof and which exhibits abnormal thickening phenomena when tested at Gao Wenjing in a suitable formulation. Therefore, the emulsification technology has high practical value in practical application of cosmetics and skin medical products in the future.
In order to provide a more concise description, some quantitative representations presented herein are not modified by the term "about". It will be understood that each quantity given herein is intended to refer to an actual given value, whether or not the term "about" is explicitly used, and is also intended to refer to approximations of such given values, including approximations of such given values resulting from experimental and/or measurement conditions, as reasonably deduced by one of ordinary skill in the art.
To provide a more concise description, some quantitative expressions herein are recited as a range from about X to about Y. It should be understood that when a range is recited, the range is not limited to the recited upper and lower limits, but rather, includes the entire range of about X to about Y amounts or any amount therebetween.
Urea
Urea is one of the natural moisturizing factors of skin, and its effects of moisturizing, softening skin, promoting transdermal penetration, etc. have been widely reported in the literature. However, the practical use of urea with potent skin care efficacy in cosmetics or dermatological products presents challenges. The urea has strict requirements on the bearing capacity of a formula system, and the bearing capacity of most of the commercial formulas of cosmetics cannot meet the requirements of compound urea.
The present invention innovatively provides a stable composition capable of carrying urea or a derivative thereof.
In some embodiments, the urea carried by the stabilizing composition of the present invention is in the form of a urea formulation. For example, the urea compound is urea: glycine: and the weight ratio of the triethyl citrate to the compound is 10:10:1. In a specific embodiment, the urea formulation is a formulation of 5% urea, 5% glycine, and 0.5% triethyl citrate.
In some embodiments, the urea carried by the stabilizing composition of the present invention is a urea derivative. For example, the urea derivative is a hydroxyalkylated derivative of urea. In a specific embodiment, the urea derivative is a hydroxyalkylated derivative having 1 to 6 carbon atoms. In a specific embodiment, the urea derivative is hydroxyethyl urea.
In some embodiments of the invention, the stabilizing composition comprises 0.1 to 20 wt% urea or a derivative thereof. In some embodiments of the invention, the stabilizing composition comprises 0.1 to 10 wt% urea or a derivative thereof.
In some embodiments of the invention, the stabilizing composition comprises greater than 1% by weight urea or a derivative thereof. In some embodiments of the invention, the stabilizing composition comprises more than 2% by weight urea or derivatives thereof. In some embodiments of the invention, the stabilizing composition comprises more than 3% by weight urea or derivatives thereof. In some embodiments of the invention, the stabilizing composition comprises more than 4% by weight urea or derivatives thereof. In some embodiments of the invention, the stabilizing composition comprises more than 5% by weight urea or derivatives thereof.
Grease and oil
The stabilizing composition of the invention carrying urea or a derivative thereof comprises a grease. In some embodiments, the oils and fats included in the stabilizing composition of the present invention are selected from the group consisting of: (1) a non-polar solid fat; (2) a non-polar liquid fat; (3) polar liquid oils and fats; (4) polar solid fats and oils; (5) silicone oil; or any mixture thereof.
In some embodiments, the stabilizing compositions of the present invention comprise white petrolatum. In some embodiments, the stabilizing composition of the present invention comprises a # 10 white oil. In some embodiments, the stabilizing composition of the present invention comprises isooctyl palmitate. In some embodiments, the stabilizing composition of the present invention comprises cetyl palmitate. For example, in some specific embodiments, the stabilizing composition of the present invention comprises cetyl palmitate ACP purchased from Croda (singapore). In some embodiments, the stabilizing composition of the present invention comprises simethicone. For example, in some embodiments, the stabilizing composition of the present invention comprises simethicone (100 cst) from dow (tensor) investment limited.
In some embodiments of the invention, the stabilizing composition comprises 0.1 to 20 wt% grease. In some embodiments of the invention, the stabilizing composition comprises 1-20% by weight of grease. In some embodiments of the invention, the stabilizing composition comprises 1-10% by weight of grease. In some embodiments of the invention, the stabilizing composition comprises 5-10% by weight of grease.
Cationic surfactants
Cationic surfactant refers to an emulsifier with cationic groups, the molecular structure of which comprises cationic groups and alkyl chains. Wherein, the cationic group mainly comprises alkyl quaternary ammonium salt, alkyl pyridinium salt and alkyl amine salt, has good heat resistance, light resistance and acid-base resistance generally, and has good surface activity, stability and biodegradability. Because of the unique charge property of the cationic surfactant, the cationic surfactant can form a film on the surface of skin or hair, so that the cationic surfactant has unique product use feel and is widely applied to hair products.
The cationic surfactant is compounded in the hair product, the alkyl chain of the cationic surfactant is attached to the surface of the cutin to form a cationic membrane, and the charge repulsion of the cationic membrane enables the matrix to have a lubricating effect, so that the hair is smooth and soft after the hair product is used, and the force required for combing the hair is reduced. In contrast, cationic surfactants are used relatively rarely in skin care products due to the wide application of anionic thickeners. However, the cationic surfactant has strong absorption and film forming properties, can remarkably shield the sticky and greasy feeling of grease, can provide a unique use feel for the product, and can provide unique competitiveness in the cosmetic market if the cationic surfactant can be applied to a proper product.
The stabilizing composition of the present invention comprises a cationic surfactant. In a specific embodiment, the cationic surfactant employed in the stabilizing composition of the present invention is distearyl dimethyl ammonium chloride. In a specific embodiment, the cationic surfactant employed in the stabilizing composition of the present invention is TA-100 from Evonik Operations GmbH.
The present invention has surprisingly found that the use of distearyldimethylammonium chloride results in a stable composition capable of supporting urea or derivatives thereof. It was also unexpected that the viscosity of the samples was significantly increased in the high temperature stability over time test after the partial samples were compounded with urea, whereas samples without compounded urea did not show a similar anomaly. The abnormal phenomenon has higher application value in the actual production of cosmetics and skin medical products: (1) The distearyl dimethyl ammonium chloride and other emulsifying agents are compounded, so that the phenomenon that the viscosity of a material body is obviously reduced after the distearyl dimethyl ammonium chloride and urea are compounded can be improved or avoided; (2) The viscosity of the sample is regulated and controlled by high-temperature aging of the material body in the preparation process; (3) This property can be used to prepare a hard cream and remain stable in the fortification test. It is also necessary to point out that the efficacy of urea is suitable for the care of dry skin, whereas cosmetic oils designed for such skin types are generally added in high amounts, and thus have greasy skin feel and poor absorption. The distearyl dimethyl ammonium chloride has extremely strong absorption and covering properties when being applied to cosmetics due to the cationic property, can effectively improve the greasy feel of a high-grease-addition formula, improves the absorbability of the distearyl dimethyl ammonium chloride, and enables consumers to obtain better use experience while meeting the efficacy of the cosmetics.
In some embodiments of the invention, the stabilizing composition comprises 0.5 to 20 wt% cationic surfactant. In some embodiments of the invention, the stabilizing composition comprises 1 to 20 wt% cationic surfactant. In some embodiments of the invention, the stabilizing composition comprises 1 to 10 wt% cationic surfactant. In some embodiments of the invention, the stabilizing composition comprises 2.5 to 10 wt% cationic surfactant. In some embodiments of the invention, the stabilizing composition comprises 5 to 10 wt% cationic surfactant.
In some embodiments of the invention, the weight ratio of cationic emulsifier to supported urea or derivative thereof is from 1:10 to 50:1. In some embodiments of the invention, the weight ratio of cationic emulsifier to supported urea or derivative thereof is from 1:10 to 10:1. In some embodiments of the invention, the weight ratio of cationic emulsifier to supported urea or derivative thereof is from 1:2 to 10:1. In one embodiment of the invention, the weight ratio of cationic emulsifier to supported urea or derivative thereof is 1:1.
Long chain fatty alcohols
The urea or derivative thereof bearing stable composition of the present invention comprises a long chain fatty alcohol. In some embodiments, the long chain fatty alcohols included in the stabilizing compositions of the present invention are long chain fatty alcohols having from 16 to 22 carbon atoms.
In some embodiments, the stabilizing composition of the present invention comprises a long chain fatty alcohol selected from the group consisting of: cetyl alcohol, cetostearyl alcohol, stearyl alcohol, arachidyl alcohol, behenyl alcohol, or mixtures thereof.
In some embodiments of the invention, the stabilizing composition comprises 0.1 to 10 wt% long chain fatty alcohol. In some embodiments of the invention, the stabilizing composition comprises 0.5 to 10 wt% long chain fatty alcohol. In some embodiments of the invention, the stabilizing composition comprises 1-10 wt% long chain fatty alcohols. In some embodiments of the invention, the stabilizing composition comprises 1-5% by weight of long chain fatty alcohols. In some embodiments of the invention, the stabilizing composition comprises 3 to 5 wt% long chain fatty alcohols.
In some embodiments of the invention, the weight ratio of cationic emulsifier to long chain fatty alcohol is from 10:1 to 1:4. In some embodiments of the invention, the weight ratio of cationic emulsifier to long chain fatty alcohol is from 10:1 to 1:2. In some embodiments of the invention, the weight ratio of cationic emulsifier to long chain fatty alcohol is from 10:1 to 1:1. In one embodiment of the invention, the weight ratio of cationic emulsifier to long chain fatty alcohol is 5:2.
Aqueous phase
The stabilizing composition of the present invention further comprises an aqueous phase. In some embodiments, the aqueous phase may be water or other aqueous carrier.
In some embodiments of the invention, the stabilizing composition comprises greater than 50% by weight of the aqueous phase. In some embodiments of the invention, the stabilizing composition comprises more than 60% by weight of the aqueous phase. In some embodiments of the invention, the stabilizing composition comprises more than 70% by weight of the aqueous phase. In some embodiments of the invention, the stabilizing composition comprises more than 80% by weight of the aqueous phase.
External preparation for skin
The composition of the present invention can be applied as an efficacy additive in skin external preparations. In some embodiments, the skin external agent is selected from the group consisting of: facial cleanser, toning lotion, emulsion, cream, gel and facial mask. Different amounts are added according to the different types of formulations.
The external skin preparation is a general concept of all ingredients commonly used outside the skin, and may be, for example, a cosmetic composition. The cosmetic composition may be basic cosmetic, facial makeup cosmetic, body cosmetic, hair care cosmetic, etc., and its dosage form is not particularly limited and may be reasonably selected according to different purposes. The cosmetic composition also contains various cosmetically acceptable medium or matrix excipients depending on dosage form and purpose.
The stable compositions of the invention form an emulsifying system, are particularly suitable for skin care of dry and medium dry skin, and have particular advantages in cosmetics for hand, foot, body care.
