WO2023020299A1 - 承载尿素或其衍生物的稳定组合物 - Google Patents
承载尿素或其衍生物的稳定组合物 Download PDFInfo
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- WO2023020299A1 WO2023020299A1 PCT/CN2022/110469 CN2022110469W WO2023020299A1 WO 2023020299 A1 WO2023020299 A1 WO 2023020299A1 CN 2022110469 W CN2022110469 W CN 2022110469W WO 2023020299 A1 WO2023020299 A1 WO 2023020299A1
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- urea
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- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 305
- 239000004202 carbamide Substances 0.000 title claims abstract description 262
- 239000000203 mixture Substances 0.000 title claims abstract description 127
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 45
- 125000002091 cationic group Chemical group 0.000 claims abstract description 33
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 27
- 239000004519 grease Substances 0.000 claims abstract description 16
- 239000008346 aqueous phase Substances 0.000 claims abstract description 15
- 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 9
- 239000004664 distearyldimethylammonium chloride (DHTDMAC) Substances 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 28
- 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 23
- 239000003093 cationic surfactant Substances 0.000 claims description 19
- 229940081733 cetearyl 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
- 239000007787 solid Substances 0.000 claims description 10
- 229960000541 cetyl alcohol Drugs 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- BTFJIXJJCSYFAL-UHFFFAOYSA-N arachidyl alcohol Natural products CCCCCCCCCCCCCCCCCCCCO BTFJIXJJCSYFAL-UHFFFAOYSA-N 0.000 claims description 3
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 229940012831 stearyl alcohol Drugs 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 7
- 150000001721 carbon Chemical group 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 238000004945 emulsification Methods 0.000 description 71
- 150000001875 compounds Chemical class 0.000 description 68
- 238000013329 compounding Methods 0.000 description 56
- 239000003921 oil Substances 0.000 description 53
- 239000002537 cosmetic Substances 0.000 description 42
- 238000012360 testing method Methods 0.000 description 39
- 210000003491 skin Anatomy 0.000 description 38
- 230000000087 stabilizing effect Effects 0.000 description 35
- 239000012071 phase Substances 0.000 description 34
- 238000013112 stability test Methods 0.000 description 32
- 230000003247 decreasing effect Effects 0.000 description 29
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 26
- 239000000463 material Substances 0.000 description 23
- 229920000642 polymer Polymers 0.000 description 18
- 239000002562 thickening agent Substances 0.000 description 18
- 239000003871 white petrolatum Substances 0.000 description 18
- 238000007792 addition Methods 0.000 description 17
- 238000009472 formulation Methods 0.000 description 17
- 230000000694 effects Effects 0.000 description 16
- 239000004094 surface-active agent Substances 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 235000019271 petrolatum Nutrition 0.000 description 14
- 239000004471 Glycine Substances 0.000 description 13
- -1 zinc salts Chemical class 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 12
- 239000001069 triethyl citrate Substances 0.000 description 12
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 description 12
- 235000013769 triethyl citrate Nutrition 0.000 description 12
- 229920002553 poly(2-methacrylolyloxyethyltrimethylammonium chloride) polymer Polymers 0.000 description 9
- 239000004698 Polyethylene Substances 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 8
- 230000032798 delamination Effects 0.000 description 8
- 238000000265 homogenisation Methods 0.000 description 8
- 238000000354 decomposition reaction Methods 0.000 description 7
- 230000001804 emulsifying effect Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 238000013517 stratification Methods 0.000 description 7
- 239000006071 cream Substances 0.000 description 6
- 230000014509 gene expression Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000000693 micelle Substances 0.000 description 6
- 230000003020 moisturizing effect Effects 0.000 description 6
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 6
- ARIWANIATODDMH-UHFFFAOYSA-N rac-1-monolauroylglycerol Chemical compound CCCCCCCCCCCC(=O)OCC(O)CO ARIWANIATODDMH-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 6
- 239000000725 suspension Substances 0.000 description 6
- 230000036962 time dependent Effects 0.000 description 6
- 239000000230 xanthan gum Substances 0.000 description 6
- 229920001285 xanthan gum Polymers 0.000 description 6
- 229940082509 xanthan gum Drugs 0.000 description 6
- 235000010493 xanthan gum Nutrition 0.000 description 6
- CLAHOZSYMRNIPY-UHFFFAOYSA-N 2-hydroxyethylurea Chemical group NC(=O)NCCO CLAHOZSYMRNIPY-UHFFFAOYSA-N 0.000 description 5
- 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
- 230000009286 beneficial effect Effects 0.000 description 5
- 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 5
- 239000011159 matrix material Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 229920000223 polyglycerol Polymers 0.000 description 5
- 229940083037 simethicone Drugs 0.000 description 5
- ODFAPIRLUPAQCQ-UHFFFAOYSA-M sodium stearoyl lactylate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC(=O)OC(C)C(=O)OC(C)C([O-])=O ODFAPIRLUPAQCQ-UHFFFAOYSA-M 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 206010013786 Dry skin Diseases 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 4
- 229940073642 ceteareth-30 Drugs 0.000 description 4
- 239000002552 dosage form Substances 0.000 description 4
- 230000037336 dry skin Effects 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 4
- 210000002615 epidermis Anatomy 0.000 description 4
- 229940031575 hydroxyethyl urea Drugs 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 230000008591 skin barrier function Effects 0.000 description 4
- 229940080352 sodium stearoyl lactylate Drugs 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- GWTCIAGIKURVBJ-UHFFFAOYSA-L dipotassium;dodecyl phosphate Chemical compound [K+].[K+].CCCCCCCCCCCCOP([O-])([O-])=O GWTCIAGIKURVBJ-UHFFFAOYSA-L 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 235000014593 oils and fats Nutrition 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 231100000435 percutaneous penetration Toxicity 0.000 description 3
- 229940033623 potassium lauryl phosphate Drugs 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 206010012434 Dermatitis allergic Diseases 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 201000008937 atopic dermatitis Diseases 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000001815 facial effect Effects 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 229940074046 glyceryl laurate Drugs 0.000 description 2
- 239000008131 herbal destillate Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 229940127554 medical product Drugs 0.000 description 2
- 239000000346 nonvolatile oil Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000007634 remodeling Methods 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
- FLPJVCMIKUWSDR-UHFFFAOYSA-N 2-(4-formylphenoxy)acetamide Chemical compound NC(=O)COC1=CC=C(C=O)C=C1 FLPJVCMIKUWSDR-UHFFFAOYSA-N 0.000 description 1
- JBYXPOFIGCOSSB-GOJKSUSPSA-N 9-cis,11-trans-octadecadienoic acid Chemical compound CCCCCC\C=C\C=C/CCCCCCCC(O)=O JBYXPOFIGCOSSB-GOJKSUSPSA-N 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-M 9-cis,12-cis-Octadecadienoate Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O OYHQOLUKZRVURQ-HZJYTTRNSA-M 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
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- 206010012438 Dermatitis atopic Diseases 0.000 description 1
- RGHNJXZEOKUKBD-SQOUGZDYSA-N Gluconic acid Natural products OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 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
- 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 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000000996 additive effect Effects 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
- 239000003513 alkali Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 229920006318 anionic polymer Polymers 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
- 208000010668 atopic eczema Diseases 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
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 229940074979 cetyl palmitate Drugs 0.000 description 1
- 229940125904 compound 1 Drugs 0.000 description 1
- 229940125773 compound 10 Drugs 0.000 description 1
- 229940126214 compound 3 Drugs 0.000 description 1
- 229940125898 compound 5 Drugs 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 229940108924 conjugated linoleic acid Drugs 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 230000001186 cumulative effect Effects 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
- 229940008099 dimethicone Drugs 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229940079593 drug Drugs 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
- 238000011156 evaluation Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- PXDJXZJSCPSGGI-UHFFFAOYSA-N hexadecanoic acid hexadecyl ester Natural products CCCCCCCCCCCCCCCCOC(=O)CCCCCCCCCCCCCCC PXDJXZJSCPSGGI-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- ZLVXBBHTMQJRSX-VMGNSXQWSA-N jdtic Chemical compound C1([C@]2(C)CCN(C[C@@H]2C)C[C@H](C(C)C)NC(=O)[C@@H]2NCC3=CC(O)=CC=C3C2)=CC=CC(O)=C1 ZLVXBBHTMQJRSX-VMGNSXQWSA-N 0.000 description 1
- 229940049918 linoleate Drugs 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 229940105132 myristate Drugs 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 208000008742 seborrheic dermatitis Diseases 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 208000017520 skin disease Diseases 0.000 description 1
- 230000037394 skin elasticity Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 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
- 230000008719 thickening Effects 0.000 description 1
- 230000000699 topical effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229960000306 zinc gluconate Drugs 0.000 description 1
- 235000011478 zinc gluconate Nutrition 0.000 description 1
- 239000011670 zinc gluconate Substances 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
Definitions
- the invention relates to the field of cosmetics, in particular to a stable composition carrying urea or its derivatives and its application in cosmetics.
- Urea is one of the natural moisturizing factors of the skin, and its functions of moisturizing, softening the skin, and promoting percutaneous penetration have been widely reported in the literature.
- Literature “Instrumental and Dermatologist Evaluation of the Effects of Glycerin and Urea on Dry Skin in Patients with Atopic Dermatitis", Skin Research and Technology, Lodén M. et al. reported that after 30 days of using a moisturizing cream containing 4% urea, 35 The average skin capacitance value of the subjects increased from 35A.U. to 42A.U.
- urea which has a strong skin care effect
- cosmetics or dermatological products faces many challenges.
- One of them is that the hydrolysis of urea will produce strong alkalinity and ionicity, which puts forward high requirements on the bearing capacity of the cosmetic formulation matrix.
- emulsion formulas sold by Shanghai Jahwa United Co., Ltd.
- urea has strict requirements on the carrying capacity of the formulation system, the carrying capacity of most commercially available cosmetic formulations cannot meet the requirements of compound urea, so urea, which has strong efficacy, good safety and low price, is widely used in cosmetic products at present. Low (according to Mintel's global market-based search results in 2020, the proportion of cosmetics containing urea is only 2.8%). Moreover, most of the current urea-added cosmetics are only added in a small amount to stabilize the pH value of the formula, and the amount added is far lower than the amount of urea added for efficacy reported in the above literature.
- the invention provides a kind of stable composition of carrying urea or its derivative, described composition comprises:
- the urea derivative is a hydroxyalkylate of urea with 1-6 carbon atoms
- 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 loaded urea or its derivatives is 1:10 to 50:1.
- the oil in the composition is selected from: non-polar solid oil; non-polar liquid oil; polar liquid oil; polar solid oil; In a preferred embodiment, the composition contains 0.1-20% by weight of oil.
- the composition comprises 2.5-10% by weight of cationic surfactant.
- the long-chain fatty alcohol in the composition is selected from: cetyl alcohol, cetearyl alcohol, stearyl alcohol, eicosanol, behenyl alcohol or mixtures thereof.
- the composition comprises 0.1-10% by weight of long chain fatty alcohols.
- the composition contains more than 1% by weight of urea or its derivatives.
- the composition comprises more than 50% by weight of the aqueous phase.
- the weight ratio of the cationic emulsifier to the long-chain fatty alcohol in the composition is 10:1 to 1:2, and the weight ratio of the cationic emulsifier to the loaded urea or its derivatives is 1:2 to 10 :1.
- the present invention also provides an external skin preparation comprising the stable composition of the present invention.
- the present invention unexpectedly discovers a stable composition capable of carrying urea or its derivatives, and the composition exhibits abnormal viscosity-increasing phenomenon in high-temperature time-lapse tests under a suitable proportion. Therefore, the emulsification technology of the present invention has high practical value in the practical application of cosmetics and skin medical products in the future.
- Urea is one of the skin's natural moisturizing factors, and its functions of moisturizing, softening the skin, and promoting percutaneous penetration have been widely reported in the literature.
- urea which has a strong skin care effect, in cosmetics or dermatological products faces many challenges.
- Urea has strict requirements on the bearing capacity of the formulation system, and the bearing capacity of most commercially available formulations of cosmetics cannot meet the requirements of compound urea.
- the invention innovatively provides a stable composition capable of carrying urea or its derivatives.
- the urea carried by the stable composition of the present invention is in the form of a urea complex.
- the urea compound is a compound formed by urea:glycine:triethyl citrate at a weight ratio of 10:10:1.
- the urea compound is a compound of 5% urea, 5% glycine and 0.5% triethyl citrate.
- the urea carried by the stable composition of the invention is a urea derivative.
- urea derivatives are hydroxyalkylated derivatives of urea.
- the urea derivative is a hydroxyalkylated derivative having 1-6 carbon atoms.
- the urea derivative is hydroxyethylurea.
- the stabilizing composition comprises 0.1-20% by weight of urea or derivatives thereof. In some embodiments of the invention, the stabilizing composition comprises 0.1-10% by weight of urea or a derivative thereof.
- the stabilizing composition comprises more than 1% by weight of urea or derivatives thereof. In some embodiments of the invention, the stabilizing composition comprises more than 2% by weight of urea or derivatives thereof. In some embodiments of the invention, the stabilizing composition comprises more than 3% by weight of urea or derivatives thereof. In some embodiments of the invention, the stabilizing composition comprises more than 4% by weight of urea or derivatives thereof. In some embodiments of the invention, the stabilizing composition comprises more than 5% by weight of urea or derivatives thereof.
- the stable composition of the present invention loaded with urea or its derivatives comprises grease.
- the grease contained in the stable composition of the present invention is selected from: (1) non-polar solid grease; (2) non-polar liquid grease; (3) polar liquid grease; (4) Polar solid grease; (5) silicone oil; or any mixture thereof.
- the stabilizing compositions of the present invention comprise white petrolatum. In some specific embodiments, the stable composition of the present invention comprises 10# white oil. In some specific embodiments, the stabilizing compositions of the present invention comprise isooctyl palmitate. In some specific embodiments, the stabilizing compositions of the present invention comprise cetyl palmitate. For example, in some specific embodiments, the stabilizing compositions of the present invention comprise Cetyl Cetyl ACP available from Croda (Singapore). In some specific embodiments, the stabilizing compositions of the present invention comprise simethicone. For example, in some specific embodiments, the stabilizing composition of the present invention comprises simethicone (100 cst) purchased from Dow (Zhangjiagang) Investment Co., Ltd.
- the stabilizing composition comprises 0.1-20% by weight of oil. In some embodiments of the invention, the stabilizing composition comprises 1-20% by weight of oil. In some embodiments of the present invention, the stabilizing composition comprises 1-10% by weight of oil. In some embodiments of the invention, the stabilizing composition comprises 5-10% by weight of oil.
- Cationic surfactant refers to an emulsifier with cationic groups, and its molecular structure includes cationic groups and alkyl chains.
- cationic groups mainly include alkyl quaternary ammonium salts, alkyl pyridinium salts, and alkyl amine salts, which generally have good heat resistance, light resistance, acid and alkali resistance, and have good surface activity, stability and biodegradation. sex. Due to the unique charge properties of cationic surfactants, they can form a film on the surface of skin or hair, so they have a unique product feel, especially widely used in hair products.
- the alkyl chains of the cationic surfactants are attached to the surface of the cutin to form a cationic film, and the charge repulsion of the cationic film makes the matrix appear lubricating, which is manifested in the smoothness and smoothness of the hair after use.
- anionic thickeners due to the wide application of anionic thickeners, the use of cationic surfactants in skin care products is relatively small.
- the strong absorption and film-forming properties of cationic surfactants can significantly shield the sticky feeling of oil, and can make the product have a unique sense of use. If it can be applied to suitable products, it can have unique advantages in the cosmetics market. Competitiveness.
- the stabilizing compositions of the present invention comprise cationic surfactants.
- the cationic surfactant employed in the stabilizing composition of the present invention is distearyldimethylammonium chloride.
- the cationic surfactant used in the stabilizing composition of the present invention is TA-100 available from Evonik Operations GmbH.
- the present inventors have surprisingly found that the use of distearyldimethylammonium chloride results in stable compositions capable of supporting urea or its derivatives. What is also unexpected is that after some samples are compounded with urea, the viscosity of the sample increases significantly in the high-temperature time-dependent stability test, while the sample without compounding urea does not show similar abnormal phenomena.
- This abnormal phenomenon has high application value in the actual production of cosmetics and skin medical products: (1) compounding distearyl dimethyl ammonium chloride with other emulsifiers can improve or avoid the compounding of the latter with urea (2) By aging the material at high temperature during the preparation process, the viscosity of the sample is then adjusted; (3) This characteristic can be used to prepare a hard cream and remain stable in the intensive test. It is also necessary to point out that the efficacy of urea is suitable for the care of dry skin, and the cosmetics designed for this type of skin generally have a high amount of oil added, so the skin feels greasy and has poor absorption. Due to its cationic properties, distearyl dimethyl ammonium chloride has strong absorption and covering properties when used in cosmetics. It can effectively improve the greasy feeling of formulas with high oil content and improve its absorption. It can meet the needs of cosmetics. At the same time of efficacy, consumers can get a better experience.
- the stabilizing composition comprises 0.5-20% by weight cationic surfactant. In some embodiments of the invention, the stabilizing composition comprises 1-20% by weight cationic surfactant. In some embodiments of the invention, the stabilizing composition comprises 1-10% by weight cationic surfactant. In some embodiments of the invention, the stabilizing composition comprises 2.5-10% by weight cationic surfactant. In some embodiments of the invention, the stabilizing composition comprises 5-10% by weight cationic surfactant.
- the weight ratio of cationic emulsifier to loaded urea or its derivatives is 1:10 to 50:1. In some embodiments of the present invention, the weight ratio of cationic emulsifier to loaded urea or its derivatives is 1:10 to 10:1. In some embodiments of the present invention, the weight ratio of cationic emulsifier to loaded urea or its derivatives is 1:2 to 10:1. In a specific embodiment of the present invention, the weight ratio of the cationic emulsifier to the loaded urea or its derivatives is 1:1.
- the stabilized compositions of the present invention loaded with urea or derivatives thereof comprise long chain fatty alcohols.
- the long-chain fatty alcohol contained in the stable composition of the present invention is a long-chain fatty alcohol with 16-22 carbon atoms.
- the long-chain fatty alcohol contained in the stabilizing composition of the present invention is selected from the group consisting of cetyl alcohol, cetearyl alcohol, stearyl alcohol, eicosanol, behenyl alcohol or mixtures thereof.
- the stabilizing composition comprises 0.1-10% by weight of long chain fatty alcohol. In some embodiments of the invention, the stabilizing composition comprises 0.5-10% by weight of long chain fatty alcohol. In some embodiments of the invention, the stabilizing composition comprises 1-10% by weight of long chain fatty alcohol. In some embodiments of the invention, the stabilizing composition comprises 1-5% by weight of long chain fatty alcohol. In some embodiments of the invention, the stabilizing composition comprises 3-5% by weight long chain fatty alcohol.
- the weight ratio of cationic emulsifier to long-chain fatty alcohol is 10:1 to 1:4. In some embodiments of the present invention, the weight ratio of cationic emulsifier to long-chain fatty alcohol is 10:1 to 1:2. In some embodiments of the present invention, the weight ratio of cationic emulsifier to long-chain fatty alcohol is 10:1 to 1:1. In a specific embodiment of the present invention, the weight ratio of the cationic emulsifier to the long-chain fatty alcohol is 5:2.
- the stabilized compositions of the present invention also comprise an aqueous phase.
- the aqueous phase can be water or other aqueous carrier.
- the stabilizing composition comprises more 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.
- composition of the present invention can be used as an efficacy additive in skin external preparations.
- the external skin preparation is selected from: cleanser, lotion, lotion, cream, gel, mask. Add different dosages according to different types of preparations.
- the skin external preparation is a general term for all ingredients that are usually used on the outside of the skin, and may be, for example, a cosmetic composition.
- the cosmetic composition can be basic cosmetics, facial makeup cosmetics, body cosmetics, hair care cosmetics, etc. There is no special limitation on the dosage form, which can be reasonably selected according to different purposes.
- the cosmetic composition also contains different cosmetically acceptable media or matrix excipients according to different dosage forms and purposes.
- the stable composition of the present invention forms an emulsified system, is especially suitable for skin care of dry and moderately dry skin, and has unique advantages in cosmetics for hand, foot and body care.
- the stable composition of the present invention is suitable for hands that can moisturize the skin, soften the skin, refine the skin, improve skin luster, prevent chapping, relieve dryness, and relieve tension.
- the proportions of skin feeling and smooth skin are 98%, 98%, 98%, 96%, 96%, 94%, 96% and 98%, and the experimental results can be supported by laboratory objective indicators (skin moisture content, Skin water loss, skin elasticity, skin scale value, and skin smoothness were improved immediately and after 4 weeks of use, and there were statistical differences compared with the control group).
- 94% of consumers agree that the product is easy to absorb and not sticky after absorption
- 98% of consumers agree that the product has a protective film feel. It can be seen from this that the technology reported in the present invention is applied to a suitable product, which can give the product a good sense of use and efficacy at the same time, so that the product has strong product competitiveness.
- TA-100 Distearyldimethylammonium chloride
- H-MY purchased from Emery Oleochemicals (M) Sdn Bhd;
- White vaseline purchased from Hansheng Chemical (Fushun) Co., Ltd.;
- Hydroxyethylurea (50%): purchased from Guangzhou Xipu Fine Chemical Technology Co., Ltd.;
- Triethyl citrate purchased from Shanghai Pujie Perfume Co., Ltd.;
- Glycine purchased from Hebei Huayang Biotechnology Co., Ltd.;
- Cetyl alcohol (cetyl alcohol): purchased from BASF;
- Behenyl alcohol (behenyl alcohol): purchased from BASF;
- Cationic conditioning agent ECON-100 purchased from Chongqing Haifan Biochemical Technology Co., Ltd.;
- Polyglyceryl pentastearate and sodium stearoyl lactylate purchased from NIKKOL CHEMICAL CO.LTD;
- Glyceryl Laurate purchased from BASF;
- Polyglyceryl-10 myristate (polyglyceryl monomyristate): purchased from NIKKOL CHEMICAL CO.LTD;
- MSE-20 Methyl Glucose Sesquistearate
- Ceteareth-30 available from BASF;
- Araton 2121 purchased from CRODA;
- Polyquaternium-37 purchased from BASF;
- Grafted corn starch 25 purchased from Daito KaseiKogyo Co., Ltd.;
- Xanthan gum purchased from Jungbunzlauer Austria AG;
- Isooctyl palmitate purchased from PALM-OLEO (KLANG) SDN BHD;
- Cetyl Cetyl ACP purchased from Croda (Singapore);
- Simethicone oil (100cst): purchased from Dow (Zhangjiagang) Investment Co., Ltd.
- Constant temperature water bath Shanghai Yiheng Scientific Instrument Co., Ltd., HWS-28;
- Bench mixer IKA EUROSTAR, power control-visc
- pH meter METTLER TOLEDO, SevenMulti;
- Viscometer BROOKFIELD, DV-S digital viscometer.
- Examples 1-18 Preparation of emulsification systems containing different surfactants and corresponding urea-containing samples.
- Phase A, Phase B and Phase C weigh appropriate amount of Phase A, Phase B and Phase C in three beakers as shown in Table 1, and heat them in a water bath at 90°C for 30 minutes respectively. Then use a desktop homogenizer to homogenize phase A at 5000rpm for 2 minutes to disperse evenly; then maintain homogenization at 5000rpm and add phase B while it is hot, and continue homogenizing for 2 minutes after adding; continue to maintain homogenization at 5000rpm and add phase C while it is hot Mix the sample and keep it homogeneous for 5 minutes after adding phase C. Thereafter, the beaker was sealed with a PE film and the sample was allowed to stand overnight at room temperature. Add phase D the next day, and use a desktop homogenizer at room temperature to homogenize again at 5000 rpm for 3 minutes to mix the sample evenly, then seal the beaker with PE film, and keep the sample for later use.
- Table 1 shows the types of surfactants included in Examples 1-18 and the feeding amount of each raw material.
- Examples 1-18 are configured with 9 kinds of composite emulsification systems containing different surfactants, each of which is used to prepare a base material and a copy of the examples containing urea.
- the preparation amount of each sample is 200g, and the preparation process uniformly adopts the concentrated aqueous phase method, and is compounded with 2% cetearyl alcohol and 6% white petrolatum, and the addition amount of urea in the examples containing urea is 5%.
- Examples 19-33 Preparation of hydrosols of various polymer thickeners and corresponding samples containing urea.
- Table 2 shows the types of polymer thickeners included in Examples 19-33 and the dosage of each raw material.
- Examples 19-33 configure 5 kinds of composite emulsification systems containing different polymer thickeners, and the conditional amount of each polymer is adjusted at 0.4% or 0.5% according to its hydrosol viscosity.
- Three samples were prepared for each polymer thickener, namely base material, urea-containing sample and urea-containing composition sample.
- the preparation amount of each sample is 200g
- the urea addition amount in the urea-containing samples is 5%
- 5% urea, 5% glycine and 0.5% triethyl citrate are added to the urea-containing composition samples.
- Test example 1 the stability test of embodiment 1-33
- each sample was equally divided into two 150ml transparent PET bottles, and after the screw caps were tightly closed, the samples were respectively placed in a 25°C incubator and a 48°C incubator. Regularly take the sample out of the incubator, let it stand for 6 hours to cool down to room temperature, measure the pH and viscosity of the sample and observe the properties of the sample, and then put the sample back into the incubator after the measurement.
- Table 3 shows the pH and viscosity of Examples 1-33 at various test time points.
- Examples 1-18 are compound emulsification systems prepared by 9 different commercially available surfactants, and corresponding samples with urea added.
- 2 cationic surfactants TA-100, examples 1-2; ECON-100, examples 3-4
- 1 anionic surfactant HR-S1, examples 5-6)
- anionic surfactants were selected.
- 1 compound nonionic surfactant polyglycerol pentastearate and sodium stearoyl lactylate, Examples 7-8), and 5 nonionic surfactants.
- nonionic surfactants can be further subdivided into: (1) monoglyceride surfactant (glyceryl laurate, embodiment 9-10); (2) polyglyceride surfactant (monomyristic acid (polyglyceryl ester, embodiment 11-12); (3) polyethylene glycol surfactant (ceteareth-30, embodiment 13-14); (4) carbohydrate surfactant ( MSE-20, Examples 15-16; Araton 2121, Examples 17-18).
- monoglyceride surfactant glyceryl laurate, embodiment 9-10
- polyglyceride surfactant monomyristic acid (polyglyceryl ester, embodiment 11-12)
- polyethylene glycol surfactant ceteareth-30, embodiment 13-14
- carbohydrate surfactant MSE-20, Examples 15-16; Araton 2121, Examples 17-18.
- Example 1 After the compound emulsification system based on TA-100 (Example 1) was left at room temperature for one month, the pH value of the sample dropped slightly from 4.99 to 4.96; the viscosity of the sample was 4780mPa ⁇ s, which was higher than that of the newly prepared sample of 3170mPa ⁇ s. After being stored at 48°C for one month, the pH value of the sample was 4.79, which was slightly lower than the initial value, while the viscosity was 2380 mPa ⁇ s, which was slightly lower than that of the fresh sample.
- Example 2 After the sample compounded with 5% urea (Example 2) was left at room temperature for one month, the pH value of the sample rose from 5.45 to 7.66, and the viscosity dropped significantly from 2180mPa ⁇ s to 680mPa ⁇ s. After the sample was placed at 48°C for one month, its viscosity increased significantly. Compared with the viscosity of the fresh sample which is 3570mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks or 1 month are 11530mPa ⁇ s, 11100mPa ⁇ s and 9720mPa ⁇ s respectively. At the same time, the sample pH also increased from 5.45 to 9.24. The above experimental results show that the TA-100 compound system can stably carry urea. In addition, in Example 2, the viscosity of the sample was significantly increased in the high-temperature stability test over time.
- Example 3 After the compound emulsification system (Example 3) based on the cationic conditioner ECON-100 was placed at room temperature for one month, the pH value of the sample dropped slightly from 3.89 to 3.86; the viscosity of the sample was too low and the suspending force was insufficient to maintain stability. Stratification occurs upon standing. After being placed at 48°C for one month, the samples also showed stratification at various time points. After the stability test, the pH value of the sample was 3.67, which was slightly lower than the initial value. After the sample compounded with 5% urea (Example 4) was left at room temperature for one month, the pH value of the sample rose slightly from 4.06 to 4.16, and the sample also showed stratification at each time point.
- Example 5 After a compound emulsification system (Example 5) based on potassium lauryl phosphate (HR-S1) was placed at room temperature for one month, the pH value of the sample dropped slightly from 7.57 to 7.45; 117mPa ⁇ s increased. After being stored at 48°C for one month, the pH value of the sample was 7.72, which was slightly higher than the initial value, but the samples were separated at various time points due to the low viscosity.
- HR-S1 potassium lauryl phosphate
- Example 6 After the sample compounded with 5% urea (Example 6) was placed at room temperature for 1 month, the pH value of the sample rose slightly from 7.43 to 7.62, and the viscosity of the samples placed at room temperature for 1 week, 2 weeks and 1 month were 392mPa ⁇ s and 1658mPa respectively ⁇ s and 2358mPa ⁇ s, which are significantly higher than the initial value of 125mPa ⁇ s. After the sample was placed at 48°C for one month, the pH value of the sample rose sharply from 7.43 to 8.93. Similarly, all tests were separated due to too low viscosity and insufficient suspension force. The above experimental results show that the compound emulsification system of potassium lauryl phosphate (HR-S1) can only stably carry urea at room temperature, but at high temperature, the material body is separated due to insufficient suspension force.
- HR-S1 potassium lauryl phosphate
- Example 7 After a compound emulsification system based on polyglycerol pentastearate and sodium stearoyl lactylate (Example 7) was placed at room temperature for one month, the pH value of the sample dropped slightly from 4.74 to 4.33; The sample 4950mPa ⁇ s increased significantly. After being stored at 48°C for one month, the pH value of the sample was 4.46, which was slightly lower than the initial value, and the viscosity was 14920 mPa ⁇ s, which was also slightly lower than that of the fresh sample.
- Example 8 After the sample compounded with 5% urea (Example 8) was left at room temperature for one month, the pH value of the sample increased from 4.80 to 5.87, and the viscosity increased significantly from 6250mPa ⁇ s to 25250mPa ⁇ s. After the sample was placed at 48°C for one month, its viscosity also increased significantly. Compared with the viscosity of the fresh sample which is 6250mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 35580mPa ⁇ s, 23830mPa ⁇ s and 28500mPa ⁇ s respectively. At the same time, the sample pH also increased from 4.80 to 8.08. The above experimental results show that the compound system based on polyglycerol pentastearate and sodium stearoyl lactylate can stably carry urea.