For example, based on the results of a 14-day consumer leave-on test feedback, it is recognized that the stable compositions of the present invention are useful for hand to moisturize skin, soften skin, fine skin, enhance skin luster, prevent chapping, alleviate tightness, smooth skin at a rate of 98%, 96%, 94%, 96% and 98% in order, and that experimental results can be supported by laboratory objective index determinations (skin moisture content, transdermal moisture loss, skin elasticity, skin scale value, skin smoothness are improved immediately and after 4 weeks of use, and have statistical differences compared to control). In addition, 94% of the consumers recognize that the product is easy to absorb and is not sticky after absorption, and 98% of the consumers recognize that the product has a protective film feel. Therefore, the technology reported by the invention is applied to proper products, and can simultaneously endow the products with good using feel and efficacy, so that the products have strong product competitiveness.
The invention will be further illustrated by the following examples. It is noted herein that the examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, since many insubstantial modifications and variations will become apparent to those skilled in the art in light of the above teachings. The test methods in the following examples, in which specific conditions are not specified, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. All percentages and parts are by weight unless otherwise indicated.
Experimental materials:
distearyldimethyl ammonium chloride (TA-100): purchased from Evonik Operations GmbH;
cetostearyl alcohol (H-MY): purchased from Emery Oleochemicals (M) Sdn Bhd;
white vaseline: purchased from hansheng chemical (pacifying) company, ltd;
urea: purchased from national pharmaceutical group chemical reagent company, inc;
hydroxyethyl urea (50%): purchased from Guangzhou Sipu fine chemical technology Co., ltd;
triethyl citrate: purchased from Shanghai Pu Jie fragrance company, inc.;
glycine: purchased from Hebei Huayang biotechnology limited;
cetyl alcohol (cetyl alcohol): purchased from BASF;
behenyl alcohol (behenyl alcohol): purchased from BASF;
Cationic conditioning agent ECON-100: purchased from Chongqing sea sail Biochemical technology Co., ltd;
laurinol phosphate potassium salt (HR-S1): purchased from dandong Ankang chemical plant in Liaoning;
polyglycerol pentastearate and sodium stearoyl lactate: purchased from NIKKOL chemistry co.ltd;
glycerol laurate: purchased from BASF;
polyglycerol-10 myristate (polyglyceryl monomyridate): purchased from NIKKOL chemistry co.ltd;
PEG-20 methyl glucose sesquistearate (MSE-20): lu Borun specialty chemical (Shanghai) Inc.;
cetostearyl alcohol polyether-30: purchased from BASF;
alatong 2121: purchased from CRODA;
polyquaternium-37 (PQ-37): purchased from BASF;
grafted corn starch 25: purchased from Daito KaseiKogyo co., ltd;
xanthan gum: purchased from Jungbunzlauer Austria AG;
sodium polyacrylate: purchased from japan, senxin;
ammonium acryloyldimethyl taurate/VP copolymer (AVC): purchased from Clariant;
10# white oil: purchased from zhejiang zheng zhshi oil technologies limited;
isooctyl palmitate: purchased from PALM-ole (KLANG) SDN BHD;
hexadecanoate ACP: purchased from Croda (singapore);
simethicone (100 cst): purchased from the dow (tensor harbor) investment company.
Experimental instrument:
weighing balance: METTER TOLEDO, PB4002-N;
Constant temperature water bath: HWS-28, shanghai-Hengsu scientific instruments Co., ltd;
table homogenizer: POLYTRON, PT 3100D;
bench stirrer: IKA EUROSTAR, power control-visc;
constant temperature oven at 25 ℃): MMM, FRIOCELL707, germany;
oven with constant temperature of 48 ℃): MMM, FRIOCELL707, germany;
pH meter: METTLER TOLEDO, sevenMulti;
a viscometer: BROOKFIELD, DV-S digital viscometer.
Examples 1 to 18: emulsifying systems containing different surfactants and the preparation of corresponding urea-containing samples.
Appropriate amounts of phase A, phase B and phase C were weighed into three beakers as shown in Table 1 and heated in a 90℃water bath for 30min, respectively. Homogenizing the phase A by using a table homogenizer at 5000rpm for 2min to uniformly disperse the phase A; homogenizing at 5000rpm, adding phase B while it is hot, and homogenizing for 2min; the homogenization was continued at 5000rpm, phase C was added to the mixed sample while hot, and after phase C was added, the homogenization was continued for 5min. After which the beaker was sealed with PE film and the sample was allowed to stand at room temperature overnight. Adding phase D the next day, homogenizing at 5000rpm for 3min at room temperature again using a table homogenizer to uniformly mix the sample, sealing the beaker with PE film, and keeping the sample for use.
Table 1 shows the amounts of the surfactant types and the respective materials contained in examples 1 to 18.
TABLE 1
Examples 1-18 were configured with 9 multiple emulsion systems containing different surfactants, one for each of the base stock and urea containing examples. The preparation amount of each sample is 200g, the preparation process uniformly adopts a concentrated water phase method, and the mixture is compounded with 2% of cetostearyl alcohol and 6% of white vaseline, and the urea addition amounts of the embodiments containing urea are all 5%.
Examples 19 to 33: and preparing hydrosols of various polymer thickeners and corresponding samples containing urea.
An appropriate amount of deionized water was weighed into a beaker as shown in Table 2, stirred at 500rpm at room temperature, polymer powder was slowly added into the beaker, and after the polymer was immersed and dispersed, the stirring speed was increased to 1000rpm and maintained for 60min to completely and uniformly disperse the polymer. After that, the raw materials listed in the phase B are added into a beaker, and stirring is continued at a speed of 1000rpm for 30min so that the solid is completely dissolved and uniformly dispersed.
Table 2 shows the types of the polymer thickeners included in examples 19 to 33 and the amounts of the respective materials to be charged.
TABLE 2
Examples 19-33 were equipped with 5 complex emulsifying systems containing different polymeric thickeners, each having a conditional weight of 0.4% or 0.5% depending on the viscosity of the hydrosol. Three samples of each polymer thickener are respectively prepared, and are respectively a base material, a urea-containing sample and a urea-containing composition sample. The preparation amount of each sample is 200g, the addition amount of urea in the urea-containing sample is 5%, and 5% urea, 5% glycine and 0.5% triethyl citrate are added in the urea-containing composition sample.
Test example 1: stability test of examples 1 to 33
After measuring the pH and viscosity of the samples of the fresh examples 1 to 33, each sample was equally divided into 2 transparent PET bottles of 150ml, and after the cap was closed and screwed, the samples were placed in a incubator of 25℃and an incubator of 48℃respectively. And taking out the sample from the incubator at regular intervals, standing for 6 hours, cooling to room temperature, measuring the pH and viscosity of the sample, observing the properties of the sample, and returning the sample to the incubator after the measurement is finished.
Table 3 shows the pH and viscosity at each time point tested for examples 1-33.
TABLE 3 Table 3
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Table 3 summarizes the pH and viscosity at each test time point for examples 1-33. Examples 1-18 were a formulated emulsifying system prepared with 9 different commercially available surfactants, and corresponding urea addition samples. Among them, 2 cationic surfactants (TA-100, examples 1-2; ECON-100, examples 3-4), 1 anionic surfactant (HR-S1, examples 5-6), 1 anionic complex nonionic surfactant (polyglycerol pentastearate and sodium stearoyl lactate, examples 7-8), and 5 nonionic surfactants were selected. The 5 nonionic surfactants can be further subdivided into: (1) Monoglyceride-based surfactants (glycerol laurate, examples 9-10); (2) Polyglycerol ester surfactants (polyglycerol monomyristoate, examples 11-12); (3) Polyethylene glycol-based surfactants (cetostearyl alcohol polyether-30, examples 13-14); (4) Sugar surfactants (MSE-20, examples 15-16; alatong 2121, examples 17-18).
After the TA-100 based compound emulsification system (example 1) was left for one month at room temperature, the sample pH was slightly lowered from 4.99 to 4.96; the sample viscosity was 4780 mPas, which was higher than that of the freshly prepared sample 3170 mPas. After 1 month of standing at 48℃the pH of the sample was 4.79, which decreased slightly from the initial value, and the viscosity was 2380 mPas, which decreased slightly from the freshly prepared sample. After 1 month of standing at room temperature, the pH of the sample (example 2) compounded with 5% urea increased from 5.45 to 7.66 and the viscosity decreased significantly from 2180 mPas to 680 mPas. The viscosity of the sample increased significantly after 1 month of standing at 48 ℃. The viscosities of the samples left at 48℃for 1 week and 2 weeks, i.e., 1 month, were 11530 mPas, 11100 mPas and 9720 mPas, respectively, compared with the viscosity of the freshly prepared samples 3570 mPas. At the same time, the sample pH also increased from 5.45 to 9.24. The experimental results show that the TA-100 compound system can stably bear urea, and in addition, in the test of the high-temperature time stability of the embodiment 2, the viscosity of a sample is obviously improved.
After the cationic conditioner ECON-100 based compound emulsion system (example 3) was left for one month at room temperature, the sample pH was slightly lowered from 3.89 to 3.86; the sample viscosity is too low, the suspension force is insufficient and cannot be kept stable, and layering phenomenon occurs after standing for a short time. After 1 month of standing at 48 ℃, the samples also show delamination at all time points, and the pH value of the samples after the stability test is 3.67, and the samples are slightly reduced compared with the initial value. After 1 month of standing at room temperature, the pH of the sample (example 4) compounded with 5% urea rose slightly from 4.06 to 4.16, and the sample also had delamination at each time point. After the sample was left at 48 ℃ for 1 month, the pH rose greatly from 4.06 to 7.58, and delamination also occurred at each test time point. The experimental results show that the cationic conditioner ECON-100 compound system cannot stably bear urea, and layering problems occur in two samples under each test condition. Furthermore, the formulated urea sample (example 4) did not observe similar tackifying properties to those exhibited by example 2 in the high temperature time course test, despite being a cationic surfactant.
After the compound emulsifying system (example 5) based on lauryl phosphate potassium salt (HR-S1) was left at room temperature for one month, the pH of the sample was reduced from 7.57 to 7.45 in a small scale; the sample viscosity was 725 mPas, which was higher than that of the freshly prepared sample 117 mPas. After 1 month of standing at 48 ℃, the pH of the sample was 7.72, which rose slightly from the initial value, but the sample was delaminated at each time point due to too low a viscosity. After 1 month of standing at room temperature, the pH of the sample (example 6) was slightly increased from 7.43 to 7.62, and the viscosities of the samples for 1 week, 2 weeks and 1 month at room temperature were 392 mPas, 1658 mPas and 2358 mPas, respectively, which were significantly increased from the initial values of 125 mPas. After the sample was left at 48℃for 1 month, the pH of the sample increased substantially from 7.43 to 8.93, and the tests were all layered due to insufficient suspension force with too low viscosity. The experimental results show that the laurinol potassium phosphate (HR-S1) compound emulsifying system can only stably bear urea at room temperature, and the material body is layered due to insufficient suspension force at high temperature.