- Example 10 After the compound emulsification system (Example 9) based on glycerol laurate was placed at room temperature for one month, the pH value of the sample dropped from 4.77 to 4.07; Set to layer. After being placed at 48°C for one month, it also separated due to the low viscosity of the material; the pH value of the sample after the stability test was 4.74, which was basically the same as the initial value. After the compound 5% urea sample (Example 10) was left at room temperature for 1 month, the pH value of the sample rose slightly from 6.32 to 7.21, and the viscosity of the samples placed at room temperature for 1 week, 2 weeks and 1 month were 992mPa ⁇ s and 3680mPa ⁇ s respectively.
- Example 11 After the compound emulsification system (Example 11) based on polyglycerol monomyristate was placed at room temperature for one month, the pH value of the sample dropped slightly from 7.99 to 6.67; the viscosity of the sample was too low and the suspending power was insufficient to maintain a stable emulsification system. When it stands still, it will be stratified. After being placed at 48°C for one month, the material body still separated due to low viscosity; the pH value of the sample after the stability test was 7.19, which was slightly lower than the initial value.
- Example 12 After the sample compounded with 5% urea (Example 12) was left at room temperature for one month, the pH value of the sample dropped slightly from 8.16 to 7.98, and the samples were separated at each time point. After the sample was placed at 48°C for one month, the pH of the sample rose from 8.16 to 8.83, and the sample also separated at each test time point.
- the above experimental results show that the polyglyceryl monomyristate compound emulsification system cannot stably carry urea, and the two samples have delamination problems under all test conditions.
- Example 13 After the compound emulsification system based on ceteareth-30 (Example 13) was left at room temperature for one month, the pH value of the sample rose slightly from 6.30 to 6.45; the viscosity of the sample was too low and the suspension force was insufficient to maintain a stable emulsification System, after a short period of standing, it will be stratified. After being placed at 48°C for one month, the material body also separated due to the low viscosity; and the pH value dropped to 4.13, which was significantly lower than the initial value. After the sample compounded with 5% urea (Example 14) was left at room temperature for one month, the pH value rose from 7.52 to 8.14, and the samples were separated at each time point.
- the pH value of the sample dropped slightly from 7.08 to 6.67; the viscosity of the sample was 167mPa ⁇ s, which was slightly lower than that of the newly prepared sample of 183mPa ⁇ s.
- the pH value of the sample was 3.86, which was significantly lower than the initial value; the viscosity of the sample after 1 week, 2 weeks and 1 month was 1700mPa s, 2600mPa s and 15670mPa s, which were higher than those of the freshly prepared samples. significantly increased.
- Example 16 After the sample compounded with 5% urea (Example 16) was left at room temperature for one month, the pH value increased from 7.13 to 7.93, and the viscosity slightly decreased from 167mPa ⁇ s to 142mPa ⁇ s. After the sample was placed at 48°C for one month, its viscosity also increased. Compared with the viscosity of the freshly prepared sample of 167mPa s, the viscosity of the samples stored at 48°C for 1 week, 2 weeks and 1 month were 1400mPa s, 2200mPa s and 1833mPa s, respectively, but the increase was significantly higher than that of the unreconstituted urea sample get smaller. At the same time, the sample pH also increased from 7.13 to 8.92.
- Example 17 After the compound emulsification system based on Araton 2121 (Example 17) was left at room temperature for one month, the pH value of the sample dropped slightly from 7.01 to 6.82; the viscosity of the sample was 46330mPa ⁇ s, which was slightly lower than that of the fresh sample (47500mPa ⁇ s). After being stored at 48°C for 1 month, the pH value of the sample was 6.52, which was lower than the initial value; the viscosity of the sample after 1 week, 2 weeks and 1 month was 50170mPa ⁇ s, 51000mPa ⁇ s and 52500mPa ⁇ s respectively, compared with the newly prepared Sample rises slightly.
- Example 18 After the sample compounded with 5% urea (Example 18) was left at room temperature for one month, the pH value increased from 6.95 to 7.19, and the viscosity slightly decreased from 48750mPa ⁇ s to 43170mPa ⁇ s. After the sample was placed at 48°C for 1 month, its viscosity showed an obvious downward trend. Compared with the 48,750mPa ⁇ s of the new sample, the viscosity of the sample placed at 48°C for 1 week, 2 weeks and 1 month were 44080mPa ⁇ s and 32250mPa ⁇ s respectively and 23000mPa ⁇ s. At the same time, the sample pH also increased from 6.95 to 7.92.
- polymeric thickeners are often used in cosmetics to provide viscosity to the formula, thereby improving the stability of the formula.
- Examples 19-33 investigated the stability of five different commercially available polymer thickener hydrosols after compounding urea.
- the polymers investigated can be divided into three categories according to the structure of the polymer chain: (1) cationic high Molecular thickener (PQ-37, Example 19-21); (2) Nonionic polymer thickener (M25, Example 22-24; Xanthan gum, Example 25-27); (3) Anionic Polymer thickener (sodium polyacrylate, examples 28-30; AVC, examples 31-33).
- Example 19 0.5% PQ-37 hydrosol (Example 19) has good stability. After the sample was placed at room temperature for one month, the viscosity increased slightly from 16430mPa ⁇ s to 18370mPa ⁇ s; and after one month at 48°C, the viscosity was 15130mPa ⁇ s, which was not significantly changed compared with the fresh sample of 16430mPa ⁇ s. After compounding PQ-37 with 5% urea (Example 20), the stability of the sample became significantly worse.
- Example 20 After Example 20 was placed at room temperature for 1 month, the pH value rose from 4.43 to 7.84, while the viscosity dropped from 18030mPa ⁇ s to 5280mPa s; while at 48°C for only one week, with the pH value rising to 8.88, the viscosity dropped significantly to 183mPa ⁇ s.
- the stability of the sample After compounding PQ-37 with 5% urea, 5% glycine and 0.5% triethyl citrate (Example 21), the stability of the sample also deteriorated significantly.
- Example 21 After one month at room temperature, the pH value of Example 21 changed from 5.23 The pH increased slightly to 5.77, while the viscosity decreased from 13230mPa ⁇ s to 5430mPa ⁇ s; and after being placed at 48°C for a week, the pH increased slightly to 5.70, but the viscosity decreased significantly to 333mPa ⁇ s.
- the above experimental results show that PQ-37 hydrosol cannot stably carry urea.
- the results of Example 21 show that the increase in pH value caused by urea decomposition is not the only reason for the loss of viscosity of the material body.
- Example 22 0.4% M25 hydrosol (Example 22) has better stability. After the sample was placed at room temperature for one month, the viscosity increased slightly from 15420mPa ⁇ s to 18270mPa ⁇ s; and after one month at 48°C, the viscosity was 8270mPa ⁇ s, which was slightly lower than that of the fresh sample (15420mPa ⁇ s). After compounding 5% urea with M25 (Example 23), the stability of the sample became worse.
- Example 20 After Example 20 was placed at room temperature for 1 month, the pH value rose from 7.13 to 7.48, and the viscosity dropped from 16080mPa ⁇ s to 15220mPa ⁇ s; After being placed at 48°C for one month, the viscosity dropped significantly to 2230mPa ⁇ s as the pH rose to 8.90.
- Example 24 After compounding PQ-37 with 5% urea, 5% glycine and 0.5% triethyl citrate (Example 24), the sample stability also deteriorated, and after Example 24 was placed at room temperature for 1 month, the pH value decreased slightly from 6.76 The pH dropped to 6.62, while the viscosity dropped from 15830mPa ⁇ s to 8700mPa ⁇ s; after being placed at 48°C for one month, the pH dropped to 6.31, but the viscosity dropped significantly to 1170mPa ⁇ s.
- the above experimental results show that the M25 hydrosol cannot stably carry urea.
- Example 25 0.5% xanthan gum hydrosol (Example 25) has good stability. After the sample was placed at room temperature for one month, the viscosity increased slightly from 1242mPa ⁇ s to 1317mPa ⁇ s; and after one month at 48°C, the viscosity was 970mPa ⁇ s, which was slightly lower than that of the freshly prepared sample. After xanthan gum is compounded with 5% urea (Example 26), the sample still maintains good stability.
- Example 20 After Example 20 is placed at room temperature for 1 month, the pH value rises from 7.04 to 7.38, while the viscosity rises slightly from 1383mPa ⁇ s After being stored at 48°C for one month, the pH value of the sample rose to 8.65, and the viscosity dropped to 867mPa ⁇ s. After compounding PQ-37 with 5% urea, 5% glycine and 0.5% triethyl citrate (Example 27), the stability of the sample did not change significantly.
- Example 21 After one month at room temperature, the pH value of Example 21 changed from 5.55 The pH value increased slightly to 7.21, while the viscosity increased slightly from 1442mPa ⁇ s to 1575mPa ⁇ s; after being stored at 48°C for one month, the pH value increased slightly to 6.04, while the viscosity of the sample decreased slightly to 1270mPa ⁇ s.
- the above experimental results show that the xanthan gum hydrosol can stably carry urea and its composition.
- Example 28 0.4% sodium polyacrylate hydrosol has good stability. After the sample was placed at room temperature for one month, the viscosity increased slightly from 2667mPa ⁇ s to 2625mPa ⁇ s; and after one month at 48°C, the viscosity was 2845mPa ⁇ s, which did not change much compared to the new sample. After compounding 5% urea with sodium polyacrylate (Example 29), the sample stability significantly deteriorated.
- Example 29 After Example 29 was placed at room temperature for 1 month, the pH value rose from 6.89 to 7.26, and the viscosity dropped from 3392mPa ⁇ s to 833mPa ⁇ s s; while at 48°C for only one week, the viscosity dropped significantly to 142mPa ⁇ s as the pH rose to 7.99.
- Example 30 After compounding sodium polyacrylate with 5% urea, 5% glycine and 0.5% triethyl citrate (Example 30), the stability of the sample also deteriorated significantly.
- Example 30 After Example 30 was left at room temperature for one month, the pH value dropped slightly from 6.51 to 6.32, while the viscosity dropped significantly from 2000mPa ⁇ s to 358mPa ⁇ s; and after being placed at 48°C for one week, the pH value dropped to 5.80, while the viscosity of the sample A sharp drop to 117mPa ⁇ s.
- the above experimental results show that the sodium polyacrylate hydrosol cannot stably carry urea and the urea composition.
- the 0.4% AVC hydrosol (Example 31) has good stability. After the sample was stored at room temperature for one month, the viscosity increased slightly from 5250mPa s to 7400mPa s; after being stored at 48°C for one month, the viscosity was 13570mPa s, which was significantly improved compared with the newly prepared sample. Rearrangement of micellar structure. After compounding AVC with 5% urea (Example 32), the stability of the sample became significantly worse.
- Example 32 After Example 32 was left at room temperature for one month, the pH value rose from 6.46 to 7.64, while the viscosity dropped from 6092mPa ⁇ s to 608mPa ⁇ s; However, after only one week at 48°C, the viscosity dropped significantly to 142mPa ⁇ s as the pH rose to 8.61. After compounding AVC with 5% urea, 5% glycine and 0.5% triethyl citrate (Example 33), the stability of the sample also deteriorated significantly.
- Example 21 after being placed at room temperature for one month, the pH value increased slightly from 5.64 to 5.73, while the viscosity decreased from 3180mPa ⁇ s to 508mPa ⁇ s; after being placed at 48°C for one week, the pH value increased slightly to 5.73, and the viscosity of the sample decreased. A sharp drop to 117mPa ⁇ s.
- the above experimental results show that the AVC hydrosol cannot stably carry urea and its composition.
- Examples 34-53 Preparation of compound emulsification systems containing different types and amounts of oils and corresponding urea-containing samples.
- Phase A, Phase B and Phase C weigh appropriate amount of Phase A, Phase B and Phase C in three beakers as shown in Table 4, and heat them in a water bath at 90°C for 30 minutes respectively. Then use a desktop homogenizer to homogenize phase A at 5000rpm for 2 minutes to disperse evenly; then maintain homogenization at 5000rpm and add phase B while it is hot, and maintain homogenization for 2 minutes after adding; continue to maintain homogeneity at 5000rpm and add phase C while it is hot Mix the sample and keep it homogeneous for 5 minutes after adding phase C. Thereafter, the beaker was sealed with a PE film and the sample was allowed to stand overnight at room temperature. Add phase D the next day, and use a desktop homogenizer at room temperature to homogenize again at 5000 rpm for 3 minutes to mix the sample evenly, then seal the beaker with PE film, and keep the sample for later use.
- Table 4 shows the types of fats and oils contained in Examples 34-53 and the feeding amount of each raw material.
- the emulsification system of Examples 34-53 is the same as that of Examples 1-2, fixed at 5% TA-100 compounded with 2% cetearyl alcohol.
- the preparation amount of each sample is 200g, and the sample preparation process also adopts the concentrated aqueous phase method consistent with that of Example 1-2.
- the effects of the type of oil and the amount of oil added on the properties of the samples were investigated.
- the fixed oil content was 6%, and various types of oils were used to prepare samples; while in Examples 44-53, the fixed oil was white petroleum jelly, so as to investigate the influence of the added oil content on the properties of the samples.
- Each sample was prepared with a base material and an example containing urea, and in the examples containing urea, the amount of urea added was 5%.
- Test example 2 the stability test of embodiment 34-53
- each sample was equally divided into two 150ml transparent PET bottles, and after the screw caps were tightly closed, the samples were respectively placed in a 25°C incubator and a 48°C incubator. Regularly take the sample out of the incubator, let it stand for 6 hours to cool down to room temperature, measure the pH and viscosity of the sample and observe the properties of the sample, and then put the sample back into the incubator after the measurement.
- Table 5 shows the pH values and viscosities of Examples 34-53 at each test time point (listing Example 1 and Example 2 for comparison).
- Table 5 summarizes the pH values and viscosities of Examples 34-53 at various test time points, and includes the corresponding data of Examples 1-2 as a comparison.
- embodiment 1-2 and embodiment 34-41 investigated the impact of 5 kinds of different oils and fats on the compound emulsification system property, these five kinds of oils and fats comprise: (1) nonpolar solid oil (white vaseline, embodiment 1- 2); (2) non-polar liquid oil (10# white oil, embodiment 34-35); (3) polar liquid oil (isooctyl palmitate, embodiment 36-37); (4) polarity Solid grease (Cetyl Cetyl ACP, Examples 38-39); (5) Silicone oil (Dimethicone (100cst), Examples 40-41).
- Examples 42-43 used the above oils in combination.
- Example 34 After the sample of emulsified 10# white oil (Example 34) was left at room temperature for one month, its pH value was 4.94, which was almost unchanged from the initial value of 4.93; the sample viscosity was 5700mPa ⁇ s, which was slightly higher than that of the newly prepared sample of 5450mPa ⁇ s . After being stored at 48°C for one month, the pH value of the sample dropped from 4.93 to 4.64, while the viscosity was 4200mPa ⁇ s, which was slightly lower than that of the fresh sample.
- Example 35 After the sample compounded with 5% urea (Example 35) was left at room temperature for one month, the pH value rose from 5.47 to 7.80, and the viscosity dropped from 8130mPa ⁇ s to 5570mPa ⁇ s. After the sample was placed at 48°C for one month, its viscosity increased. Compared with the viscosity of the fresh sample which is 1092mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 9500mPa ⁇ s, 8840mPa ⁇ s and 8450mPa ⁇ s respectively. At the same time, the sample pH also rose from 5.47 to 9.21. The above experimental results show that the TA-100 compound system can stably carry urea after emulsifying 10# white oil, and in the high temperature stability test over time, the viscosity of the sample shows an upward trend.
- the sample After the sample was placed at 48°C for one month, its viscosity increased significantly. Compared with the viscosity of the fresh sample which is 3570mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 5000mPa ⁇ s, 9630mPa ⁇ s and 8280mPa ⁇ s respectively. At the same time, the sample pH also rose from 4.30 to 9.16.
- the above experimental results show that the TA-100 compound system can stably carry urea after emulsifying isooctyl palmitate, and the viscosity of the sample shows an upward trend in the high temperature stability test over time.
- Example 38 After the sample of emulsified cetyl cetyl cetyl ACP (Example 38) was placed at room temperature for 1 month, its pH value was 4.59, which was slightly higher than the initial value of 4.47; Slight increase. After being stored at 48°C for one month, the pH value of the sample was 4.46, which was almost unchanged compared with the fresh sample, while the viscosity was 6300mPa ⁇ s, which was slightly increased compared with the fresh sample. After the sample compounded with 5% urea (Example 39) was left at room temperature for one month, the pH value increased from 4.87 to 7.40, and the viscosity increased from 3570mPa ⁇ s to 4570mPa ⁇ s.
- the sample After the sample was placed at 48°C for one month, its viscosity increased significantly. Compared with the viscosity of the fresh sample which is 3570mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 12380mPa ⁇ s, 17330mPa ⁇ s and 15330mPa ⁇ s respectively. At the same time, the sample pH also increased from 4.87 to 8.98.
- the above experimental results show that the TA-100 compound system can stably carry urea after emulsifying hexadecyl cetyl ester ACP, and the viscosity of the sample shows an obvious upward trend in the high temperature stability test over time.
- Example 40 After the sample (Example 40) of emulsified simethicone oil (100cst) was placed at room temperature for 1 month, its pH value was 5.04, which was slightly lower than the initial value of 5.08; significantly increased. After being placed at 48°C for one month, the pH value of the sample is also 5.04, and the viscosity is 11230mPa ⁇ s, which is significantly higher than that of the fresh sample. After the sample compounded with 5% urea (Example 41) was left at room temperature for one month, the pH value of the sample increased from 5.55 to 7.70, and the viscosity decreased from 4820 mPa ⁇ s to 2330 mPa ⁇ s.
- the viscosities of the sample and the one-month sample were 8380 mPa ⁇ s, 16650 mPa ⁇ s and 17000 mPa ⁇ s, respectively.
- the sample pH also increased from 5.55 to 9.21.
- the above experimental results show that the TA-100 compound system can stably carry urea after emulsifying simethicone oil (100cst), and the viscosity of the sample shows an obvious upward trend in the high-temperature stability test over time.
- Example 42 After a sample emulsified with various oils (Example 42) was left at room temperature for one month, its pH dropped slightly from 6.10 to 5.86, while its viscosity was 1280 mPa ⁇ s, which was slightly higher than that of the fresh sample (858 mPa ⁇ s). After being placed at 48°C for one month, the pH value of the sample dropped from 6.10 to 5.46, while the viscosity was 880mPa ⁇ s, which had no significant change compared with the fresh sample. After the sample compounded with 5% urea (Example 43) was left at room temperature for one month, the pH value increased from 6.21 to 7.98, and the viscosity also increased slightly from 858mPa ⁇ s to 1380mPa ⁇ s.
- Examples 44-53 fixed the oil as white petrolatum, and investigated the effect of the amount of oil added on the properties of the TA-100 compound emulsification system.
- the amount of fat added in Examples 44-45, 46-47, 48-49, 1-2, 50-51 and 52-53 is 0%, 1%, 3%, 6%, 10% and 20%.
- Example 44 After the uncompounded oil sample (Example 44) was left at room temperature for one month, its pH value was 4.97, which was slightly lower than the initial value of 5.29; the viscosity of the sample was 2150mPa ⁇ s, which was slightly higher than that of the fresh sample (1700mPa ⁇ s). After being stored at 48°C for one month, the pH value of the sample was 4.88, and the viscosity was 1280 mPa ⁇ s, which was slightly lower than that of the fresh sample. After the sample compounded with 5% urea (Example 45) was left at room temperature for one month, the pH value rose from 5.27 to 7.14, and the viscosity dropped from 1270mPa ⁇ s to 258mPa ⁇ s.
- Example 46 After the compound 1% white petrolatum sample (Example 46) was left at room temperature for one month, its pH value was 5.01, which was slightly lower than the initial value of 5.25; the viscosity of the sample was 1980mPa ⁇ s, which was slightly higher than that of the newly prepared sample (1720mPa ⁇ s). After being stored at 48°C for one month, the pH value of the sample was 4.84, and the viscosity was 1330mPa ⁇ s, which was slightly lower than that of the newly prepared sample. After the sample compounded with 5% urea (Example 47) was left at room temperature for one month, the pH value rose from 5.75 to 7.27, and the viscosity dropped from 1320mPa ⁇ s to 300mPa ⁇ s.
- Example 48 After the compound 3% white vaseline sample (Example 48) was left at room temperature for one month, its pH value was 4.97, which was slightly lower than the initial value of 5.29; the viscosity of the sample was 2120mPa ⁇ s, which was slightly higher than that of the newly prepared sample of 1900mPa ⁇ s. After being stored at 48°C for one month, the pH value of the sample was 4.88, and the viscosity was 1330mPa ⁇ s, which was slightly lower than that of the newly prepared sample. After the sample compounded with 5% urea (Example 49) was left at room temperature for one month, the pH value rose from 5.76 to 7.41, and the viscosity dropped from 1530mPa ⁇ s to 333mPa ⁇ s.
- Example 50 After the compound 10% white petrolatum sample (Example 50) was left at room temperature for one month, its pH value was 5.09, which was slightly lower than the initial value of 5.29; the viscosity of the sample was 2670mPa ⁇ s, which was slightly higher than that of the newly prepared sample of 2200mPa ⁇ s. After being stored at 48°C for one month, the pH value of the sample was 5.20, and the viscosity was 1620mPa ⁇ s, which was lower than that of the fresh sample.
- Example 51 After the sample compounded with 5% urea (Example 51) was left at room temperature for one month, the pH value of the sample increased from 5.78 to 7.43, and the viscosity decreased from 1770 mPa ⁇ s to 392 mPa ⁇ s. After the sample was left at 48° C. for one month, its viscosity increased significantly. Compared with the viscosity of the fresh sample which is 1770mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 8680mPa ⁇ s, 18750mPa ⁇ s and 21500mPa ⁇ s respectively. At the same time, the sample pH also increased from 5.78 to 9.28. The above experimental results show that the TA-100 compound emulsification system has a good urea load capacity when compounded with 10% white petrolatum, and the properties of related samples are not significantly different from those in Examples 1-2.
- the sample (embodiment 52) compounded with 20% white petrolatum was placed at room temperature for 1 month, and its pH value was 5.00, which decreased compared to the initial value of 5.40; rise. After being placed at 48°C for one month, the pH value of the sample was 4.95, and the viscosity was 4820mPa ⁇ s, which was slightly lower than that of the newly prepared sample. After the sample compounded with 5% urea (Example 53) was left at room temperature for one month, the pH value rose from 5.76 to 7.55, and the viscosity dropped from 2380mPa ⁇ s to 800mPa ⁇ s. After the sample was left at 48° C. for one month, its viscosity increased significantly.
- the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 14230mPa ⁇ s, 18170mPa ⁇ s and 19500mPa ⁇ s respectively.
- the sample pH also increased from 5.76 to 9.23.
- Examples 54-62 Preparation of TA-100 compound emulsification system samples with different urea addition amounts and urea compositions or derivatives.
- Phase A, Phase B and Phase C weigh appropriate amount of Phase A, Phase B and Phase C in three beakers as shown in Table 6, and heat them in a water bath at 90°C for 30 minutes respectively. Then use a desktop homogenizer to homogenize phase A at 5000rpm for 2 minutes to disperse evenly; then maintain homogenization at 5000rpm and add phase B while it is hot, and maintain homogenization for 2 minutes after adding; continue to maintain homogeneity at 5000rpm and add phase C while it is hot Mix the sample and keep it homogeneous for 5 minutes after adding phase C. Thereafter, the beaker was sealed with a PE film and the sample was allowed to stand overnight at room temperature. Add phase D the next day, and use a desktop homogenizer at room temperature to homogenize again at 5000 rpm for 3 minutes to mix the sample evenly, then seal the beaker with PE film, and keep the sample for later use.
- Table 6 has shown the charging amount of each raw material of embodiment 54-62.
- the emulsification system of Examples 54-62 is the same as that of Examples 1-2, fixed at 5% TA-100 compounded with 2% H-MY.
- the preparation amount of each sample is 200g, and the sample preparation process also adopts the concentrated aqueous phase method consistent with that of Example 1-2.
- Examples 54-61 were all compounded with 6% white petrolatum.
- Example 62 emulsifies 5 kinds of oils (the ratio of oils and fats is the same as that of Example 42), and formulates a urea composition.
- Test example 3 the stability test of embodiment 54-62
- each sample was equally divided into two 150ml transparent PET bottles, and after the screw caps were tightly closed, the samples were respectively placed in a 25°C incubator and a 48°C incubator. Regularly take the sample out of the incubator, let it stand for 6 hours to cool down to room temperature, measure the pH and viscosity of the sample and observe the properties of the sample, and then put the sample back into the incubator after the measurement.
- Table 7 shows the pH values and viscosities of Examples 54-62 at various test time points (Examples 1-2 and Examples 42-43 are listed for comparison).
- Table 7 summarizes the pH values and viscosities of Examples 54-62 at various test time points, and includes the data of Examples 1-2 and Examples 42-43 for comparison. Among them, Examples 1-2 and Examples 54-59 investigated the effects of 8 different urea additions on the properties of the compound emulsification system, according to the order of urea additions: 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 have the same matrix as the above examples, but respectively compounded urea composition (5% urea+5% glycine+0.5% triethyl citrate) and urea derivatives (5% hydroxyethylurea ).
- Example 62 a variety of oils (the emulsified oils are the same as in Example 42) were compounded, and a urea composition was compounded to simulate a complex system close to the actual formulation of cosmetics.
- Example 54 After the sample compounded with 0.1% urea (Example 54) was left at room temperature for one month, its pH value increased slightly from 4.92 to 6.19, and the sample viscosity was 2730mPa ⁇ s, which was a slight increase compared with the freshly prepared sample of 1750mPa ⁇ s. After being stored at 48°C for 1 month, the pH value of the sample increased from 4.92 to 7.98. The viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month were 1020mPa ⁇ s, 850mPa ⁇ s and 608mPa ⁇ s, respectively. The 1750mPa ⁇ s showed a gradual downward trend.
- Example 55 After the sample compounded with 0.2% urea (Example 55) was left at room temperature for one month, its pH value increased slightly from 5.09 to 5.20, and the sample viscosity was 2630mPa ⁇ s, which was slightly higher than that of the newly prepared sample (1780mPa ⁇ s). After being stored at 48°C for 1 month, the pH value of the sample increased from 5.09 to 8.50. The viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month were 780mPa ⁇ s, 580mPa ⁇ s and 408mPa ⁇ s, respectively. The 1750mPa ⁇ s showed a gradual downward trend.
- Example 56 After the sample compounded with 0.5% urea (Example 56) was left at room temperature for one month, its pH value rose from 5.04 to 5.66, and the sample viscosity was 2170 mPa ⁇ s, which was slightly higher than that of the newly prepared sample (1950 mPa ⁇ s). After being stored at 48°C for 1 month, the pH value of the sample increased from 5.04 to 8.82. The viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month were 530mPa ⁇ s, 750mPa ⁇ s and 2142mPa ⁇ s, respectively, compared with the fresh samples The 1950mPa ⁇ s showed a trend of decreasing first and then rising.
- Example 57 After the sample compounded with 1% urea (Example 57) was left at room temperature for one month, its pH value rose from 5.09 to 6.20, and the sample viscosity was 1620mPa ⁇ s, which was slightly lower than that of the freshly prepared sample (1900mPa ⁇ s). After being stored at 48°C for 1 month, the pH value of the sample increased from 5.09 to 8.97. The viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month were 520mPa ⁇ s, 1050mPa ⁇ s and 10830mPa ⁇ s, respectively. The 1900mPa ⁇ s showed a trend of decreasing first and then rising sharply.
- Example 58 After the sample compounded with 2% urea (Example 58) was left at room temperature for one month, its pH value rose from 5.13 to 6.71, and the sample viscosity was 1030 mPa ⁇ s, which was slightly lower than that of the fresh sample (1180 mPa ⁇ s). After being stored at 48°C for 1 month, the pH value of the sample increased from 5.13 to 9.08. The viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month were 1270mPa ⁇ s, 6920mPa ⁇ s and 16250mPa ⁇ s, respectively. The 1180mPa ⁇ s presents a gradual upward trend.
- Example 59 After the sample compounded with 10% urea (Example 59) was left at room temperature for one month, its pH value increased from 5.64 to 7.62, and the sample viscosity was 600mPa ⁇ s, which was significantly lower than that of the fresh sample (1780mPa ⁇ s). After being stored at 48°C for 1 month, the pH value of the sample increased from 5.64 to 9.15. The viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month were 15630mPa ⁇ s, 10050mPa ⁇ s and 11750mPa ⁇ s, respectively. The 1780mPa ⁇ s rises significantly and basically remains stable.
- the pH value of the compound urea composition sample (Example 60) dropped slightly from 5.59 to 5.58 after being left at room temperature for one month, and the sample viscosity was 500 mPa ⁇ s, which was slightly lower than that of the newly prepared sample (820 mPa ⁇ s). After being stored at 48°C for 1 month, the pH value of the sample increased slightly from 5.59 to 5.89.
- the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month were 4330mPa ⁇ s, 8200mPa ⁇ s and 13580mPa ⁇ s, respectively, compared with the fresh The 820mPa ⁇ s of the samples showed a gradual upward trend.
- Example 61 After the sample compounded with 5% hydroxyethyl urea (Example 61) was left at room temperature for one month, its pH value dropped slightly from 8.42 to 8.16, and the viscosity of the sample was 6820 mPa ⁇ s, which was slightly lower than that of the newly prepared sample (8330 mPa ⁇ s). After being stored at 48°C for 1 month, the pH value of the sample increased slightly from 8.42 to 8.92. The viscosities of samples stored at 48°C for 1 week, 2 weeks and 1 month were 8200mPa ⁇ s, 10000mPa ⁇ s and 8120mPa ⁇ s, respectively. The 8330mPa ⁇ s of the sample increased slightly.
- Example 62 After the sample (Example 62) compounded with various oils and urea compositions was left at room temperature for one month, its pH value dropped slightly from 6.76 to 6.19, and the viscosity of the sample was 620mPa ⁇ s, which was slightly higher than that of the newly prepared sample (458mPa ⁇ s). After being stored at 48°C for 1 month, the pH value of the sample dropped from 6.76 to 5.93. The viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month were 5025mPa ⁇ s, 20170mPa ⁇ s and 11530mPa ⁇ s, respectively, compared with the fresh samples The 458mPa ⁇ s rises significantly.
- the TA-100 compound emulsification system can carry different amounts of urea, urea derivatives and urea compositions, and all samples have no problems of delamination and demulsification.