After the compound emulsifying system (example 7) based on polyglycerol pentastearate and sodium stearoyl lactate was left at room temperature for one month, the pH of the sample was reduced from 4.74 to 4.33 in small steps; the sample viscosity was 18580 mPas, which was significantly higher than that of the freshly prepared sample 4950 mPas. After 1 month of standing at 48℃the pH of the sample was 4.46, which decreased slightly from the initial value, and the viscosity was 149420 mPas, which decreased slightly as compared to the freshly prepared sample. After 1 month of standing at room temperature, the pH of the sample (example 8) compounded with 5% urea increased from 4.80 to 5.87, and the viscosity increased significantly from 6250 mPas to 25250 mPas. The viscosity of the sample also increased significantly after 1 month of standing at 48 ℃. The viscosities of the samples for 1 week, 2 weeks and 1 month at 48℃were 35580 mPas, 23830 mPas and 28500 mPas, respectively, compared to the viscosity of the freshly prepared samples 6250 mPas. At the same time, the sample pH also increased from 4.80 to 8.08. The experimental result shows that the compound system based on polyglycerol pentastearate and sodium stearoyl lactate can stably bear urea.
After the glycerol laurate-based compound emulsifying system (example 9) was left for one month at room temperature, the pH of the sample was reduced from 4.77 to 4.07; however, the sample viscosity is too low, the suspension force is insufficient, a stable emulsifying system cannot be maintained, and the sample can be layered after standing for a short time. After 1 month of standing at 48 ℃, delamination is also caused by too low viscosity of the material; the pH of the sample after stability testing was 4.74, which was substantially the same as the initial value. After 1 month of standing at room temperature, the pH of the compounded 5% urea sample (example 10) was slightly raised from 6.32 to 7.21, and the viscosities of the samples for 1 week, 2 weeks and 1 month at room temperature were 992 mPas, 3680 mPas and 7830 mPas, respectively, which were significantly raised (< 150 mPas) from the initial values. However, after the sample was left to stand at 48 ℃ for 1 month, the pH of the sample increased from 6.32 to 7.37, delamination occurred at each test due to insufficient suspension force due to too low viscosity, and demulsification was evident from 2 weeks of standing, forming an oil cake at the top of the body. The experimental results show that the compound emulsifying system based on glycerol laurate can only stably bear urea at room temperature, and the viscosity of the micelle reconstituted material rises, but in a Gao Wenjing stability test, the micelle reconstituted material is layered due to insufficient suspension force, and the emulsifying capacity of the surfactant is reduced to break emulsion.
After the compound emulsifying system based on the polyglyceryl monomyristoate (example 11) was left at room temperature for one month, the pH of the sample was slightly reduced from 7.99 to 6.67; the sample viscosity is too low, the suspension force is insufficient, a stable emulsifying system cannot be maintained, and the sample can be layered after standing for a short time. After standing at 48 ℃ for 1 month, the material body is still layered due to too low viscosity; the pH of the sample after stability testing was 7.19, which was reduced from the initial value. After 1 month of standing at room temperature, the sample (example 12) formulated with 5% urea had slightly decreased from 8.16 to 7.98 in pH and was layered at each time point. After the sample was left at 48℃for 1 month, the pH of the sample was raised from 8.16 to 8.83 and the samples were likewise layered at each test time. The experimental results show that the compound emulsion system of the polyglyceryl monomyristoate can not stably bear urea, and layering problems occur in two samples under each test condition.
After a one month standing at room temperature of the cetostearyl alcohol polyether-30-based compound emulsifying system (example 13), the pH of the sample rose slightly from 6.30 to 6.45; the sample viscosity is too low, the suspension force is insufficient, a stable emulsifying system cannot be maintained, and the sample can be layered after standing for a short time. After standing at 48 ℃ for 1 month, the material body is layered due to too low viscosity; and the pH drops to 4.13, which is significantly lower than the initial value. After 1 month of standing at room temperature, the pH of the sample (example 14) formulated with 5% urea increased from 7.52 to 8.14 and the sample was layered at each time point. After the sample was left at 48 ℃ for 1 month, the sample pH was raised from 7.52 to 9.06 and the samples were layered at each test time. The experimental results show that the cetostearyl alcohol polyether-30 compound system cannot stably bear urea, and layering problems occur in two samples under each test condition.
After the MSE-20 based compound emulsification system (example 15) was left at room temperature for one month, the sample pH was reduced slightly from 7.08 to 6.67; the sample viscosity was 167 mPas, which was slightly lower than that of the freshly prepared sample 183 mPas. After being placed at 48 ℃ for 1 month, the pH value of the sample is 3.86, and compared with the initial value, the pH value of the sample is obviously reduced; the viscosity of the samples after 1 week, 2 weeks and 1 month was 1700 mPas, 2600 mPas and 15670 mPas, respectively, which were significantly higher than the viscosity of the freshly prepared samples. After 1 month of standing at room temperature, the pH of the sample of 5% urea (example 16) was raised from 7.13 to 7.93 and the viscosity was slightly reduced from 167 mPas to 142 mPas. The viscosity of the sample also increased after 1 month at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 1400 mPas, 2200 mPas and 1833 mPas, respectively, compared with the viscosity of the freshly prepared samples, but the rise was significantly smaller than that of the samples without urea compounding. At the same time, the sample pH also increased from 7.13 to 8.92. The experimental result shows that the compound system based on MSE-20 can stably bear urea, however, the compound of urea obviously influences the micelle reconstruction of the surface activity at high temperature, so that the viscosity rise amplitude of the compound urea sample in the high-temperature time stability test is obviously lower than that of the compound urea sample.
After the composite emulsifying system based on the Arragon 2121 (example 17) is placed for one month at room temperature, the pH value of the sample is reduced from 7.01 to 6.82 in a small scale; the sample viscosity was 46330 mPas, which was slightly lower than the newly prepared sample 47500 mPas. After 1 month of standing at 48 ℃, the pH value of the sample is 6.52, and the pH value is reduced compared with the initial value; the viscosity of the samples was 50170 mPas, 51000 mPas and 52500 mPas in this order for 1 week, 2 weeks and 1 month, and slightly increased as compared to the freshly prepared samples. After 1 month of standing at room temperature, the pH of the sample of 5% urea (example 18) was raised from 6.95 to 7.19 and the viscosity was slightly lowered from 48750 mPas to 43170 mPas. The viscosity of the sample showed a significant decrease after 1 month of standing at 48℃compared to 48750 mPas for the freshly prepared sample, and the viscosities of the samples for 1 week, 2 weeks and 1 month at 48℃were 44080 mPas, 32250 mPas and 23000 mPas, respectively. At the same time, the sample pH also increased from 6.95 to 7.92. The experimental result shows that the compound system based on the Alatron 2121 can stably bear urea, however, the compound urea obviously influences the high-temperature stability of the emulsion system, and the viscosity of a sample after 1 month stability test is less than half of an initial value.
The above experimental data indicate that of the 9 emulsification systems tested, only 4 emulsification systems can carry urea, with the emulsification systems based on MSE-20 and alatong 2121 having shown a more pronounced impact of the urea formulation on the stability of the respective emulsification systems at high temperatures. As can be seen, for most surfactants, the loading of urea is a great challenge to its formulation stability. It is necessary to point out that the TA-100-based compound emulsion system (example 2) has good stability, and the high-temperature tackifying performance which is not possessed by the non-compound urea sample (example 1) also appears after the compound urea is compounded, so the properties of the compound emulsion system are studied more intensively below.
In addition to surfactants, polymeric thickeners are often used in cosmetics to provide viscosity to the formulation, which in turn improves the stability of the formulation. Examples 19-33 examined the stability of five different commercial polymeric thickener hydrosols after compounding urea, the polymers examined can be divided into three categories according to the structure of the polymeric chain: (1) Cationic polymeric thickeners (PQ-37, examples 19-21); (2) Nonionic polymeric thickeners (M25, examples 22-24; xanthan gum, examples 25-27); (3) Anionic polymeric thickeners (sodium polyacrylate, examples 28-30; AVC, examples 31-33). Three samples were prepared for each polymer, one of which was not compounded with urea, the second with 5% urea, and the third with 5% urea, 5% glycine, and 0.5% triethyl citrate.
The 0.5% PQ-37 hydrosol (example 19) had good stability. After the sample was left at room temperature for 1 month, the viscosity increased slightly from 16430 mPas to 18370 mPas; in contrast, after the sample was left at 48℃for one month, the viscosity was 15130 mPas, and the change in viscosity was not significant as compared with the newly prepared sample 16430 mPas. After compounding PQ-37 with 5% urea (example 20), the sample stability was significantly degraded, the pH increased from 4.43 to 7.84 and the viscosity decreased from 18030 mPa-s to 5280 mPa-s after 1 month of standing at room temperature for example 20; and after only one week at 48℃the viscosity dropped to 183 mPas with the pH rising to 8.88. After PQ-37 was compounded with 5% urea, 5% glycine and 0.5% triethyl citrate (example 21), the sample stability also significantly deteriorated, the pH slightly increased from 5.23 to 5.77 and the viscosity decreased from 13230 mpa.s to 5430 mpa.s after 1 month of standing at room temperature in example 21; after a week of standing at 48℃the pH rose to a small extent to 5.70, while the viscosity dropped to 333 mPas. The experimental results show that the PQ-37 hydrosol cannot stably bear urea. And the results of example 21 show that the rise in pH caused by urea decomposition is not the only cause of bulk tack-free.
The 0.4% m25 hydrosol (example 22) was better in stability. After the sample was left at room temperature for 1 month, the viscosity increased slightly from 15420 mPas to 18270 mPas; and after one month at 48 ℃, the viscosity was 8270mpa·s, which was lower than that of the freshly prepared sample 15420mpa·s. After compounding 5% urea with M25 (example 23) the sample stability was degraded, example 20 was left at room temperature for 1 month, the pH increased from 7.13 to 7.48, and the viscosity decreased from 16080 mPa-s to 15220 mPa-s; after a month at 48℃the viscosity dropped significantly to 2230 mPas with increasing pH to 8.90. After PQ-37 was compounded with 5% urea, 5% glycine and 0.5% triethyl citrate (example 24), the sample stability was likewise deteriorated, the pH value was reduced slightly from 6.76 to 6.62 and the viscosity was reduced from 15830 mPa-s to 8700 mPa-s after 1 month standing at room temperature in example 24; after a month of standing at 48℃the pH was reduced to 6.31, while the viscosity was greatly reduced to 1170 mPa.s. The experimental results show that the M25 hydrosol cannot stably bear urea.
The 0.5% xanthan gum hydrosol (example 25) has good stability. After the sample is left at room temperature for 1 month, the viscosity is slightly increased from 1242 mPas to 1317 mPas; and after one month at 48 ℃, the viscosity was 970mpa·s, which was reduced slightly compared with the freshly prepared sample. After compounding xanthan gum with 5% urea (example 26), the sample remained well stable, and after example 20 was left at room temperature for 1 month, the pH increased from 7.04 to 7.38, while the viscosity increased slightly from 1383 mPa-s to 1425 mPa-s; and after one month of standing at 48℃the pH of the sample rose to 8.65 and the viscosity dropped to 867 mPas. After PQ-37 was compounded with 5% urea, 5% glycine and 0.5% triethyl citrate (example 27), the sample stability was not significantly changed, and after example 21 was left at room temperature for 1 month, the pH was slightly increased from 5.55 to 7.21 and the viscosity was slightly increased from 1442 mPa-s to 1575 mPa-s; and after one month of standing at 48 ℃, the pH value rose slightly to 6.04, while the sample viscosity decreased slightly to 1270 mPa-s. The experimental results show that the xanthan gum hydrosol can stably bear urea and the composition thereof.