- the main performance is to destroy the existing micelle structure to reduce the viscosity of the material body; but in the case of high urea content and more decomposition products, it promotes new polymerization.
- the formation of micelles with greater density increases the viscosity of the material significantly.
- Example 60 and Example 61 compounded urea composition and urea derivatives on the basis of Example 1.
- the above two examples can stably carry urea, and the properties are similar to other compounded urea samples. It should be pointed out that the pH values of the two samples did not increase significantly, indicating that the phenomenon that urea promotes the remodeling of TA-100 micelles does not only occur under strong alkaline conditions.
- the TA-100 compound emulsification system reported in the present invention can exhibit its unique properties under the premise of meeting the national cosmetics regulations on sample pH supervision standards.
- Example 62 On the basis of Example 60, various oils were compounded, and the performance of this sample in the stability test was basically the same as that of the latter.
- the emulsification system reported in this invention still has good load-carrying properties and exhibits unique viscosity-increasing properties, indicating that the compound emulsification system has a wide range of adjustment space for oils and additives, which is beneficial to Its application in cosmetics.
- Examples 63-88 Preparation of TA-100 composite emulsification system samples with the addition amount of TA-100 adjusted, the type and amount of long-chain fatty alcohol added, and the corresponding urea-containing samples.
- Phase A, Phase B and Phase C weigh appropriate amount of Phase A, Phase B and Phase C in three beakers as shown in Table 8, and heat them in a water bath at 90°C for 30 minutes respectively. Then use a desktop homogenizer to homogenize phase A at 5000rpm for 2 minutes to disperse evenly; then maintain homogenization at 5000rpm and add phase B while it is hot, and continue homogenizing for 2 minutes after adding; continue to maintain homogenization at 5000rpm and add phase C while it is hot Mix the sample and keep it homogeneous for 5 minutes after adding phase C. Thereafter, the beaker was sealed with a PE film and the sample was allowed to stand overnight at room temperature. Add phase D the next day, and use a desktop homogenizer at room temperature to homogenize again at 5000 rpm for 3 minutes to mix the sample evenly, then seal the beaker with PE film, and keep the sample for later use.
- Table 8 shows the types of long-chain fatty alcohols added in Examples 63-88 and the feeding amount of each raw material.
- the fixation process of Examples 63-88 is the concentrated aqueous phase method, the amount of oil added is 6% white petrolatum, and the preparation amount of each sample is 200 g.
- the addition amount of TA-100 was fixed at 5%.
- Examples 79-88 fixed the long-chain fatty alcohol as 2% H-MY, and investigated the effect of the addition amount of TA-100 on the properties of the material body.
- Each sample was prepared with a base material and an example containing urea, and the addition amount of urea in the examples containing urea was 5%.
- Test example 4 the stability test of embodiment 63-88
- each sample was equally divided into two 150ml transparent PET bottles, and after the screw caps were tightly closed, the samples were respectively placed in a 25°C incubator and a 48°C incubator. Regularly take the sample out of the incubator, let it stand for 6 hours to cool down to room temperature, measure the pH and viscosity of the sample and observe the properties of the sample, and then put the sample back into the incubator after the measurement.
- Table 9 shows the pH and viscosity of Examples 63-88 at various test time points (listed in Examples 1-2).
- Table 9 summarizes the pH values and viscosities of Examples 63-88 at various test time points, and includes the data of Examples 1-2 for comparison.
- embodiment 1-2 and embodiment 63-74 investigated the influence of 7 kinds of different H-MY addition amounts, according to the order of H-MY addition amount: 0% (embodiment 63-64), 0.5% ( Examples 65-66, 1% (Example 67-68), 2% (Example 1-2), 3% (Example 69-70), 4% (Example 71-72) and 5% (Example 71-72) Examples 73-74).
- Examples 75-76 and 77-78 were compounded with 2% behenyl alcohol and 2% cetyl alcohol respectively.
- Example 63 The sample (Example 63) without reconstituted long-chain fatty alcohol was placed at room temperature for 1 month, and its pH value was 6.06, which increased slightly compared with the initial value of 5.61; risen. After being placed at 48°C for one month, the pH value of the sample was 5.35, which was slightly lower than the initial value, while the viscosity was 617mPa ⁇ s, which was basically the same as that of the freshly prepared sample. After the sample compounded with 5% urea (Example 64) was left at room temperature for one month, the pH value increased from 5.90 to 7.38, and the viscosity decreased slightly from 1030 mPa ⁇ s to 783 mPa ⁇ s.
- the sample After the sample was placed at 48°C for one month, its viscosity decreased significantly. Compared with the viscosity of the fresh sample which is 1030mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 280mPa ⁇ s, 280mPa ⁇ s and 280mPa ⁇ s respectively.
- the sample pH also increased from 5.90 to 8.98. It is necessary to point out that solid blocks appear in all the above samples, which is due to the insufficient stability of the emulsified system, which in turn leads to the precipitation of oil and accumulation into blocks.
- Example 65 After the sample (Example 65) with a compounding amount of cetearyl alcohol (H-MY) of 0.5% was placed at room temperature for 1 month, its pH value was 5.68, which increased slightly compared to the initial value of 5.31; the sample viscosity was 400mPa ⁇ s , which is slightly higher than the 380mPa ⁇ s of the newly prepared sample. After being placed at 48°C for one month, the pH value of the sample was 4.97, which was slightly lower than the initial value, while the viscosity was 725mPa ⁇ s, which was higher than that of the fresh sample.
- H-MY cetearyl alcohol
- Example 66 After the sample compounded with 5% urea (Example 66) was left at room temperature for one month, the pH value increased from 5.62 to 7.41, and the viscosity decreased slightly from 420mPa ⁇ s to 250mPa ⁇ s. After the sample was placed at 48°C for one month, its viscosity decreased. Compared with the viscosity of 420mPa ⁇ s for the fresh sample, the viscosity of the samples stored at 48°C for 1 week, 2 weeks and 1 month were 270mPa ⁇ s, 280mPa ⁇ s and 208mPa ⁇ s, respectively. At the same time, the sample pH also increased from 5.62 to 9.00.
- Example 67 After the sample (Example 67) with a compounding amount of cetearyl alcohol (H-MY) of 1% was placed at room temperature for 1 month, its pH value was 5.49, a slight increase compared to the initial value of 5.31; the sample viscosity was 358mPa ⁇ s , which is slightly lower than the 430mPa ⁇ s of the newly prepared sample. After being placed at 48°C for one month, the pH value of the sample was 4.81, which was lower than the initial value, while the viscosity was 575 mPa ⁇ s, which was slightly higher than that of the fresh sample.
- H-MY cetearyl alcohol
- Example 68 After the sample compounded with 5% urea (Example 68) was left at room temperature for one month, the pH value increased from 5.65 to 7.46, and the viscosity decreased from 670mPa ⁇ s to 267mPa ⁇ s. After the sample was placed at 48°C for one month, its viscosity showed an obvious upward trend. Compared with the viscosity of the freshly prepared sample which is 670mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 2880mPa ⁇ s, 5330mPa ⁇ s and 7920mPa ⁇ s respectively. At the same time, the sample pH also increased from 5.65 to 9.00.
- the above experimental results show that the TA-100 emulsification system compounded with 1% cetearyl alcohol can carry urea, and its properties are basically the same as those in Example 2.
- Example 69 After the sample (Example 69) with a compounding amount of cetearyl alcohol (H-MY) of 3% was placed at room temperature for 1 month, its pH value was 5.62, a slight increase compared to the initial value of 5.32; the sample viscosity was 9630mPa ⁇ s , a slight increase compared to the 7780mPa ⁇ s of the new sample. After being stored at 48°C for one month, the pH value of the sample was 4.79, which was lower than the initial value, while the viscosity was 8450 mPa ⁇ s, which was slightly higher than that of the fresh sample.
- H-MY cetearyl alcohol
- Example 70 After the sample compounded with 5% urea (Example 70) was left at room temperature for one month, the pH value increased from 5.76 to 7.63, and the viscosity decreased slightly from 36420mPa ⁇ s to 31580mPa ⁇ s. After the sample was placed at 48°C for one month, its viscosity showed a slight downward trend. Compared with the viscosity of the fresh sample which is 36420mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 23580mPa ⁇ s, 23000mPa ⁇ s and 21670mPa ⁇ s respectively. At the same time, the sample pH also increased from 5.76 to 9.06.
- Example 2 The above experimental results show that the TA-100 emulsification system compounded with 3% cetearyl alcohol can carry urea.
- the difference from Example 2 is that the immediate viscosity of the sample increases significantly after compounding urea, and the urea-containing sample is Viscosity decreased slightly in the test over time, indicating that a higher amount of cetearyl alcohol can make the TA-100 compound emulsification system exhibit unique properties.
- Example 71 The sample (Example 71) with a compounding amount of cetearyl alcohol (H-MY) of 4% was left at room temperature for 1 month, and its pH value was 5.62, a slight increase compared to the initial value of 5.16; the sample viscosity was 32580mPa ⁇ s , which is slightly lower than that of the newly prepared sample at 36830mPa ⁇ s. After being stored at 48°C for one month, the pH value of the sample was 5.79, which was higher than the initial value, while the viscosity was 35330 mPa ⁇ s, which was slightly lower than that of the fresh sample.
- H-MY cetearyl alcohol
- Example 72 After the sample compounded with 5% urea (Example 72) was left at room temperature for one month, the pH value rose from 5.79 to 7.83, and the viscosity was 53420 mPa ⁇ s, which was consistent with the fresh sample. After the sample was placed at 48°C for one month, its viscosity showed a slight upward trend. Compared with the viscosity of the fresh sample which is 53420mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 48420mPa ⁇ s, 59920mPa ⁇ s and 65170mPa ⁇ s respectively. At the same time, the sample pH also increased from 5.79 to 8.94.
- Example 73 The sample (Example 73) with a compounding amount of cetearyl alcohol (H-MY) of 5% was left at room temperature for 1 month, and its pH value was 5.57, a slight increase compared to the initial value of 5.05; the sample viscosity was 32580mPa ⁇ s , compared with the new sample 45250mPa ⁇ s decreased. After being placed at 48°C for one month, the pH value of the sample was 5.90, which was higher than the initial value, while the viscosity was 35000mPa ⁇ s, which was lower than that of the fresh sample.
- H-MY cetearyl alcohol
- Example 74 After the sample of 5% urea (Example 74) was left at room temperature for one month, the pH value rose from 5.79 to 7.99, and the viscosity rose from 53420mPa ⁇ s to 66250mPa ⁇ s. After the sample was placed at 48°C for one month, its viscosity showed an upward trend. Compared with the viscosity of the fresh sample which is 53420mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 48420mPa ⁇ s, 61630mPa ⁇ s and 73080mPa ⁇ s respectively. At the same time, the sample pH also increased from 5.79 to 8.96.
- the above experimental results show that the TA-100 emulsification system compounded with 5% cetearyl alcohol can carry urea, and consistent with Example 2, the urea-containing sample shows an upward trend in the high-temperature time-dependent stability test.
- Example 75 After the sample (Example 75) compounded with 2% behenyl alcohol (i.e. behenyl alcohol) was placed at room temperature for 1 month, its pH value was 5.28, a slight increase compared to the initial value of 4.88; Compared with the new sample 13580mPa ⁇ s decreased. After being placed at 48°C for one month, the pH value of the sample was 5.12, which was higher than the initial value, while the viscosity was 10500 mPa ⁇ s, which was slightly lower than that of the fresh sample.
- behenyl alcohol i.e. behenyl alcohol
- Example 76 After the sample compounded with 5% urea (Example 76) was left at room temperature for one month, the pH value rose from 5.54 to 7.67, and the viscosity dropped from 14170 mPa ⁇ s to 7500 mPa ⁇ s. After the sample was placed at 48°C for one month, its viscosity showed an upward trend. Compared with the viscosity of the fresh sample which is 14170mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 15670mPa ⁇ s, 26080mPa ⁇ s and 27250mPa ⁇ s respectively. At the same time, the sample pH also increased from 5.54 to 9.06.
- the above experiments show that the TA-100 compound emulsification system has a broad space in the selection of the type and compound amount of long-chain fatty alcohols.
- the viscosity of the material body can be adjusted by adjusting the type and amount of the long-chain fatty alcohol added to meet the viscosity requirements of cosmetic formulas of different models, which is beneficial to the practical application of the present invention in the cosmetics industry.
- the viscosity of the sample increases significantly after adding urea, indicating that the compound emulsification system reported in this invention has more advantages in the application of cream or high-viscosity emulsion.
- Embodiment 1-2 and embodiment 79-88 investigated the influence of 6 kinds of different TA-100 additions, according to the order of TA-100 additions: 0% (embodiment 79-80), 0.5% (embodiment 81-82), 2.5% (Examples 83-84), 5% (Examples 1-2), 7.5% (Examples 85-86) and 10% (Examples 87-88).
- the pH value of the sample without TA-100 added (Example 79) dropped slightly from 4.88 to 4.62 after being left at room temperature for one month; in addition, because the emulsifying ability and suspending power of the formula were too low, the material was found to be separated at various test time points and demulsification. After being placed at 48°C for one month, the samples were also delaminated and demulsified at various time points. After the stability test, the pH value of the sample was 4.57, which was slightly lower than the initial value. After the sample compounded with 5% urea (Example 80) was left at room temperature for one month, the pH value rose from 6.13 to 8.29, and the samples showed delamination and demulsification at various time points.
- Example 81 After the compound emulsification system (Example 81) with 0.5% compounding amount of TA-100 was left at room temperature for one month, the pH value of the sample dropped slightly from 5.38 to 4.87; the samples were uniformly separated at each time point. After being placed at 48°C for one month, the samples were still separated due to the low viscosity at various time points. After the stability test, the pH value of the samples was 4.85, which was slightly lower than the initial value. After the sample compounded with 5% urea (Example 82) was left at room temperature for one month, the pH value rose from 6.18 to 8.23, and the sample still showed stratification at each time point. However, Example 82 exhibited unique properties in the high-temperature test at 48°C over time.
- the viscosities of the samples stored at 48°C for 1 week, 2 weeks, and 1 month were 1350mPa ⁇ s, 4458mPa ⁇ s, and 18250mPa ⁇ s, respectively. There is a significant upward trend from the initial value.
- the above experimental results show that the compound emulsification system with 0.5% compounding amount of TA-100 shows a phenomenon that the viscosity increases significantly in the high temperature time test. This finding means that a lower concentration of TA-100 can be used to compound with other surfactants, which may increase the urea carrying capacity of the latter, so that the formulations that cannot stably carry urea can meet the national regulations on the stability of cosmetics Requirements, it has high value in the practical application of cosmetic industry.
- Example 83 The sample (Example 83) with a compounding amount of TA-100 of 2.5% was placed at room temperature for 1 month, and its pH was 4.97, which was lower than the initial value of 5.60; s rises slightly. After being stored at 48°C for one month, the pH value of the sample was 4.85, which was lower than the initial value, while the viscosity was 542 mPa ⁇ s, which was higher than that of the fresh sample. After the sample compounded with 5% urea (Example 84) was left at room temperature for one month, the pH value increased from 6.13 to 8.17, and the viscosity slightly decreased from 420mPa ⁇ s to 383mPa ⁇ s.
- Example 85 The sample (Example 85) with a compounding amount of TA-100 of 7.5% was left at room temperature for one month, and its pH was 4.89, which was slightly lower than the initial value of 5.23; the viscosity of the sample was 28170mPa ⁇ s, which was 27000mPa ⁇ s compared to the fresh sample rise slightly. After being placed at 48°C for one month, the pH value of the sample was 4.79, which was slightly lower than the initial value, and the viscosity was 23670 mPa ⁇ s, which was also slightly lower than that of the fresh sample.
- Example 86 After the sample compounded with 5% urea (Example 86) was left at room temperature for one month, the pH value rose from 6.15 to 7.67, and the viscosity dropped from 41420mPa ⁇ s to 25500mPa ⁇ s. After the sample was placed at 48°C for one month, its viscosity showed a trend of first decreasing and then increasing. Compared with the viscosity of the fresh sample which is 41420mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 12930mPa ⁇ s, 25670mPa ⁇ s and 55300mPa ⁇ s respectively. At the same time, the sample pH also increased from 6.15 to 9.14. The above experimental results show that the compound emulsification system with TA-100 added at 7.5% can carry urea, and the properties of related samples are basically consistent with those in Examples 1-2.
- the sample (Example 87) with a compounding amount of TA-100 of 10% was placed at room temperature for one month, and its pH was 4.97, which was slightly lower than the initial value of 5.08; the viscosity of the sample was 30420mPa ⁇ s, which was 29080mPa ⁇ s compared to the fresh sample rise slightly.
- the pH value of the sample was 4.90, which was slightly lower than the initial value, while the viscosity was 28330 mPa ⁇ s, which was slightly lower than that of the fresh sample.
- Example 88 After the sample compounded with 5% urea (Example 88) was left at room temperature for one month, the pH value rose from 5.58 to 7.47, and the viscosity dropped from 49180 mPa ⁇ s to 23920 mPa ⁇ s. After the sample was placed at 48°C for one month, its viscosity showed a trend of first decreasing and then increasing. Compared with the viscosity of the fresh sample which is 49180mPa ⁇ s, the viscosities of the samples stored at 48°C for 1 week, 2 weeks and 1 month are 16270mPa ⁇ s, 45500mPa ⁇ s and 85700mPa ⁇ s respectively. At the same time, the sample pH also increased from 5.58 to 9.24. The above experimental results show that the compound emulsification system with 10% addition of TA-100 can carry urea, and the properties of related samples are basically consistent with those of Examples 1-2.
- the compound emulsification system reported in the present invention has the ability to stably carry urea within a wide range of TA-100 compounding amount.
- the viscosity of the material can be changed by adjusting the amount of TA-100 added, which is beneficial to the application of the technology reported in this invention to various cosmetic formulations.
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Abstract
本发明提供了一种承载尿素或其衍生物的稳定组合物，所述组合物包含：(a)油脂；(b)阳离子乳化剂，所述阳离子乳化剂是二硬脂基二甲基氯化铵；(c)长链脂肪醇，所述长链脂肪醇的碳链长度为16-22；(d)水相；其中，所述尿素衍生物是尿素的碳原子数为1-6的羟烷基化物，其中，所述阳离子乳化剂与长链脂肪醇的重量比为10:1至1:4，所述阳离子乳化剂与承载的尿素或其衍生物的重量比为1:10至50:1。
Description
本发明涉及化妆品领域，具体涉及承载尿素或其衍生物的稳定组合物及其在化妆品中的应用。
尿素是皮肤的天然保湿因子之一，其保湿、软化肌肤、促进经皮渗透等功效已被文献广泛报道。文献“仪器和皮肤科医生评估甘油和尿素对特应性皮炎患者干性皮肤的影响”，《皮肤研究和技术》，Lodén M.等报道了使用含有4％尿素的保湿霜30天后，35位受试者的皮肤电容值平均值从35A.U.上升到了42A.U.(皮肤表层含水量越高，电容值越高)、表皮水分流失量平均值从约11g/(m
2·h)下降到月8.5g/(m
2·h)，干燥度总分平均值自3.2下降至0.8，以上实验结果均显著优于未添加尿素的对照组，且具有统计学差异，证明了尿素保湿、柔肤、强韧肌肤屏障的功效。文献“尿素对人表皮、皮肤的影响”，Hellgren等报道了将干燥后的表皮浸没于10％尿素溶液中，90h基本达到平衡后表皮吸水量接近初始质量的300％，吸水量约等于浸没于蒸馏水中样品的3倍。干燥皮肤吸水量的增加，来自于尿素水溶液提高了表皮的渗透性。文献“透皮促渗剂对两种锌盐经皮渗透新的影响”，Science Technology and Engineering，2016；16:1671-1815陈传秀，金青，谭然然，课题组研究了尿素对共轭亚油酸锌及葡萄糖酸锌经皮渗透的影响，发现在料体中加入2％尿素，共轭亚油酸锌的单位时间累积渗透量由188.23μg/cm
2上升到了388.04μg/cm
2，葡萄糖酸锌的单位时间累积渗透量由682.26μg/cm
2上升到了1020.49μg/cm
2，且随着尿素含量的提升渗透速率仍有进一步的提高。
近年来的研究对尿素对皮肤的护理功效有了更为深入的揭示。如文献“尿素摄取通过调节表皮基因表达增强人体屏障功能和抗菌防御”，皮肤病 研究杂志Susanne G.-B.,(2012)132,1561–1572报道了尿素可提高与皮肤屏障相关基因AMP、LL-37及β-防卫素-2的表达，并对尿素调控基因表达，提高皮肤屏障和抗菌的作用机理进行了详细的研究。根据研究结果，作者认为尿素并非只是机体代谢产物，而作为一种小分子调节剂，具有修饰皮肤屏障相关基因表达的效果。此外，《尿素和皮肤：一个著名的分子重访》汇总了尿素作为药品，应用于牛皮鲜、过敏性皮炎、湿疹、溢脂性皮炎等皮肤疾病的治疗。
但是，将具有强效皮肤护理功效的尿素实际应用于化妆品或皮肤医疗品中，却面临诸多挑战。其中之一为尿素的水解会产生较强的碱性及离子性，对化妆品配方基质的承载力提出很高的要求。例如，上海家化联合股份有限公司的12种在售乳液配方进行测试后发现(粘度1000mPa·s至20000mPa·s，每个配方使用乳化剂及增稠剂均不同)，其中11种配方在复配尿素及尿素+甘氨酸+柠檬三乙酯组合物后，在高温经时稳定性测试中粘度显著下降，并出现分层、破乳等稳定性问题，无法满足国家法规对化妆品稳定性的要求。在对以上12种配方涉及的乳化剂和增稠剂进行进一步测试后发现，以上物质在与尿素复配后，大多数样品在高温经时测试中无法保持稳定(测试例1)。
因尿素对配方体系承载力要求苛刻，大部分化妆品市售配方的承载力不能满足复配尿素的要求，故使得功效性强，安全性良好，价格低廉的尿素，在目前化妆品商品中使用率很低(据2020年Mintel基于全球市场的搜索结果，含尿素的化妆品比例仅为2.8％)。而且，当下添加尿素化妆品中，多数仅为微量添加以起到稳定配方pH值的作用，其添加量远低于上述文献报道的尿素功效添加量。
因此，开发能够稳定承载尿素或其衍生物、或者包含尿素或其衍生物的组合物的配方基质，对于促进尿素及其衍生物在化妆品中的应用具有重要的意义。
发明内容
一方面，本发明提供了一种承载尿素或其衍生物的稳定组合物，所述 组合物包含：
(a)油脂；
(b)阳离子乳化剂，所述阳离子乳化剂是二硬脂基二甲基氯化铵；
(c)长链脂肪醇，所述长链脂肪醇的碳链长度为16-22；
(d)水相；
其中，所述尿素衍生物是尿素的碳原子数为1-6的羟烷基化物，
其中，所述阳离子乳化剂与长链脂肪醇的重量比为10:1至1:4，所述阳离子乳化剂与承载的尿素或其衍生物的重量比为1:10至50:1。
在优选的实施方式中，组合物中的油脂选自：非极性固态油脂；非极性液态油脂；极性液态油脂；极性固态油脂；硅油；或它们的混合物。在优选的实施方式中，组合物包含0.1-20重量％的油脂。
在优选的实施方式中，组合物包含2.5-10重量％的阳离子表面活性剂。
在优选的实施方式中，组合物中的长链脂肪醇选自：十六醇、鲸蜡硬脂醇、十八醇、二十醇、二十二醇或它们的混合物。在优选的实施方式中，组合物包含0.1-10重量％的长链脂肪醇。
在优选的实施方式中，组合物包含1重量％以上的尿素或其衍生物。
在优选的实施方式中，组合物包含50重量％以上的水相。
在优选的实施方式中，组合物中阳离子乳化剂与长链脂肪醇的重量比为10:1至1:2，阳离子乳化剂与承载的尿素或其衍生物的重量比为1:2至10:1。
另一方面，本发明还提供了一种皮肤外用剂，其包含本发明所述的稳定组合物。
本发明意外地发现了一种可承载尿素或其衍生物的稳定组合物，并且该组合物在合适配比下于高温经时测试中表现出反常的增粘现象。因此，本发明的乳化技术在未来化妆品和皮肤医疗品的实际应用中具有很高的实用价值。
为了提供更简明的描述，本文给出的一些数量表述没有用术语“约”修 饰。应当理解，无论是否明确地使用了术语“约”，本文所给出的每个量都意在指代实际的给定值，并且还意在指代由本领域的普通技术人员可合理推测出的这些给定值的近似值，包括这些给定值的由实验和/或测量条件所引起的近似值。
为了提供更简洁的描述，本文中一些数量表述被叙述为约X量至约Y量的范围。应当理解，当叙述范围时，该范围并不限制于所叙述的上下界限，而应包括约X量至约Y量的整个范围或它们之间的任何量。
尿素
尿素是皮肤的天然保湿因子之一，其保湿、软化肌肤、促进经皮渗透等功效已被文献广泛报道。然而，将具有强效皮肤护理功效的尿素实际应用于化妆品或皮肤医疗品中，却面临诸多挑战。尿素对配方体系承载力要求苛刻，大部分化妆品市售配方的承载力不能满足复配尿素的要求。
本发明创新性地提供了一种能够承载尿素或其衍生物的稳定组合物。
在一些具体的实施方式中，本发明的稳定组合物承载的尿素是尿素复配物的形式。例如，所述尿素复配物是尿素：甘氨酸：柠檬酸三乙酯以重量比10:10:1形成的复配物。在一个具体的实施方式中，尿素复配物是5％尿素、5％甘氨酸和0.5％柠檬酸三乙酯的复配物。
在一些具体的实施方式中，本发明的稳定组合物承载的尿素是尿素衍生物。例如，尿素衍生物是尿素的羟烷基化衍生物。在一个具体的实施方式中，尿素衍生物是碳原子数为1-6的羟烷基化衍生物。在一个具体的实施方式中，尿素衍生物是羟乙基脲。
在本发明的一些实施方式中，稳定组合物包含0.1-20重量％的尿素或其衍生物。在本发明的一些实施方式中，稳定组合物包含0.1-10重量％的尿素或其衍生物。
在本发明的一些实施方式中，稳定组合物包含1重量％以上的尿素或其衍生物。在本发明的一些实施方式中，稳定组合物包含2重量％以上的尿素或其衍生物。在本发明的一些实施方式中，稳定组合物包含3重量％以上的尿素或其衍生物。在本发明的一些实施方式中，稳定组合物包含4 重量％以上的尿素或其衍生物。在本发明的一些实施方式中，稳定组合物包含5重量％以上的尿素或其衍生物。
油脂
本发明承载尿素或其衍生物的稳定组合物包含油脂。在一些具体的实施方式中，本发明的稳定组合物中包含的油脂选自：(1)非极性固态油脂；(2)非极性液态油脂；(3)极性液态油脂；(4)极性固态油脂；(5)硅油；或者它们的任意混合物。
在一些具体的实施方式中，本发明的稳定组合物包含白凡士林。在一些具体的实施方式中，本发明的稳定组合物包含10#白油。在一些具体的实施方式中，本发明的稳定组合物包含棕榈酸异辛酯。在一些具体的实施方式中，本发明的稳定组合物包含十六酸十六酯。例如，在一些具体的实施方式中，本发明的稳定组合物包含购自Croda(新加坡)的十六酸十六酯ACP。在一些具体的实施方式中，本发明的稳定组合物包含二甲基硅油。例如，在一些具体的实施方式中，本发明的稳定组合物包含购自陶氏(张家港)投资有限公司的二甲基硅油(100cst)。