The 0.4% sodium polyacrylate hydrosol (example 28) has good stability. After the sample was left at room temperature for 1 month, the viscosity increased slightly from 2667 mPas to 2625 mPas; and after being left at 48 ℃ for one month, the viscosity is 2845 mPas, and the viscosity is less changed compared with a new sample. After compounding sodium polyacrylate with 5% urea (example 29), the sample stability was significantly degraded, the pH increased from 6.89 to 7.26 and the viscosity decreased from 3392 mPa-s to 833 mPa-s after 1 month of standing at room temperature for example 29; and after only one week at 48 ℃, the pH increased to 7.99 and the viscosity decreased significantly to 142 mPas. After compounding sodium polyacrylate with 5% urea, 5% glycine and 0.5% triethyl citrate (example 30), the sample stability also significantly deteriorated. Example 30 after 1 month at room temperature, the pH value was reduced from 6.51 to 6.32 with a large decrease in viscosity from 2000 mPas to 358 mPas; after one week of standing at 48℃the pH was reduced to 5.80, while the viscosity of the sample was greatly reduced to 117 mPas. The experimental results show that the sodium polyacrylate hydrosol can not stably bear urea and a urea composition.
The 0.4% avc hydrosol (example 31) was stable. After the sample was left at room temperature for 1 month, the viscosity increased slightly from 5250 mPas to 7400 mPas; and after being placed at 48 ℃ for one month, the viscosity is 13570 mPas, which is obviously improved compared with a new sample, and the reason is probably that the rearrangement of micelle structures is promoted by high temperature. After AVC was compounded with 5% urea (example 32), the sample stability was significantly degraded, and after example 32 was left at room temperature for 1 month, the pH increased from 6.46 to 7.64 and the viscosity decreased from 6092 mPa-s to 608 mPa-s; after only one week at 48℃the viscosity decreased significantly to 142 mPas with an increase in pH to 8.61. After AVC was formulated with 5% urea, 5% glycine and 0.5% triethyl citrate (example 33), the sample stability was also significantly degraded. Example 21 after 1 month at room temperature, the pH rose slightly from 5.64 to 5.73, while the viscosity decreased from 3180 mPas to 508 mPas; after the sample was left at 48℃for one week, the pH value was raised to 5.73 by a small margin, and the viscosity of the sample was lowered to 117 mPas by a large margin. The experimental results show that the AVC hydrosol cannot stably bear urea and the composition thereof.
The experimental results show that four of the five tested high-molecular thickeners cannot stably bear urea. However, there are also many limitations in practical cosmetic applications such as low thickening efficiency and inability to formulate higher viscosity dosage forms, and sticky skin feel affects product feel. In addition, it should be noted that four polymers with significantly reduced viscosity in the stability test, after the composition of urea+glycine+triethyl citrate was compounded, although the pH remained substantially stable, a significant viscosity reduction phenomenon still occurred in the stability test, indicating that the pH rise due to urea decomposition was not the only cause of sample viscosity loss. The strong ionic nature of the urea decomposition products likewise places high demands on the stability of the formulation. Most of the macromolecular thickeners form a gel structure by means of repulsive force between the same charges, the electric double layer can be weakened by the enhancement of the ionic property, and the repulsive force of the charges between molecules of the thickener is reduced to lose viscosity, so that the choice space of the macromolecular thickener with good stability after the urea is compounded is extremely limited.
As can be seen, most surfactants and polymeric thickeners do not have the ability to stably carry urea, thus greatly limiting the practical use of urea with strong skin care efficacy in cosmetics. Moreover, after examining 12 kinds of emulsion formulations sold by Shanghai household Co., ltd (viscosity of 1000 mPas to 20000 mPas, each formulation using different emulsifiers), only cationic formulations using the same emulsifiers as in examples 1-2 can meet the national regulation on cosmetic stability after compounding urea. The other 11 formulas of surfactant based on anions, saccharides, polyethylene glycol and polyglycerol esters and compounding various high polymer thickeners all have the obvious problems of viscosity reduction, layering and even demulsification. It can be seen that the TA-100 based cationic emulsion formulation exhibits good stability and interesting high temperature viscosification properties after compounding with urea, and TA-100 is further explored below.
Examples 34 to 53: and (3) preparing a compound emulsifying system containing different grease types and grease amounts and corresponding urea-containing samples.
Appropriate amounts of phase A, phase B and phase C were weighed into three beakers as shown in Table 4 and heated in a 90℃water bath for 30min, respectively. Homogenizing the phase A by using a table homogenizer at 5000rpm for 2min to uniformly disperse the phase A; homogenizing at 5000rpm, adding phase B while it is hot, and homogenizing for 2min; the homogenization was continued at 5000rpm, phase C was added to the mixed sample while hot, and after phase C was added, the homogenization was continued for 5min. After which the beaker was sealed with PE film and the sample was allowed to stand at room temperature overnight. Adding phase D the next day, homogenizing at 5000rpm for 3min at room temperature again using a table homogenizer to uniformly mix the sample, sealing the beaker with PE film, and keeping the sample for use.
Table 4 shows the types of oils and fats contained in examples 34 to 53 and the amounts of the respective raw materials fed.
TABLE 4 Table 4
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The emulsification system of examples 34-53 was the same as examples 1-2, fixed as 5% TA-100 with 2% cetostearyl alcohol. The preparation amount of each sample is 200g, and the sample preparation process also adopts a concentrated water phase method consistent with the embodiment 1-2. On this basis, the influence of the type of the oil and the amount of the oil added on the properties of the sample was examined. Wherein examples 34-43 had a fixed grease addition of 6%, and samples were prepared using a plurality of different types of grease; while examples 44-53 fix the oil as white petrolatum to examine the effect of the amount of oil added on the properties of the samples. Each sample was prepared separately for each base and urea-containing example, with urea addition at 5%.
Test example 2: stability test of examples 34 to 53
After measuring the pH and viscosity of the samples of the new examples 34 to 53, each sample was equally divided into 2 transparent PET bottles of 150ml, and after the cap was closed and screwed, the samples were placed in a incubator of 25℃and an incubator of 48℃respectively. And taking out the sample from the incubator at regular intervals, standing for 6 hours, cooling to room temperature, measuring the pH and viscosity of the sample, observing the properties of the sample, and returning the sample to the incubator after the measurement is finished.
Table 5 shows the pH and viscosity at each test time point for examples 34-53 (see examples 1 and 2 for comparison).
TABLE 5
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Table 5 summarizes the pH and viscosity at each test time point for examples 34-53 and lists the corresponding data for examples 1-2 for comparison. Wherein examples 1-2 and examples 34-41 examined the effect of 5 different oils on the properties of the formulated emulsifying system, the five oils comprising: (1) Non-polar solid fats (white petrolatum, examples 1-2); (2) Non-polar liquid fats & oils (10 # white oil, examples 34-35); (3) Polar liquid fats and oils (isooctyl palmitate, examples 36-37); (4) Polar solid fats and oils (cetyl palmitate ACP, examples 38-39); (5) Silicone oil (simethicone (100 cst)), examples 40-41. In addition, examples 42 to 43 were used by compounding the above oils.
The sample of emulsified 10# white oil (example 34) had a pH of 4.94 after 1 month at room temperature, which was almost unchanged from the initial value of 4.93; the sample viscosity was 5700 mPas and slightly increased compared to the freshly prepared sample 5450 mPas. After 1 month of standing at 48℃the pH of the sample was reduced from 4.93 to 4.64 and the viscosity was 4200 mPas, which was a small drop compared to the freshly prepared sample. After 1 month of standing at room temperature, the pH of the sample of 5% urea (example 35) was increased from 5.47 to 7.80 and the viscosity was decreased from 8130 mPas to 5570 mPas. The viscosity of the sample increased after 1 month at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 9500 mPas, 8840 mPas and 8450 mPas, respectively, compared with the viscosity of the freshly prepared samples 1092 mPas. At the same time, the sample pH also increased from 5.47 to 9.21. The experimental result shows that the TA-100 compound system can stably bear urea after emulsifying 10# white oil, and the viscosity of a sample is in an ascending trend in a high-temperature time stability test.
After the sample (example 36) of the emulsified isooctyl palmitate was left at room temperature for 1 month, the pH was 4.24 and increased slightly from the initial value of 4.09; the sample viscosity was 7930 mPas, which was higher than 6170 mPas of the freshly prepared sample. After 1 month of standing at 48℃the pH of the sample was 4.09, which was consistent with the initial value, and the viscosity was 4930 mPas, which was slightly lower than the freshly prepared sample. After 1 month of standing at room temperature, the pH of the sample (example 37) compounded with 5% urea increased from 4.30 to 6.79 and the viscosity decreased greatly from 3570 mPas to 1100 mPas. The viscosity of the sample increased significantly after 1 month of standing at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 5000 mPas, 9630 mPas and 8280 mPas, respectively, compared to the viscosity of the freshly prepared samples 3570 mPas. At the same time, the sample pH also increased from 4.30 to 9.16. The experimental result shows that the TA-100 compound system can stably bear urea after emulsifying the isooctyl palmitate, and the viscosity of a sample is in an ascending trend in a high-temperature time stability test.
After a sample of emulsified hexadecanoyl ester ACP (example 38) was left at room temperature for 1 month, its pH was 4.59, slightly raised from the initial value of 4.47; the sample viscosity was 7480 mPas, which was significantly higher than that of the freshly prepared sample 6100 mPas. After 1 month of standing at 48℃the pH of the sample was 4.46, which showed little change compared to the freshly prepared sample, while the viscosity was 6300 mPas, which increased slightly compared to the freshly prepared sample. After 1 month at room temperature, the pH of the sample of 5% urea (example 39) was raised from 4.87 to 7.40 and the viscosity from 3570 mPas to 4570 mPas. The viscosity of the sample increased significantly after 1 month of standing at 48 ℃. The viscosities of the samples placed at 48℃for 1 week, 2 weeks and 1 month were 12380 mPas, 17330 mPas and 15330 mPas, respectively, compared to the viscosity of the freshly prepared samples 3570 mPas. At the same time, the sample pH also increased from 4.87 to 8.98. The experimental result shows that the TA-100 compound system can stably bear urea after emulsifying hexadecyl palmitate ACP, and the viscosity of a sample is obviously increased in a high-temperature time stability test.