在本发明的一些实施方式中，稳定组合物包含0.1-20重量％的油脂。在本发明的一些实施方式中，稳定组合物包含1-20重量％的油脂。在本发明的一些实施方式中，稳定组合物包含1-10重量％的油脂。在本发明的一些实施方式中，稳定组合物包含5-10重量％的油脂。
阳离子表面活性剂
阳离子表面活性剂指一种带有阳离子基团的乳化剂，其分子结构包括阳离子基团和烷基链。其中，阳离子基团主要包括烷基季铵盐、烷基吡啶盐、烷基胺盐，普遍具有良好的耐热、耐光、酸碱耐受性，并具有良好的表面活性、稳定性和生物降解性。因阳离子表面活性剂独特的电荷性质，能够在皮肤或头发表面成膜，故而具有独特的产品使用感，尤其在发用产品中应用广泛。
在发用产品中复配阳离子表面活性剂，阳离子表面活性剂的烷基链附 着于角质表面而形成阳离子膜，阳离子膜的电荷排斥性使基质出现润滑作用，具体表现为产品使用后头发光滑、柔软，并且减少了梳理头发所需的力。相比而言，因阴离子增稠剂的广泛应用，护肤品中阳离子表面活性剂使用相对较少。然而，阳离子表面活性剂具有的强吸收感和成膜性，可显著屏蔽油脂的粘腻感，能够使产品具有独特的使用感，若能够应用在合适产品中即可在化妆品市场中具备独特的竞争力。
本发明的稳定组合物包含阳离子表面活性剂。在一个具体的实施方式中，本发明的稳定组合物采用的阳离子表面活性剂是二硬脂基二甲基氯化铵。在一个具体的实施方式中，本发明的稳定组合物采用的阳离子表面活性剂是购自Evonik Operations GmbH的TA-100。
本发明意外地发现，采用二硬脂基二甲基氯化铵可以得到能够承载尿素或其衍生物的稳定组合物。还出乎意料的是，部分样品在与尿素复配后，在高温经时稳定性测试中，样品粘度显著提升，而未复配尿素的样品却未出现类似反常现象。该反常现象在化妆品和皮肤医疗品实际生产中具有较高的应用价值：(1)将二硬脂基二甲基氯化铵与其它乳化剂复配，可改善或避免后者与尿素复配后料体粘度显著降低的现象；(2)通过在配制过程中对料体进行高温陈化，继而调控样品粘度；(3)可利用该特性制备硬质膏霜并在强化试验中保持稳定。还有必要指出的是，尿素的功效适用于干性皮肤的护理，而为此类肤质设计的化妆品油脂添加量普遍较高，故而肤感油腻、吸收性差。二硬脂基二甲基氯化铵因其阳离子特性，应用于化妆品中具有极强的吸收感和遮盖性，可有效善高油脂添加量配方的油腻感，提升其吸收性，在满足化妆品的功效性的同时，让消费者获得更好使用体验。
在本发明的一些实施方式中，稳定组合物包含0.5-20重量％的阳离子表面活性剂。在本发明的一些实施方式中，稳定组合物包含1-20重量％的阳离子表面活性剂。在本发明的一些实施方式中，稳定组合物包含1-10重量％的阳离子表面活性剂。在本发明的一些实施方式中，稳定组合物包含2.5-10重量％的阳离子表面活性剂。在本发明的一些实施方式中，稳定组合物包含5-10重量％的阳离子表面活性剂。
在本发明的一些实施方式中，阳离子乳化剂与承载的尿素或其衍生物的重量比为1:10至50:1。在本发明的一些实施方式中，阳离子乳化剂与承载的尿素或其衍生物的重量比为1:10至10:1。在本发明的一些实施方式中，阳离子乳化剂与承载的尿素或其衍生物的重量比为1:2至10:1。在本发明的一个具体实施方式中，阳离子乳化剂与承载的尿素或其衍生物的重量比为1:1。
长链脂肪醇
本发明承载尿素或其衍生物的稳定组合物包含长链脂肪醇。在一些具体的实施方式中，本发明的稳定组合物中包含的长链脂肪醇是碳原子数是16-22的长链脂肪醇。
在一些具体的实施方式中，本发明的稳定组合物包含的长链脂肪醇选自：十六醇、鲸蜡硬脂醇、十八醇、二十醇、二十二醇或它们的混合物。
在本发明的一些实施方式中，稳定组合物包含0.1-10重量％的长链脂肪醇。在本发明的一些实施方式中，稳定组合物包含0.5-10重量％的长链脂肪醇。在本发明的一些实施方式中，稳定组合物包含1-10重量％的长链脂肪醇。在本发明的一些实施方式中，稳定组合物包含1-5重量％的长链脂肪醇。在本发明的一些实施方式中，稳定组合物包含3-5重量％的长链脂肪醇。
在本发明的一些实施方式中，阳离子乳化剂与长链脂肪醇的重量比为10:1至1:4。在本发明的一些实施方式中，阳离子乳化剂与长链脂肪醇的重量比为10:1至1:2。在本发明的一些实施方式中，阳离子乳化剂与长链脂肪醇的重量比为10:1至1:1。在本发明的一个具体实施方式中，阳离子乳化剂与长链脂肪醇的重量比为5:2。
水相
本发明的稳定组合物还包含水相。在一些具体的实施方式中，水相可以是水或其它含水载体。
在本发明的一些实施方式中，稳定组合物包含50重量％以上的水相。 在本发明的一些实施方式中，稳定组合物包含60重量％以上的水相。在本发明的一些实施方式中，稳定组合物包含70重量％以上的水相。在本发明的一些实施方式中，稳定组合物包含80重量％以上的水相。
皮肤外用剂
本发明的组合物可以作为功效添加剂应用于皮肤外用剂中。在一些实施方式中，所述皮肤外用剂选自：洁面乳、化妆水、乳液、膏霜、啫喱、面膜。根据制剂的不同类型添加不同的用量。
所述皮肤外用剂是通常用于皮肤外部的所有成分的统称概念，例如可以是化妆品组合物。所述化妆品组合物中可以是基础化妆品、面部妆容化妆品、身体用化妆品、头发护理用化妆品等，对其剂型无特殊限制，根据不同目的可合理选择。所述化妆品组合物中根据剂型和目的的不同还含有不同的化妆品学层面允许的介质或基质赋形剂。
本发明的稳定组合物形成乳化体系，尤其适用于干性及中干性的皮肤的皮肤护理，并且在手部、足部、身体护理的化妆品中具有独特的优势。
例如，根据一项14天消费者留置测试反馈的结果，认同本发明的稳定组合物适用于手部能够滋润肌肤、柔软肌肤、细致肌肤、提升肌肤光泽、预防皴裂、缓解干裂、缓解紧绷感、光滑皮肤的比例依次为98％、98％、98％、96％、96％、94％、96％和98％，且实验结果可以得到实验室客观指标测定的支持(皮肤含水量、经皮水分流失、皮肤弹性、皮肤鳞屑值、皮肤平滑度在即时和使用4周后均有改善，且相比对照组具有统计学差异)。此外，94％的消费者认同该产品易于吸收且吸收后不粘腻，98％的消费者认同该产品具有保护膜感。由此可知，本发明所报道的技术应用在合适产品中，可同时赋予产品良好的使用感与功效，使产品具有很强的产品竞争力。
下面结合具体实施例，以进一步阐述本发明。有必要在此指出的是，实施例只用于对本发明进行进一步的说明，不能理解为对本发明保护范围的限制，该领域的技术熟练人员可以根据上述本发明的内容做出一些非本质的改进和调整。下列实施例中未注明具体条件的试验方法，通常按照常 规条件，或按照制造厂商所建议的条件。除非另有说明，所有的百分比和份数按重量计。
实验材料：
二硬脂基二甲基氯化铵(TA-100)：购自Evonik Operations GmbH；
鲸蜡硬脂醇(H-MY)：购自Emery Oleochemicals(M)Sdn Bhd；
白凡士林：购自汉圣化工(抚顺)有限公司；
尿素：购自国药集团化学试剂有限公司；
羟乙基脲(50％)：购自广州西普精细化工科技有限公司；
柠檬酸三乙酯：购自上海浦杰香料有限公司；
甘氨酸：购自河北华阳生物科技有限公司；
鲸蜡醇(十六醇)：购自BASF；
山嵛醇(二十二醇)：购自BASF；
阳离子调理剂ECON-100：购自重庆海帆生化科技有限公司；
月桂醇磷酸酯钾盐(HR-S1)：购自辽宁丹东安康化学厂；
聚甘油五硬脂酸酯及硬脂酰乳酸钠：购自NIKKOL CHEMICAL CO.LTD；
甘油月桂酸酯：购自BASF；
聚甘油-10肉豆蔻酸酯(单豆蔻酸聚甘油酯)：购自NIKKOL CHEMICAL CO.LTD；
PEG-20甲基葡糖倍半硬脂酸酯(MSE-20)：路博润特种化工(上海)有限公司；
鲸蜡硬脂醇聚醚-30：购自BASF；
阿拉通2121：购自CRODA；
聚季铵盐-37(PQ-37)：购自BASF；
接枝玉米淀粉25：购自Daito KaseiKogyo Co.,Ltd.；
黄原胶：购自Jungbunzlauer Austria AG；
聚丙烯酸钠：购自森馨日本；
丙烯酰二甲基牛磺酸铵/VP共聚物(AVC)：购自Clariant；
10#白油：购自浙江正信石油科技有限公司；
棕榈酸异辛酯：购自PALM-OLEO(KLANG)SDN BHD；
十六酸十六酯ACP：购自Croda(新加坡)；
二甲基硅油(100cst)：购自陶氏(张家港)投资有限公司。
实验仪器：
称量天平：METTLER TOLEDO，PB4002-N；
恒温水浴锅：上海一恒科学仪器有限公司，HWS-28；
台式均质机：POLYTRON，PT 3100 D；
台式搅拌器：IKA EUROSTAR，power control-visc；
25℃恒温烘箱：德国MMM公司，FRIOCELL707；
48℃恒温烘箱：德国MMM公司，FRIOCELL707；
pH计：METTLER TOLEDO，SevenMulti；
粘度计：BROOKFIELD，DV-S数显粘度计。
实施例1-18：含有不同表面活性剂的乳化体系及相应含尿素样品的制备。
按表1所示在三个烧杯中称取适量A相、B相及C相，分别于90℃水浴锅中加热30min。之后使用台式均质机以5000rpm均质A相2min使之分散均匀；此后保持5000rpm均质并趁热加入B相，加完后继续均质2min；继续保持5000rpm均质，趁热将C相加入混合样品，加完C相后保持均质5min。此后使用PE膜将烧杯封口后将样品室温静置过夜。次日加入D相，室温再次使用台式均质机以5000rpm均质3min使样品混合均匀，再用PE膜将烧杯封口，保留样品待用。
表1显示了实施例1-18中包含的表面活性剂种类及各原料的投料量。
表1
实施例1-18配置了9种含有不同表面活性剂的复合乳化体系，每种表面活性剂分别配制基料及含有尿素的实施例各一份。各样品配制量均为200g，配制工艺统一采用浓缩水相法，且与2％鲸蜡硬脂醇和6％白凡士林复配，含有尿素的实施例的尿素添加量均为5％。
实施例19-33：各种高分子增稠剂的水溶胶及含尿素相应样品的制备。
按表2所示在烧杯中称取适量去离子水，在室温下保持500rpm搅拌，缓缓将高分子粉末加入烧杯，待高分子浸润分散后提升搅拌速度至1000rpm并保持60min使高分子完全分散均匀。此后将B相所列原料加入烧杯，继续以1000rpm的速度搅拌30min使固体完全溶解分散均匀。
表2显示了实施例19-33中包含的高分子增稠剂种类及各原料的投料量。
表2
实施例19-33配置了5种含有不同高分子增稠剂的复合乳化体系，各高分子条件量依据其水溶胶粘度调节在0.4％或0.5％。每种高分子增稠剂分 别配制三份样品，分别为基料、含尿素样品及含尿素组合物样品。各样品配制量均为200g，含尿素样品中尿素添加量均为5％，含尿素组合物样品中添加了5％尿素、5％甘氨酸和0.5％柠檬酸三乙酯。
测试例1：实施例1-33的稳定性测试
测定新制实施例1-33样品的pH及粘度后，将各样品平分装入2个150ml透明PET瓶，盖紧旋盖后将样品分别置入25℃恒温箱和48℃恒温箱。定期将样品从恒温箱中取出，静置6h待其冷却至室温后测定样品的pH和粘度并观察样品性状，测定完毕后再将样品放回恒温箱。
表3显示了实施例1-33在各测试时间点的pH值和粘度。
表3
表3汇总了实施例1-33在各个测试时间点的pH值及粘度。其中，实施例1-18为9种不同的市售表面活性剂所制备的复配乳化体系，以及相应的添加尿素样品。其中，选取阳离子表面活性剂2个(TA-100，实施例1-2；ECON-100，实施例3-4)、阴离子表面活性剂1个(HR-S1，实施例5-6)、阴离子复配非离子表面活性剂1个(聚甘油五硬脂酸酯及硬脂酰乳酸钠，实施例7-8)、以及非离子表面活性剂5个。5个非离子表面活性剂可继续细分为：(1)单甘油酯类表面活性剂(甘油月桂酸酯，实施例9-10)；(2) 聚甘油酯类表面活性剂(单豆蔻酸聚甘油酯，实施例11-12)；(3)聚乙二醇类类表面活性剂(鲸蜡硬脂醇聚醚-30，实施例13-14)；(4)糖类表面活性剂(MSE-20，实施例15-16；阿拉通2121，实施例17-18)。
基于TA-100的复配乳化体系(实施例1)在室温放置一月后，样品pH值从4.99略微下降至4.96；样品粘度为4780mPa·s，相比新制样品3170mPa·s有所上升。在48℃放置1月后，样品pH值为4.79，相比初始值小幅下降，而粘度为2380mPa·s，相比新制样品小幅下降。复配5％尿素的样品(实施例2)在室温放置1月后，样品pH值自5.45上升至7.66，粘度从2180mPa·s大幅下降至680mPa·s。该样品在48℃放置1月后，其粘度明显上升。相比新制样品的粘度3570mPa·s，48℃放置1周、2周即1月的样品的粘度分别为11530mPa·s、11100mPa·s和9720mPa·s。与此同时，样品pH也从5.45上升至9.24。以上实验结果表明，TA-100复配体系可稳定承载尿素，此外实施例2在高温经时稳定性测试中，样品粘度明显提升。
基于阳离子调理剂ECON-100的复配乳化体系(实施例3)在室温放置一月后，样品pH值从3.89略微下降至3.86；因样品粘度过低，悬浮力不足而无法保持稳定，短时静置即出现分层现象。在48℃放置1月后，同样在各个时间点样品均出现分层现象，稳定性测试后样品pH值为3.67，相比初始值小幅下降。复配5％尿素的样品(实施例4)在室温放置1月后，样品pH值自4.06略微上升至4.16，样品同样在各时间点均出现分层现象。该样品在48℃放置1月后，pH从4.06大幅上升至7.58，在各个测试时间点亦出现分层。以上实验结果表明，阳离子调理剂ECON-100复配体系无法稳定承载尿素，两份样品在各测试条件下均出现分层问题。此外，尽管同为阳离子表面活性剂，复配尿素样品(实施例4)并未观察到类似于实施例2在高温经时测试中表现出的增粘特性。
基于月桂醇磷酸酯钾盐(HR-S1)的复配乳化体系(实施例5)在室温放置一月后，样品pH值从7.57小幅下降至7.45；样品粘度为725mPa·s，相比新制样品117mPa·s有所上升。在48℃放置1月后，样品pH值为7.72，相比初始值小幅上升，但样品在各个时间点均因为粘度过低而出现分层。 复配5％尿素的样品(实施例6)在室温放置1月后，样品pH值自7.43小幅上升至7.62，室温放置1周、2周及1月的样品的粘度分别为392mPa·s、1658mPa·s和2358mPa·s，相比初始值125mPa·s上升明显。该样品在48℃放置1月后，样品pH值从7.43大幅上升至8.93，同样各个测试均因粘度过低悬浮力不足而分层。以上实验结果表明，月桂醇磷酸酯钾盐(HR-S1)复配乳化体系仅能在室温下稳定承载尿素，在高温下则因悬浮力不足导致料体分层。
基于聚甘油五硬脂酸酯及硬脂酰乳酸钠的复配乳化体系(实施例7)在室温放置一月后，样品pH值从4.74小幅下降至4.33；样品粘度为18580mPa·s，相比新制样品4950mPa·s显著上升。在48℃放置1月后，样品pH值为4.46，相比初始值小幅下降，而粘度为14920mPa·s，相比新制样品同样小幅下降。复配5％尿素的样品(实施例8)在室温放置1月后，样品pH值自4.80上升至5.87，粘度从6250mPa·s显著上升至25250mPa·s。该样品在48℃放置1月后，其粘度亦明显上升。相比新制样品的粘度6250mPa·s，48℃放置1周、2周及1月的样品的粘度分别为35580mPa·s、23830mPa·s和28500mPa·s。与此同时，样品pH值也从4.80上升至8.08。以上实验结果表明，基于聚甘油五硬脂酸酯及硬脂酰乳酸钠复配体系可稳定承载尿素。