A sample of emulsified simethicone (100 cst) (example 40) had a pH of 5.04 after 1 month at room temperature, which was slightly lower than the initial value of 5.08; the sample viscosity was 9630 mPas, which was significantly higher than 3250 mPas of the freshly prepared sample. After 1 month of standing at 48℃the pH of the sample was also 5.04, while the viscosity was 11230 mPas, which was significantly higher than the viscosity of the freshly prepared sample. After 1 month of standing at room temperature, the pH of the sample (example 41) compounded with 5% urea increased from 5.55 to 7.70 and the viscosity decreased from 4820 mPas to 2330 mPas. After the sample was left at 48℃for 1 month, the viscosities of the sample and the sample for 1 month were 8380 mPas, 16650 mPas and 17000 mPas, respectively. At the same time, the sample pH also increased from 5.55 to 9.21. The experimental result shows that the TA-100 compound system can stably bear urea after emulsifying the simethicone (100 cst), and the viscosity of a sample is obviously increased in a high-temperature time stability test.
After the sample (example 42) in which the various oils and fats were emulsified was left to stand at room temperature for 1 month, the pH thereof was reduced from 6.10 to 5.86 in a small amount, and the viscosity thereof was 1280 mPas, which was slightly increased from that of the freshly prepared sample 858 mPas. After 1 month of standing at 48℃the pH of the sample was reduced from 6.10 to 5.46, while the viscosity was 880 mPas, which was not significantly changed from the freshly prepared sample. After 1 month of standing at room temperature, the pH of the sample (example 43) compounded with 5% urea increased from 6.21 to 7.98, and the viscosity also increased slightly from 858 mPas to 1380 mPas. The viscosity of the sample increased significantly after 1 month of standing at 48 ℃. The viscosities of the samples placed at 48℃for 1 week, 2 weeks and 1 month were 5025 mPas, 20170 mPas and 11530 mPas, respectively, compared with the viscosity of the freshly prepared samples 1092 mPas. At the same time, the sample pH also increased from 6.21 to 9.02. The experimental result shows that the TA-100 compound system can stably bear urea after emulsifying the compound grease, and the viscosity of a sample also has a significant rising trend in a high-temperature time stability test.
The following conclusions can be drawn from the above experimental results: although the samples of examples 34-43 were slightly different in nature due to the differences in grease properties. But in general all samples showed the following commonalities consistent with examples 1-2: all examples can stably carry urea and the viscosity of the sample rises in a high temperature stability test over time after compounding urea. The TA-100 compound emulsion system has wide grease selection space after compounding urea, and is beneficial to the practical application of the technology reported by the invention in cosmetics.
Examples 44-53 fix the fat as white vaseline, and examine the influence of the fat addition on the properties of the TA-100 compound emulsion system. The amounts of oils and fats added in examples 44 to 45, examples 46 to 47, examples 48 to 49, examples 1 to 2, examples 50 to 51 and examples 52 to 53 were 0%, 1%, 3%, 6%, 10% and 20% in this order.
After 1 month at room temperature, the pH of the uncomplexed grease sample (example 44) was 4.97, which was slightly lower than the initial value of 5.29; the sample viscosity was 2150 mPas, which was slightly higher than 1700 mPas of the freshly prepared sample. After 1 month of standing at 48℃the pH of the sample was 4.88 and the viscosity was 1280 mPas, which was lower than the viscosity of the freshly prepared sample. After 1 month at room temperature, the pH of the sample of 5% urea (example 45) was raised from 5.27 to 7.14 and the viscosity was lowered from 1270 mPas to 258 mPas. The viscosity of the sample increased significantly after 1 month of standing at 48 ℃. The viscosities of the samples for 1 week, 2 weeks and 1 month at 48℃were 4250 mPas, 14500 mPas and 14750 mPas, respectively, compared to the viscosity of the freshly prepared samples. At the same time, the sample pH also increased from 5.27 to 9.24. The experimental results show that the TA-100 compound emulsion system has good urea bearing property under the condition of no compound grease, and the properties of related samples are not obviously different from those of examples 1-2.
After the 1% white vaseline sample (example 46) was allowed to stand at room temperature for 1 month, the pH was 5.01, which was slightly lower than the initial value of 5.25; the sample viscosity was 1980 mPas, which was slightly higher than that of the freshly prepared sample 1720 mPas. After 1 month of standing at 48℃the sample had a pH of 4.84 and a viscosity of 1330 mPas, which was lower than the viscosity of the freshly prepared sample. After 1 month at room temperature, the pH of the sample of 5% urea (example 47) was raised from 5.75 to 7.27 and the viscosity was lowered from 1320 mPas to 300 mPas. The viscosity of the sample increased significantly after 1 month of standing at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 3450 mPas, 13670 mPas and 14830 mPas, respectively, compared with the viscosity of the freshly prepared samples. At the same time, the sample pH also increased from 5.75 to 9.23. The experimental results show that the TA-100 compound emulsion system has good urea bearing property when 1% white vaseline is compounded, and the properties of related samples are not obviously different from those of examples 1-2.
After the compound 3% white vaseline sample (example 48) was left at room temperature for 1 month, its pH was 4.97, which was slightly lower than the initial value of 5.29; the sample viscosity was 2120 mPas, which was significantly higher than that of the freshly prepared sample 1900 mPas. After 1 month of standing at 48℃the pH of the sample was 4.88 and the viscosity was 1330 mPas, which was lower than the viscosity of the freshly prepared sample. After 1 month at room temperature, the pH of the sample (example 49) compounded with 5% urea increased from 5.76 to 7.41 and the viscosity decreased from 1530 mPas to 333 mPas. The viscosity of the sample increased significantly after 1 month of standing at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 5800 mPas, 16080 mPas and 1650 mPas, respectively, compared with the viscosities of the freshly prepared samples of 1530 mPas. At the same time, the sample pH also increased from 5.76 to 9.26. The experimental results show that the TA-100 compound emulsion system has good urea bearing property when being compounded with 3% white vaseline, and the properties of related samples are not obviously different from those of examples 1-2.
After the compounded 10% white vaseline sample (example 50) was left at room temperature for 1 month, its pH was 5.09, which was slightly lower than the initial value of 5.29; the sample viscosity was 2670 mPas, which was significantly higher than that of the freshly prepared sample 2200 mPas. After 1 month at 48℃the pH of the sample was 5.20 and the viscosity was 1620 mPas, which was lower than the viscosity of the freshly prepared sample. After 1 month of standing at room temperature, the pH of the sample (example 51) compounded with 5% urea increased from 5.78 to 7.43 and the viscosity decreased from 1770 mPas to 392 mPas. The viscosity of the sample increased significantly after 1 month of standing at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 8680 mPas, 18750 mPas and 21500 mPas, respectively, compared to the viscosity of the freshly prepared samples 1770 mPas. At the same time, the sample pH also increased from 5.78 to 9.28. The experimental results show that the TA-100 compound emulsion system has good urea bearing property when 10% white vaseline is compounded, and the properties of related samples are not obviously different from those of examples 1-2.
After the sample (example 52) compounded with 20% white vaseline is left at room temperature for 1 month, the pH value is 5.00, and the pH value is reduced compared with the initial value of 5.40; the sample viscosity was 10630 mPas, which was slightly higher than that of the 7020 mPas of the freshly prepared sample. After 1 month of standing at 48℃the pH of the sample was 4.95 and the viscosity was 4820 mPas, which was lower than the viscosity of the freshly prepared sample. After 1 month of standing at room temperature, the pH of the sample of 5% urea (example 53) was raised from 5.76 to 7.55 and the viscosity was lowered from 2380 mPas to 800 mPas. The viscosity of the sample increased significantly after 1 month of standing at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 14230 mPas, 18170 mPas and 19500 mPas, respectively, compared with the viscosity of the freshly prepared samples 2380 mPas. At the same time, the sample pH also increased from 5.76 to 9.23. The experimental results show that the TA-100 compound emulsion system has good urea bearing property when being compounded with 20% white vaseline, and the properties of related samples are not obviously different from those of examples 1-2.
Combining the experimental results of examples 44-53, we found that the viscosity of the TA-100 complex emulsion system gradually increased as the amount of white petrolatum complex increased. In the range of 0-20% of white vaseline, the TA-100 compound emulsion system can stably bear urea, and the properties of the sample are basically consistent compared with those of examples 1-2. Experimental results of examples 34-53 prove that the TA-100 compound emulsion system has good urea bearing capacity under all the above test conditions, has wide adjustment space of grease addition amount and compound type, and is beneficial to practical application of the technology reported by the invention in the cosmetic industry.
Examples 54 to 62: preparing TA-100 compound emulsion system samples with different urea addition amounts and urea compositions or derivatives.
Appropriate amounts of phase A, phase B and phase C were weighed into three beakers as shown in Table 6 and heated in a 90℃water bath for 30min, respectively. Homogenizing the phase A by using a table homogenizer at 5000rpm for 2min to uniformly disperse the phase A; homogenizing at 5000rpm, adding phase B while it is hot, and homogenizing for 2min; the homogenization was continued at 5000rpm, phase C was added to the mixed sample while hot, and after phase C was added, the homogenization was continued for 5min. After this time the beaker was sealed with PE film and the sample was allowed to stand at room temperature overnight. Adding phase D the next day, homogenizing at 5000rpm for 3min at room temperature again using a table homogenizer to uniformly mix the sample, sealing the beaker with PE film, and keeping the sample for use.
Table 6 shows the amounts of the respective raw materials of examples 54 to 62.
TABLE 6
The emulsification system of examples 54-62 was the same as examples 1-2, fixed at 5% TA-100 and 2% H-MY. The preparation amount of each sample is 200g, and the sample preparation process also adopts a concentrated water phase method consistent with the embodiment 1-2. Wherein, examples 54-61 are compounded with 6% white vaseline, on the basis of which the influence of urea addition amount, urea derivative and urea composition on the properties of the sample is examined. Example 62 5 oils were emulsified (oil blend ratio same as example 42) and urea compositions were formulated.
Test example 3: stability test of examples 54 to 62
After measuring the pH and viscosity of the samples of fresh examples 54-62, each sample was equally divided into 2 transparent PET bottles of 150ml, and after the cap was closed and screwed, the samples were placed in a incubator of 25℃and an incubator of 48℃respectively. And taking out the sample from the incubator at regular intervals, standing for 6 hours, cooling to room temperature, measuring the pH and viscosity of the sample, observing the properties of the sample, and returning the sample to the incubator after the measurement is finished.
Table 7 shows the pH and viscosity at each test time point for examples 54-62 (see examples 1-2 and examples 42-43 for comparison).
TABLE 7
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Table 7 summarizes the pH and viscosity at various test time points for examples 54-62 and compares the data for examples 1-2 and examples 42-43. Wherein examples 1-2 and examples 54-59 examined the effect of 8 different urea additions on the properties of the compounded emulsifying system, and the order of urea additions was: 0% (example 1), 0.1% (example 54), 0.2% (example 55), 0.5% (example 56), 1% (example 57), 2% (example 58), 5% (example 2), and 10% (example 59). Example 60 and example 61 are identical to the substrates of the previous examples, but are formulated with urea composition (5% urea +5% glycine +0.5% triethyl citrate) and urea derivative (5% hydroxyethyl urea), respectively. Example 62 multiple oils were formulated (emulsified oils and fats as in example 42) and urea compositions were formulated to simulate a complex system approaching the actual formulation of a cosmetic.
After the sample (example 54) containing 0.1% urea was left at room temperature for 1 month, the pH value was slightly increased from 4.92 to 6.19, and the viscosity of the sample was 2730 mPas, which was slightly increased as compared with 1750 mPas of the freshly prepared sample. After 1 month of standing at 48 ℃, the pH of the sample increased from 4.92 to 7.98. The viscosities of the samples at 48℃for 1 week, 2 weeks and 1 month were 1020 mPas, 850 mPas and 608 mPas, respectively, and tended to decrease gradually from 1750 mPas of the freshly prepared samples.
After the sample (example 55) containing 0.2% urea was left at room temperature for 1 month, the pH value was slightly increased from 5.09 to 5.20, and the viscosity of the sample was 2630 mPas, which was higher than that of the freshly prepared sample 1780 mPas. After 1 month of standing at 48 ℃, the pH of the sample increased from 5.09 to 8.50. The viscosities of the samples at 48℃for 1 week, 2 weeks and 1 month were 780 mPas, 580 mPas and 408 mPas, respectively, and tended to decrease gradually from 1750 mPas of the freshly prepared samples.
After the sample (example 56) containing 0.5% urea was left at room temperature for 1 month, the pH value increased from 5.04 to 5.66, and the viscosity of the sample was 2170 mPas, which was slightly higher than that of the freshly prepared sample 1950 mPas. After 1 month of standing at 48 ℃, the pH of the sample increased from 5.04 to 8.82. The viscosities of the samples for 1 week, 2 weeks and 1 month at 48℃were 530 mPas, 750 mPas and 2142 mPas, respectively, and tended to decrease and then increase compared to 1950 mPas of the freshly prepared samples.
After 1 month of standing at room temperature, the pH of the sample (example 57) containing 1% urea increased from 5.09 to 6.20, and the viscosity of the sample was 1620 mPas, which was slightly lower than that of the freshly prepared sample 1900 mPas. After 1 month of standing at 48 ℃, the pH of the sample increased from 5.09 to 8.97. The viscosities of the samples at 48℃for 1 week, 2 weeks and 1 month were 520 mPas, 1050 mPas and 10830 mPas, respectively, and tended to decrease and then increase significantly compared to 1900 mPas of the freshly prepared samples.
After the sample (example 58) containing 2% urea was left at room temperature for 1 month, the pH value was increased from 5.13 to 6.71, and the viscosity of the sample was 1030 mPas, which was slightly lower than that of the freshly prepared sample 1180 mPas. After 1 month of standing at 48 ℃, the pH of the sample increased from 5.13 to 9.08. The viscosities of the samples at 48℃for 1 week, 2 weeks and 1 month were 1270 mPas, 6920 mPas and 16250 mPas, respectively, and tended to rise gradually from 1180 mPas of the freshly prepared samples.
After the sample (example 59) compounded with 10% urea was left to stand at room temperature for 1 month, the pH value thereof increased from 5.64 to 7.62, the viscosity of the sample was 600 mPas, and the viscosity was significantly lower than that of the freshly prepared sample 1780 mPas. After 1 month of standing at 48 ℃, the pH of the sample increased from 5.64 to 9.15. The viscosities of the samples at 48℃for 1 week, 2 weeks and 1 month were 15630 mPas, 10050 mPas and 11750 mPas respectively, which increased significantly and remained substantially stable compared to 1780 mPas of the freshly prepared samples.
After 1 month of standing at room temperature, the pH of the sample of the urea composition (example 60) was slightly lowered from 5.59 to 5.58, and the viscosity of the sample was 500 mPas, which was lower than that of the freshly prepared sample of 820 mPas. After 1 month of standing at 48 ℃, the pH of the sample rose slightly from 5.59 to 5.89. The viscosities of the samples at 48℃for 1 week, 2 weeks and 1 month were 4330 mPas, 8200 mPas and 13580 mPas, respectively, and were gradually increased compared with the 820 mPas of the freshly prepared samples.
After the sample (example 61) compounded with 5% hydroxyethyl urea was left to stand at room temperature for 1 month, the pH value thereof was slightly lowered from 8.42 to 8.16, and the viscosity of the sample was 6820 mPas, which was slightly lowered as compared with the freshly prepared sample 8330 mPas. After 1 month of standing at 48 ℃, the pH of the sample rose slightly from 8.42 to 8.92. The viscosities of the samples at 48℃for 1 week, 2 weeks and 1 month were 8200 mPas, 10000 mPas and 8120 mPas, respectively, and were slightly increased compared with 8330 mPas of the freshly prepared sample.
After the sample (example 62) containing the plurality of oils and urea compositions was left at room temperature for 1 month, the pH value was reduced from 6.76 to 6.19, the viscosity of the sample was 620 mPas, and the viscosity was increased to a small extent as compared with the fresh sample 458 mPas. After 1 month of standing at 48 ℃, the pH of the sample was reduced from 6.76 to 5.93. The viscosities of the samples at 48℃for 1 week, 2 weeks and 1 month were 5025 mPas, 20170 mPas and 11530 mPas, respectively, and the viscosity was significantly higher than that of the freshly prepared sample at 458 mPas.
The above experimental results can be summarized as follows:
(1) The TA-100 compound emulsion system can bear urea, urea derivatives and urea compositions with different addition amounts, and all samples have no layering and demulsification problems.
(2) Samples with low urea complex amount (0.1% -0.2%, examples 54-55) show a decreasing trend in viscosity in the high temperature time-dependent strengthening test; samples with lower urea dosing (0.5% -1%, examples 56-57) had viscosity rising and then falling during the high temperature time-dependent fortification test; samples with higher urea dosing (2% -10%, examples 2 and examples 58-59) had an increasing viscosity during the high temperature time-dependent boost test. This phenomenon may be derived from the water-soluble anionic small molecules produced by urea decomposition that promote reconstitution of TA-100 micelles. Under the conditions of low urea content and less decomposition products, the existing micelle structure is destroyed to reduce the viscosity of the material; however, when the urea amount is high and the decomposition products are large, the formation of new micelles having a high degree of polymerization is promoted, and the viscosity of the material is remarkably increased. The experimental result shows that the TA-100 compound emulsifying system has unique properties more easily when the urea with higher content is compounded, and has practical value in the formula of adding the urea with efficacy.
(3) Example 60 and example 61 were formulated with urea compositions and urea derivatives based on example 1, both of which stably supported urea and had properties similar to other formulated urea samples. It should be noted that the pH of the two samples did not rise significantly, indicating that urea does not merely occur under strongly alkaline conditions to promote TA-100 micelle reconstitution. The TA-100 compound emulsion system reported by the invention can show unique properties on the premise of meeting the national cosmetic regulation on the sample pH supervision standard.
(4) Example 62 multiple greases were formulated on the basis of example 60, the samples behaving substantially in accordance with the latter in the stability test. The emulsion system reported by the invention still has good bearing property and unique tackifying performance, which indicates that the compound emulsion system has wide grease and additive placing adjustment space, and is beneficial to the application in cosmetics.
Examples 63 to 88: and (3) adjusting the adding amount of TA-100, the adding type and the adding amount of long-chain fatty alcohol, and preparing a TA-100 composite emulsifying system sample and a corresponding urea-containing sample.
Appropriate amounts of phase A, phase B and phase C were weighed into three beakers as shown in Table 8 and heated in a 90℃water bath for 30min, respectively. Homogenizing the phase A by using a table homogenizer at 5000rpm for 2min to uniformly disperse the phase A; homogenizing at 5000rpm, adding phase B while it is hot, and homogenizing for 2min; the homogenization was continued at 5000rpm, phase C was added to the mixed sample while hot, and after phase C was added, the homogenization was continued for 5min. After which the beaker was sealed with PE film and the sample was allowed to stand at room temperature overnight. Adding phase D the next day, homogenizing at 5000rpm for 3min at room temperature again using a table homogenizer to uniformly mix the sample, sealing the beaker with PE film, and keeping the sample for use.
Table 8 shows the types of the long-chain fatty alcohols added in examples 63 to 88 and the amounts of the respective materials fed.
TABLE 8
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Examples 63-88 were fixed by a concentrated aqueous phase method with an oil addition of 6% white petrolatum and each sample was formulated at 200g. Among them, examples 63 to 78 were carried out with the TA-100 content fixed at 5%, and on the basis of this, the effect of the amount of the long-chain fatty alcohol added and the type of the added on the properties of the material was examined. Examples 79-88 fix long chain fatty alcohols to 2% H-MY, the effect of TA-100 addition on the bulk properties was examined. Each sample was prepared separately as a base stock and as a urea-containing example, with the urea addition of the urea-containing example being 5%.
Test example 4: stability test of examples 63-88
After measuring the pH and viscosity of the samples of the new examples 63 to 88, each sample was equally divided into 2 transparent PET bottles of 150ml, and after the cap was closed and screwed, the samples were placed in a incubator of 25℃and an incubator of 48℃respectively. And taking out the sample from the incubator at regular intervals, standing for 6 hours, cooling to room temperature, measuring the pH and viscosity of the sample, observing the properties of the sample, and returning the sample to the incubator after the measurement is finished.
Table 9 shows the pH and viscosity at each test time point for examples 63-88 (see examples 1-2).
TABLE 9
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Table 9 summarizes the pH and viscosity at various test time points for examples 63-88 and compares the data for examples 1-2. Wherein examples 1-2 and examples 63-74 examined the effect of 7 different H-MY additions, in order according to the H-MY addition: 0% (examples 63-64), 0.5% (examples 65-66, 1% (examples 67-68), 2% (examples 1-2), 3% (examples 69-70), 4% (examples 71-72), and 5% (examples 73-74), examples 75-76, and examples 77-78 were formulated with 2% behenyl alcohol and 2% cetyl alcohol, respectively.
After the sample (example 63) without the long-chain fatty alcohol was left at room temperature for 1 month, the pH value was 6.06, which was slightly raised from the initial value of 5.61; the sample viscosity was 1042 mPas, which was higher than that of the freshly prepared sample 620 mPas. After 1 month of standing at 48 ℃, the pH of the sample was 5.35, which was slightly lower than the initial value, and the viscosity was 617 mPas, which was substantially consistent with the freshly prepared sample. After 1 month at room temperature, the pH of the sample (example 64) formulated with 5% urea increased from 5.90 to 7.38 and the viscosity decreased slightly from 1030 mPas to 783 mPas. The viscosity of the sample drops significantly after 1 month at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 280 mPas, 280 mPas and 280 mPas respectively, compared with the viscosity of the freshly prepared samples. At the same time, the sample pH also increased from 5.90 to 8.98. It is necessary to point out that the above samples all show solid lumps, which are caused by insufficient stability of the emulsion system, and consequently cause grease to precipitate and agglomerate. The experimental results show that the TA-100 emulsifying system without compounding long-chain fatty alcohol can not stably emulsify grease, and the phenomenon that the viscosity is obviously increased in a high-temperature time stability test after compounding urea is also not observed.
A sample with a cetostearyl alcohol (H-MY) dosage of 0.5% (example 65) had a pH of 5.68 after 1 month at room temperature, which increased slightly from the initial value of 5.31; the sample viscosity was 400 mPas, which was slightly higher than the 380 mPas of the freshly prepared sample. After 1 month of standing at 48℃the pH of the sample was 4.97, which decreased slightly from the initial value, and the viscosity was 725 mPas, which increased slightly from the freshly prepared sample. After 1 month at room temperature, the pH of the sample (example 66) compounded with 5% urea increased from 5.62 to 7.41 and the viscosity decreased slightly from 420 mPas to 250 mPas. The viscosity of the sample decreased after 1 month at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 270 mPas, 280 mPas and 208 mPas, respectively, compared to the viscosity of the freshly prepared samples of 420 mPas. At the same time, the sample pH also increased from 5.62 to 9.00. The experimental results show that the TA-100 emulsion system compounded with 0.5% cetostearyl alcohol can bear urea, but no significant increase in viscosity in the high temperature stability test after compounding urea is observed. The properties of the low long chain fatty alcohol formulated samples are seen to be significantly different from example 2.
A sample (example 67) with a 1% compound of cetostearyl alcohol (H-MY) had a pH of 5.49 and increased slightly from the initial value of 5.31 after 1 month at room temperature; the sample viscosity was 358 mPas, which was slightly lower than that of the freshly prepared sample 430 mPas. After 1 month of standing at 48℃the pH of the sample was 4.81, which was lower than the initial value, and the viscosity was 575 mPas, which was slightly higher than the freshly prepared sample. After 1 month at room temperature, the pH of the sample of 5% urea (example 68) was raised from 5.65 to 7.46 and the viscosity was lowered from 670 mPas to 267 mPas. The viscosity of the sample showed a significant increase after 1 month at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 2880 mPas, 5330 mPas and 7920 mPas, respectively, compared with the viscosity of the freshly prepared samples. At the same time, the sample pH also increased from 5.65 to 9.00. The experimental results show that the TA-100 emulsion system compounded with 1% cetostearyl alcohol can bear urea and the properties are basically consistent compared with example 2.
After 1 month at room temperature, the sample with a 3% compound of cetostearyl alcohol (H-MY) (example 69) had a pH of 5.62 and increased slightly from the initial value of 5.32; the sample viscosity was 9630 mPas, which was slightly higher than 7780 mPas of the freshly prepared sample. After 1 month of standing at 48℃the pH of the sample was 4.79, which was somewhat lower than the initial value, while the viscosity was 8450 mPas, which was slightly higher than the freshly prepared sample. After 1 month of standing at room temperature, the pH of the sample (example 70) compounded with 5% urea increased from 5.76 to 7.63 and the viscosity decreased slightly from 36420 mPas to 31580 mPas. The viscosity of the sample tended to decrease slightly after being left at 48℃for 1 month. The viscosities of the samples for 1 week, 2 weeks and 1 month at 48℃were 23580 mPas, 23000 mPas and 21670 mPas, respectively, compared to the viscosity of the freshly prepared samples 36420 mPas. At the same time, the sample pH also increased from 5.76 to 9.06. The experimental results show that the TA-100 emulsifying system compounded with 3% cetylstearyl alcohol can bear urea, and the difference from example 2 is that the viscosity of the sample is obviously increased immediately after the urea is compounded, and the viscosity of the urea-containing sample is slightly reduced in a high-temperature time test, so that the TA-100 compound emulsifying system can show unique properties due to the higher adding amount of cetylstearyl alcohol.
After a sample (example 71) having a compound amount of 4% cetylstearyl alcohol (H-MY) was left at room temperature for 1 month, the pH was 5.62, which was slightly higher than the initial value of 5.16; the sample viscosity was 32580 mPas and was slightly lower than the 36830 mPas of the freshly prepared sample. After 1 month of standing at 48℃the pH of the sample was 5.79, which was slightly higher than the initial value, and the viscosity was 35330 mPas, which was slightly lower than the freshly prepared sample. After 1 month of standing at room temperature, the pH of the sample (example 72) compounded with 5% urea increased from 5.79 to 7.83, and the viscosity of 53420 mPas was consistent with the freshly prepared sample. The viscosity of the sample tended to rise slightly after 1 month at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 48420 mPas, 59920 mPas and 65170 mPas, respectively, compared to the viscosity of the freshly prepared samples 53420 mPas. At the same time, the sample pH also increased from 5.79 to 8.94. The experimental result shows that the TA-100 emulsifying system compounded with 4% cetostearyl alcohol can bear urea, and the urea-containing sample has a small ascending trend in a high-temperature time stability test. Unlike example 2, a significant increase in the viscosity of the sample immediately after compounding urea occurred.
A sample with a cetostearyl alcohol (H-MY) dosage of 5% (example 73) had a pH of 5.57 after 1 month at room temperature, which increased slightly from the initial value of 5.05; the sample viscosity was 32580 mPas, which was lower than the 45250 mPas of the freshly prepared sample. After 1 month of standing at 48℃the pH of the sample was 5.90, which was higher than the initial value, and the viscosity was 35000 mPas, which was lower than the freshly prepared sample. After a sample of 5% urea (example 74) was left at room temperature for 1 month, the pH increased from 5.79 to 7.99 and the viscosity increased from 53420 mPas to 66250 mPas. The viscosity of the sample tended to rise after 1 month at 48 ℃. The viscosities of the samples placed at 48℃for 1 week, 2 weeks and 1 month were 48420 mPas, 61630 mPas and 73080 mPas, respectively, compared to the viscosity of the freshly prepared samples 53420 mPas. At the same time, the sample pH also increased from 5.79 to 8.96. The experimental results show that the TA-100 emulsion system compounded with 5% cetostearyl alcohol can bear urea, and the urea-containing sample is in an ascending trend in a high-temperature time stability test consistent with example 2.
After 1 month at room temperature, the sample (example 75) formulated with 2% behenyl alcohol (i.e., behenyl alcohol) had a pH of 5.28, which increased slightly from the initial value of 4.88; the sample viscosity was 8250 mPas, which was lower than that of the freshly prepared sample 13580 mPas. After 1 month of standing at 48℃the pH of the sample was 5.12, which increased somewhat from the initial value, while the viscosity was 10500 mPas, which decreased slightly from the freshly prepared sample. After a sample of 5% urea was compounded (example 76), the pH was raised from 5.54 to 7.67 and the viscosity was lowered from 14170 mPas to 7500 mPas after 1 month standing at room temperature. The viscosity of the sample tended to rise after 1 month at 48 ℃. The viscosities of the samples for 1 week, 2 weeks and 1 month at 48℃were 15670 mPas, 26080 mPas and 27250 mPas, respectively, compared to the viscosity of the freshly prepared samples 14170 mPas. At the same time, the sample pH also increased from 5.54 to 9.06. The experimental result shows that the TA-100 emulsifying system compounded with 2% of behenyl alcohol can bear urea, and the urea-containing sample is in an ascending trend in a high-temperature time stability test. However, the initial viscosity of the corresponding samples was higher than in examples 1 and 2, indicating that the longer carbon chain of behenyl alcohol contributed to the formation of the formulation viscosity.
After 1 month at room temperature, the pH of the sample (example 77) formulated with 2% cetyl alcohol was 5.68, which increased slightly from the initial value of 5.42; the sample viscosity was 2325 mPas, which was elevated compared to 1700 mPas of the freshly prepared sample. After 1 month of standing at 48℃the pH of the sample was 6.70, which was slightly higher than the initial value, while the viscosity was 750 mPas, which was significantly lower than the freshly prepared sample. After 1 month at room temperature, the pH of the sample (example 78) compounded with 5% urea increased from 5.92 to 7.27 and the viscosity increased from 2920 mPas to 5258 mPas. The viscosity of the sample tended to rise after 1 month at 48 ℃. The viscosities of the samples placed at 48℃for 1 week, 2 weeks and 1 month were 10880 mPas, 16170 mPas and 15670 mPas, respectively, compared to 2920 mPas of the freshly prepared samples. At the same time, the sample pH also increased from 5.92 to 9.26. The experimental results show that the TA-100 emulsion system compounded with 2% cetyl alcohol can bear urea, and the properties of the related samples are basically consistent with those of examples 1-2.
The experimental results show that the prepared sample can stably bear urea after TA-100 is compounded with proper types and addition amount of long-chain fatty alcohol. However, with the different amounts and types of fatty alcohol compounding, the following characteristics were found in the experiment:
(1) The sample emulsion system without the long-chain fatty alcohol has poor stability, and oil blocks are generated due to oil phase aggregation caused by demulsification in the stability test.
(2) After compounding the urea, the low-content long-chain fatty alcohol samples (0.5% and examples 65-67) did not have a significant viscosity rise in the high-temperature stability over time test.
(3) After compounding the high-content long-chain fatty alcohol sample (> 3%, examples 69-74) and compounding the urea, the instant viscosity is obviously increased.
(4) Samples of formulated behenyl alcohol (examples 76-77) showed a higher viscosity than samples of cetyl stearyl alcohol and cetyl alcohol formulated at the same level.
The experiment shows that the TA-100 compound emulsifying system has wide space in the selection of the type and the compound amount of the long-chain fatty alcohol. The viscosity of the material can be adjusted by adjusting the adding type and the adding amount of the long-chain fatty alcohol so as to meet the requirements of the viscosity of cosmetic formulas of different types, thereby being beneficial to the practical application of the invention in the cosmetic industry. In addition, when the compounding amount of the long-chain fatty alcohol is higher, the viscosity of the sample after urea is added is obviously increased, which shows that the compound emulsion system reported by the invention has more advantages in the application of cream or high-viscosity emulsion.
Examples 1-2 and examples 79-88 examined the effect of 6 different TA-100 additions, in order according to the TA-100 addition: 0% (examples 79-80), 0.5% (examples 81-82), 2.5% (examples 83-84), 5% (examples 1-2), 7.5% (examples 85-86), and 10% (examples 87-88).
After a sample without TA-100 added (example 79) was left for one month at room temperature, the pH was slightly lowered from 4.88 to 4.62; in addition, because the emulsifying capacity and the suspension force of the formula are too low, material delamination and demulsification are found at each test time point. After 1 month of standing at 48 ℃, the samples were also layered and demulsified at various time points, and the pH of the samples after stability testing was 4.57, with a small decrease from the initial value. After 1 month of standing at room temperature, the pH of the sample (example 80) formulated with 5% urea increased from 6.13 to 8.29, and the sample had delamination and demulsification at each time point. After the sample was left at 48℃for 1 month, the pH of the sample was raised from 9.17, and the samples were aliquoted and demulsified at each test time. The experimental results show that the sample without the TA-100 has no capability of emulsifying and supporting the material body, and can not stably bear urea, thus proving the core effect of the TA-100 in the compound emulsifying system.
After the TA-100 complex formulation of 0.5% of the complex emulsion system (example 81) was left for one month at room temperature, the pH of the sample was slightly reduced from 5.38 to 4.87; samples were layered at each time point. After 1 month of standing at 48 ℃, the samples still delaminate at various time points due to too low viscosity, and the pH of the samples after stability testing was 4.85, which was slightly lower than the initial value. After 1 month of standing at room temperature, the pH of the sample (example 82) formulated with 5% urea increased from 6.18 to 8.23, and the sample still delaminated at each time point. However, example 82 exhibited unique properties in the test at 48℃ Gao Wenjing, and the viscosity of the samples placed at 48℃for 1 week, 2 weeks and 1 month were 1350 mPas, 4458 mPas and 18250 mPas, respectively, with a significant tendency to rise from the initial values. The experimental result shows that the TA-100 compound amount is 0.5% of the compound emulsion system, namely the phenomenon that the viscosity is obviously increased in the high-temperature time test is shown. The discovery means that the TA-100 with lower concentration can be compounded with other surfactants, namely the urea bearing capacity of the TA-100 can be improved, so that the formula which cannot bear urea stably originally can meet the regulatory requirement of national regulation on the stability of cosmetics, and the TA-100 has high value in practical application of the cosmetics industry.
The sample with a TA-100 dose of 2.5% (example 83) had a pH of 4.97 after 1 month at room temperature, which was reduced from the initial value of 5.60; the sample viscosity was 383 mPas, which was slightly higher than the 370 mPas of the freshly prepared sample. After 1 month at 48℃the pH of the sample was 4.85, which was lower than the initial value, and the viscosity was 542 mPas, which was higher than the fresh sample. After 1 month of standing at room temperature, the pH of the sample of 5% urea (example 84) was raised from 6.13 to 8.17 and the viscosity was slightly reduced from 420 mPas to 383 mPas. The viscosity of the sample showed a significant increase after 1 month at 48 ℃. The viscosities of the samples left at 48℃for 1 week, 2 weeks and 1 month were 24200 mPas, 23500 mPas and 63920 mPas, respectively, compared to the viscosity of the freshly prepared samples of 420 mPas. At the same time, the sample pH also increased from 6.13 to 9.24. The experimental results show that the compound emulsion system with the TA-100 addition amount of 2.5% can bear urea, and the properties of the related samples are basically consistent with those of the examples 1-2.
The sample with a TA-100 dose of 7.5% (example 85) had a pH of 4.89 after 1 month at room temperature and decreased slightly from the initial value of 5.23; the sample viscosity was 28170 mPas, which was slightly higher than 27000 mPas of the freshly prepared sample. After 1 month of standing at 48℃the pH of the sample was 4.79, which decreased slightly from the initial value, and the viscosity was 23670 mPas, which also decreased slightly from the freshly prepared sample. After 1 month of standing at room temperature, the pH of the sample of 5% urea (example 86) was increased from 6.15 to 7.67 and the viscosity was decreased from 41420 mPas to 25500 mPas. The viscosity of the sample tended to decrease and then increase after being left to stand at 48℃for 1 month. The viscosities of the samples placed at 48℃for 1 week, 2 weeks and 1 month were 12930 mPas, 25670 mPas and 55300 mPas, respectively, compared to the viscosity of the freshly prepared samples 41420 mPas. At the same time, the sample pH also increased from 6.15 to 9.14. The experimental results show that the compound emulsion system with the TA-100 addition amount of 7.5% can bear urea, and the properties of the related samples are basically consistent with those of the examples 1-2.
A sample with a TA-100 dose of 10% (example 87) had a pH of 4.97 after 1 month at room temperature and was slightly lower than the initial value of 5.08; the sample viscosity was 30420 mPas, which was slightly higher than the newly prepared sample 29080 mPas. After 1 month of standing at 48℃the pH of the sample was 4.90, which was slightly lower than the initial value, and the viscosity was 28330 mPas, which was slightly lower than the freshly prepared sample. After 1 month at room temperature, the pH of the sample of 5% urea (example 88) was raised from 5.58 to 7.47 and the viscosity was lowered from 49180 mPas to 23920 mPas. The viscosity of the sample tended to decrease and then increase after being left to stand at 48℃for 1 month. The viscosities of the samples placed at 48℃for 1 week, 2 weeks and 1 month were 16270 mPas, 45500 mPas and 85700 mPas, respectively, compared to the viscosity of the freshly prepared samples 49180 mPas. At the same time, the sample pH also increased from 5.58 to 9.24. The experimental results show that the compound emulsion system with the TA-100 addition amount of 10% can bear urea, and the properties of the related samples are basically consistent with those of examples 1-2.
The experimental results show that the prepared compound emulsion system can stably bear urea within a wider TA-100 compound range after the dosage and the variety of the long-chain fatty alcohol are fixed. However, depending on the amount of TA-100 compounded, the following properties were found in the experiment:
(1) Samples without TA-100 (examples 79-80) did not possess oil emulsifying and structural supporting capabilities and had problems of delamination and demulsification under all test conditions. The phenomenon of tackifying in a high-temperature time test after the urea is compounded is not shown, and the key effect of TA-100 in a compound system is proved.
(2) Compounding the sample with low TA-100 content (0.5%, example 81), delamination due to insufficient levitation force; however, after urea is compounded (example 82), the viscosity of the material body is obviously improved in a high-temperature time stability test, and the sample with lower TA-100 addition amount has the characteristic of high-temperature tackifying after the urea is compounded. The discovery explains a brand new formulation design thought, and the compounding use of a small amount of TA-100 and other emulsifying systems is beneficial to improving the bearing capacity of urea of the TA-100, so that the requirement of national law on the stability of cosmetics is met.
(3) The viscosity of the sample compounded with high TA-100 content (> 5% and examples 85-88) is obviously increased immediately after urea is compounded, and the viscosity is firstly decreased and then increased in the high-temperature time stability test, probably because the urea decomposition product promotes the micelle reconstruction of TA-100.
In conclusion, the compound emulsifying system reported by the invention has the capability of stably bearing urea in a wider range of TA-100 compound amount. The viscosity of the material body can be changed by adjusting the addition amount of TA-100, which is beneficial to the application of the technology reported by the invention in various cosmetic formulations.
The following are examples of specific applications of the composite system in skin external preparations, and formulations and preparation methods of these dosage forms. In the following tables, "-" indicates no addition.
Application example 1: preparation of face cream
Application example 2: preparation of the emulsion
Application example 3: preparation of essence
Application example 4: preparation of facial mask
Application example 5: preparation of eye cream
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Application example 6: preparation of the spray
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Claims (7)
1. A stable composition carrying urea or a derivative thereof, the composition consisting of:
(a) 0.1-20 wt% of grease;
(b) 2.5-10 wt% of a cationic emulsifier which is distearyldimethyl ammonium chloride;
(c) 1-5 wt% of a long chain fatty alcohol having a carbon chain length of 16-22;
(d) An aqueous phase;
wherein the composition comprises more than 2% by weight of urea or a derivative thereof,
wherein the urea derivative is a hydroxyalkanoate with carbon number of 1-6 of urea,
wherein the weight ratio of the cationic emulsifier to the long chain fatty alcohol is 5:2, and the weight ratio of the cationic emulsifier to the supported urea or the derivative thereof is 1:2 to 10:1.
2. The composition of claim 1, wherein the grease is selected from the group consisting of: a non-polar solid fat; a non-polar liquid fat; polar liquid grease; polar solid grease; silicone oil; or mixtures thereof.
3. The composition of claim 1, wherein the composition comprises 1-20% by weight of grease.
4. The composition of claim 1, wherein the long chain fatty alcohol is selected from the group consisting of: cetyl alcohol, cetostearyl alcohol, stearyl alcohol, arachidyl alcohol, behenyl alcohol, or mixtures thereof.
5. The composition of claim 1, wherein the composition comprises 2-10% by weight urea or a derivative thereof.
6. The composition of claim 1, wherein the composition comprises greater than 50% by weight of the aqueous phase.
7. A skin external agent comprising the composition according to any one of claims 1 to 6.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110956699.9A CN113648232B (en) | 2021-08-19 | 2021-08-19 | Stable composition carrying urea or derivatives thereof |
| PCT/CN2022/110469 WO2023020299A1 (en) | 2021-08-19 | 2022-08-05 | Stable composition carrying urea or derivative thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110956699.9A CN113648232B (en) | 2021-08-19 | 2021-08-19 | Stable composition carrying urea or derivatives thereof |
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| Publication Number | Publication Date |
|---|---|
| CN113648232A CN113648232A (en) | 2021-11-16 |
| CN113648232B true CN113648232B (en) | 2024-01-23 |
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| CN202110956699.9A Active CN113648232B (en) | 2021-08-19 | 2021-08-19 | Stable composition carrying urea or derivatives thereof |
Country Status (2)
| Country | Link |
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| CN (1) | CN113648232B (en) |
| WO (1) | WO2023020299A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113648232B (en) * | 2021-08-19 | 2024-01-23 | 上海家化联合股份有限公司 | Stable composition carrying urea or derivatives thereof |
| FR3130145A1 (en) * | 2021-12-15 | 2023-06-16 | L'oreal | High urea skin conditioning cosmetic composition |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112515992A (en) * | 2020-12-08 | 2021-03-19 | 上海家化联合股份有限公司 | Stable composition comprising triethyl citrate and glycine |
| CN112515994A (en) * | 2020-12-08 | 2021-03-19 | 上海家化联合股份有限公司 | Stable composition comprising urea |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050113268A1 (en) * | 2003-11-26 | 2005-05-26 | Landa Peter A. | Increased moisturization efficacy using hydroxyalkylurea |
| JP2005330242A (en) * | 2004-05-21 | 2005-12-02 | Shiseido Co Ltd | W/o type emulsion preparation |
| JP2005330243A (en) * | 2004-05-21 | 2005-12-02 | Shiseido Co Ltd | W/o type emulsion preparation |
| DE102006034533A1 (en) * | 2006-07-24 | 2008-01-31 | Beiersdorf Ag | Cosmetic preparation, useful e.g. for hair restructuring, for topical application on skin and/or hair and to prepare shampoo, comprises hydroxyalkyl-urea derivative and cationic caring agent such as cationic- surfactant and/or polymer |
| US20080299054A1 (en) * | 2007-05-30 | 2008-12-04 | Conopco, Inc., D/B/A Unilever | Personal care compositions with enhanced fragrance delivery |
| CN113648232B (en) * | 2021-08-19 | 2024-01-23 | 上海家化联合股份有限公司 | Stable composition carrying urea or derivatives thereof |
-
2021
- 2021-08-19 CN CN202110956699.9A patent/CN113648232B/en active Active
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- 2022-08-05 WO PCT/CN2022/110469 patent/WO2023020299A1/en unknown
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112515992A (en) * | 2020-12-08 | 2021-03-19 | 上海家化联合股份有限公司 | Stable composition comprising triethyl citrate and glycine |
| CN112515994A (en) * | 2020-12-08 | 2021-03-19 | 上海家化联合股份有限公司 | Stable composition comprising urea |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113648232A (en) | 2021-11-16 |
| WO2023020299A1 (en) | 2023-02-23 |
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