基于甘油月桂酸酯的复配乳化体系(实施例9)在室温放置一月后，样品pH值从4.77下降至4.07；但样品粘度过低悬浮力不足，无法保持稳定的乳化体系，短时静置即分层。在48℃放置1月后，同样因料体粘度过低而分层；稳定性测试后样品pH值为4.74，相比初始值基本相同。复配5％尿素样品(实施例10)在室温放置1月后，样品pH值自6.32小幅上升至7.21，室温放置1周、2周和1月的样品的粘度分别为992mPa·s、3680mPa·s和7830mPa·s，相比初始值上升明显(＜150mPa·s)。但该样品在48℃放置1月后，样品pH从6.32上升至7.37，在各个测试均因粘度过低悬浮力不足而出现分层，并且从放置2周开始破乳明显，在料体顶部形成油块。以上实验结果表明，基于甘油月桂酸酯的复配乳化体系仅能在室温中稳定承载尿素，且因为胶束重构料体粘度上升，但是在高温经时 稳定性测试中则因悬浮力不足而分层，并且胶束重构会导致表面活性剂乳化能力下降而破乳。
基于单豆蔻酸聚甘油酯的复配乳化体系(实施例11)在室温放置一月后，样品pH值从7.99略微下降至6.67；因样品粘度过低悬浮力不足无法保持稳定的乳化体系，短时静置即分层。在48℃放置1月后，料体仍因粘度过低而分层；稳定性测试后样品pH值为7.19，相比初始值有所下降。复配5％尿素的样品(实施例12)在室温放置1月后，样品pH值自8.16略微下降至7.98，在各时间点均分层。该样品在48℃放置1月后，样品pH从8.16上升至8.83，在各个测试时间点样品同样分层。以上实验结果表明，单豆蔻酸聚甘油酯复配乳化体系无法稳定承载尿素，两份样品在各测试条件下均出现分层问题。
基于鲸蜡硬脂醇聚醚-30的复配乳化体系(实施例13)在室温放置一月后，样品pH值从6.30小幅上升至6.45；样品粘度过低悬浮力不足，无法保持稳定的乳化体系，短时静置即分层。在48℃放置1月后，料体同样因粘度过低而分层；而pH值下降至4.13，相比初始值明显偏低。复配5％尿素的样品(实施例14)在室温放置1月后，pH值自7.52上升至8.14，且样品在各时间点均分层。该样品在48℃放置1月后，样品pH从7.52上升至9.06，且在各个测试时间点样品均分层。以上实验结果表明，鲸蜡硬脂醇聚醚-30复配体系无法稳定承载尿素，两份样品在各测试条件下均出现分层问题。
基于MSE-20的复配乳化体系(实施例15)在室温放置一月后，样品pH值从7.08小幅下降至6.67；样品粘度为167mPa·s，相比新制样品183mPa·s略微下降。在48℃放置1月后，样品pH值为3.86，相比初始值显著下降；放置1周、2周和1月样品粘度依次为1700mPa·s、2600mPa·s和15670mPa·s，相比新制样品显著上升。复配5％尿素的样品(实施例16)在室温放置1月后，pH值自7.13上升至7.93，粘度从167mPa·s略微下降至142mPa·s。该样品在48℃放置1月后，其粘度亦有所上升。相比新制样品的粘度167mPa·s，48℃放置1周、2周和1月的样品的粘度分别为1400mPa·s、2200mPa·s和1833mPa·s，但上升幅度相比未复配尿 素样品显著变小。与此同时，样品pH也从7.13上升至8.92。以上实验结果表明，基于MSE-20的复配体系可稳定承载尿素，然而尿素的复配显著影响了该表活在高温下的胶束重构，故复配尿素样品在高温经时稳定性测试中，料体粘度上升幅度显著低于未复配尿素样品。
基于阿拉通2121的复配乳化体系(实施例17)在室温放置一月后，样品pH值从7.01小幅下降至6.82；样品粘度为46330mPa·s，相比新制样品47500mPa·s略微下降。在48℃放置1月后，样品pH值为6.52，相比初始值有所下降；放置1周、2周和1月样品粘度依次为50170mPa·s、51000mPa·s和52500mPa·s，相比新制样品略微上升。复配5％尿素的样品(实施例18)在室温放置1月后，pH值自6.95上升至7.19，粘度从48750mPa·s略微下降至43170mPa·s。该样品在48℃放置1月后，其粘度呈明显下降趋势，相比新制样品的48750mPa·s，48℃放置1周、2周和1月的样品的粘度分别为44080mPa·s、32250mPa·s和23000mPa·s。与此同时，样品pH也从6.95上升至7.92。以上实验结果表明，基于阿拉通2121的复配体系可稳定承载尿素，然而复配尿素显著影响了该乳化体系的高温稳定性，在1月稳定性测试后样品粘度尚不足初始值的一半。
以上实验数据表明，在测试的9个乳化体系中，仅4个乳化体系可承载尿素，其中基于MSE-20和阿拉通2121的乳化体系已经显现出尿素的复配在高温下对相应乳化体系稳定性的较明显冲击。可见，对于大多数表面活性剂，承载尿素对其配方稳定性是很大的挑战。有必要指出，基于TA-100的复配乳化体系(实施例2)除具有良好的稳定性之外，复配尿素后还出现了未复配尿素样品(实施例1)所不具有的高温增粘性能，故下文将对该复配乳化体系的性质进行更为深入的研究。
除表面活性剂外，在化妆品中经常使用高分子增稠剂为配方提供粘度，继而提升配方稳定性。实施例19-33考察了五种不同市售高分子增稠剂水溶胶在复配尿素后的稳定性，所考察的高分子根据高分子链的结构可分为三类：(1)阳离子高分子增稠剂(PQ-37，实施例19-21)；(2)非离子高分子增稠剂(M25，实施例22-24；黄原胶，实施例25-27)；(3)阴离 子高分子增稠剂(聚丙烯酸钠，实施例28-30；AVC，实施例31-33)。每个高分子分别制备样品三份，其中一份未复配尿素，第二份复配5％尿素，第三份复配5％尿素、5％甘氨酸和0.5％柠檬酸三乙酯。
0.5％PQ-37水溶胶(实施例19)稳定性良好。样品在室温放置1月后，粘度自16430mPa·s小幅上升至18370mPa·s；而在48℃放置一个月后，粘度为15130mPa·s，相比新制样品16430mPa·s变化也不显著。将PQ-37复配5％尿素后(实施例20)，样品稳定性显著变差，实施例20在室温放置1月后，pH值从4.43上升至7.84，而粘度自18030mPa·s下降至5280mPa·s；而48℃仅放置一周后，随pH值上升至8.88，粘度大幅下降至183mPa·s。将PQ-37复配5％尿素、5％甘氨酸和0.5％柠檬酸三乙酯后(实施例21)，样品稳定性亦明显变差，实施例21在室温放置1月后，pH值从5.23小幅上升至5.77，而粘度却从13230mPa·s下降至5430mPa·s；而在48℃放置一周后，pH小幅上升至5.70，粘度却大幅下降至333mPa·s。以上实验结果表明，PQ-37水溶胶无法稳定承载尿素。且实施例21的结果表明，尿素分解导致的pH值的上升，并非导致料体失粘的唯一原因。
0.4％M25水溶胶(实施例22)稳定性较好。样品在室温放置1月后，粘度自15420mPa·s小幅上升至18270mPa·s；而在48℃放置一个月后，粘度为8270mPa·s，相比新制样品15420mPa·s有所下降。将M25复配5％尿素后(实施例23)样品稳定性变差，实施例20在室温放置1月后，pH值从7.13上升至7.48，而粘度自16080mPa·s下降至15220mPa·s；而48℃放置一月后，随pH上升至8.90，粘度大幅下降至2230mPa·s。将PQ-37复配5％尿素、5％甘氨酸和0.5％柠檬酸三乙酯后(实施例24)，样品稳定性同样变差，实施例24在室温放置1月后，pH值从6.76小幅下降至6.62，而粘度却从15830mPa·s下降至8700mPa·s；而在48℃放置一月后，pH下降至6.31，粘度却大幅下降至1170mPa·s。以上实验结果表明，M25水溶胶无法稳定承载尿素。
0.5％黄原胶水溶胶(实施例25)稳定性良好。样品在室温放置1月后，粘度自1242mPa·s小幅上升至1317mPa·s；而在48℃放置一个月后，粘度为970mPa·s，相比新制样品小幅下降。将黄原胶复配5％尿素后(实施 例26)，样品仍保持良好的稳定性，实施例20在室温放置1月后，pH值从7.04上升至7.38，而粘度自1383mPa·s略微上升至1425mPa·s；而在48℃放置一月后，样品pH值上升至8.65，粘度下降至867mPa·s。将PQ-37复配5％尿素、5％甘氨酸和0.5％柠檬酸三乙酯后(实施例27)，样品稳定性亦无明显变化，实施例21在室温放置1月后，pH值从5.55小幅上升至7.21，而粘度从1442mPa·s小幅上升至1575mPa·s；而在48℃放置一月后，pH值小幅上升至6.04，而样品粘度小幅下降至1270mPa·s。以上实验结果表明，黄原胶水溶胶可稳定承载尿素及其组合物。
0.4％聚丙烯酸钠水溶胶(实施例28)稳定性良好。样品在室温放置1月后，粘度自2667mPa·s小幅上升至2625mPa·s；而在48℃放置一个月后，粘度为2845mPa·s，相比新制样变化不大。将聚丙烯酸钠复配5％尿素后(实施例29)样品稳定性显著变差，实施例29在室温放置1月后，pH值从6.89上升至7.26，而粘度自3392mPa·s下降至833mPa·s；而48℃仅放置一周后，随值pH上升至7.99，粘度大幅下降至142mPa·s。将聚丙烯酸钠复配5％尿素、5％甘氨酸和0.5％柠檬酸三乙酯后(实施例30)，样品稳定性亦明显变差。实施例30在室温放置1月后，pH值从6.51小幅下降至6.32，而粘度却从2000mPa·s大幅下降至358mPa·s；而在48℃放置一周后，pH值下降至5.80，同时样品粘度大幅下降至117mPa·s。以上实验结果表明，聚丙烯酸钠水溶胶无法稳定承载尿素及尿素组合物。
0.4％AVC水溶胶(实施例31)稳定性良好。样品在室温放置1月后，粘度自5250mPa·s小幅上升至7400mPa·s；而在48℃放置一个月后，粘度为13570mPa·s，相比新制样品有显著提升，其原因可能为高温促进其胶束结构的重新排布。将AVC复配5％尿素后(实施例32)样品稳定性显著变差，实施例32在室温放置1月后，pH值从6.46上升至7.64，而粘度自6092mPa·s下降至608mPa·s；而48℃仅放置一周后，随值pH上升至8.61，粘度大幅下降至142mPa·s。将AVC复配5％尿素、5％甘氨酸和0.5％柠檬酸三乙酯后(实施例33)，样品稳定性亦明显变差。实施例21在室温放置1月后，pH值从5.64小幅上升至5.73，而粘度却从3180mPa·s下降至508mPa·s；而在48℃放置一周后，pH值小幅上升至5.73，样品粘度却 大幅下降至117mPa·s。以上实验结果表明，AVC水溶胶无法稳定承载尿素及其组合物。
以上实验结果表明，受试的五种高分子增稠剂中有四种无法稳定承载尿素。而仅有可承载尿素的黄原胶在化妆品实际应用中亦存在诸多局限，譬如增稠效率较低无法配制较高粘度的剂型，肤感粘腻影响产品使用感。此外需要指出，在稳定性测试中粘度明显下降的四种高分子，在复配尿素+甘氨酸+柠檬酸三乙酯的组合物后，尽管pH值基本保持稳定，但仍然在稳定性测试中出现显著降粘的现象，表明尿素分解的导致pH值上升并非是样品失粘的唯一原因。尿素分解产物的强离子性同样对配方稳定性提出了很高的要求。而大多数高分子增稠剂依靠相同电荷间的排斥力形成凝胶结构，离子性的增强可削弱双电层，导致增稠剂分子间的电荷斥力降低而失粘，故在复配尿素后仍具有良好稳定性的高分子增稠剂的选择空间极其有限。
可见，大多数表面活性剂和高分子增稠剂不具备稳定承载尿素的能力，因而极大限制了具有强护肤功效的尿素在化妆品中的实际应用。而且，在考察上海家化联合股份有限公司的12种在售乳液配方后发现(粘度在1000mPa·s至20000mPa·s，每种配方使用乳化剂不同)，有且仅有与实施例1-2使用相同乳化剂的阳离子配方在复配尿素后可满足国家法规对化妆品稳定性的要求。其余11种基于阴离子类、糖类、聚乙二醇类、聚甘油酯类的表面活性剂并复配各类高分子增稠剂的配方，均出现了显著降粘、分层甚至破乳的稳定性问题。可见，基于TA-100的阳离子乳化配方在与尿素复配后表现出良好的稳定性以及有趣的高温增粘特性，下文将对TA-100与尿素复配进行更深入的探究。
实施例34-53：含有不同油脂种类及油脂量的复配乳化体系及相应含尿素样品的制备。
按表4所示在三个烧杯中称取适量A相、B相及C相，分别于90℃水浴锅中加热30min。之后使用台式均质机以5000rpm均质A相2min使之分散均匀；此后保持5000rpm均质并趁热加入B相，加完后保持均质2min；继续保持5000rpm均质，趁热将C相加入混合样品，加完C相后保持均质 5min。此后使用PE膜将烧杯封口后将样品室温静置过夜。次日加入D相，室温再次使用台式均质机以5000rpm均质3min使样品混合均匀，再用PE膜将烧杯封口，保留样品待用。
表4显示了实施例34-53中包含的油脂种类及各原料的投料量。
表4
实施例34-53的乳化体系与实施例1-2相同，固定为5％TA-100复配2％鲸蜡硬脂醇。各样品配制量均为200g，样品配制工艺亦采用了与实施例1-2一致的浓缩水相法。在此基础上，考察了油脂种类及油脂添加量对样品性质的影响。其中，实施例34-43固定油脂添加量为6％，使用多种不同类型油脂配制样品；而实施例44-53则固定油脂为白凡士林，以考察油脂添加量对样品性质的影响。每种样品均分别配制基料及含有尿素的实施例各一份，含有尿素的实施例中，尿素添加量均为5％。
测试例2：实施例34-53的稳定性测试
测定新制实施例34-53样品的pH及粘度后，将各样品平分装入2个150ml透明PET瓶，盖紧旋盖后将样品分别置入25℃恒温箱和48℃恒温箱。定期将样品从恒温箱中取出，静置6h待其冷却至室温后测定样品的pH和粘度并观察样品性状，测定完毕后再将样品放回恒温箱。
表5显示了实施例34-53在各测试时间点的pH值和粘度(列入实施例1和实施例2作为对比)。
表5
表5汇总了实施例34-53在各个测试时间点的pH值及粘度，并列入了实施例1-2的相应数据作为对比。其中，实施例1-2和实施例34-41考察了5种不同油脂对复配乳化体系性质的影响，这五种油脂包括：(1)非极性固态油脂(白凡士林，实施例1-2)；(2)非极性液态油脂(10#白油，实施例34-35)；(3)极性液态油脂(棕榈酸异辛酯，实施例36-37)；(4)极性固态油脂(十六酸十六酯ACP，实施例38-39)；(5)硅油(二甲基硅油(100cst)，实施例40-41)。此外，实施例42-43将以上油脂复配使用。
乳化10#白油的样品(实施例34)在室温放置1月后，其pH值为4.94，相比初始值4.93几乎没有变化；样品粘度为5700mPa·s，相比新制样品5450mPa·s略微上升。在48℃放置1月后，样品pH值自4.93下降至4.64，而粘度为4200mPa·s，相比新制样品小幅下降。复配5％尿素的样品(实施例35)室温放置1月后，pH值自5.47上升至7.80，粘度从8130mPa·s下降至5570mPa·s。该样品在48℃放置1月后，其粘度有所上升。相比新制样品的粘度1092mPa·s，48℃放置1周、2周及1月的样品的粘度分别为9500mPa·s、8840mPa·s和8450mPa·s。与此同时，样品pH值也从5.47上升至9.21。以上实验结果表明，TA-100复配体系乳化10#白油后 可稳定承载尿素，并且在高温经时稳定性测试中，样品粘度呈上升趋势。
乳化棕榈酸异辛酯的样品(实施例36)在室温放置1月后，其pH值为4.24，相比初始值4.09小幅上升；样品粘度为7930mPa·s，相比新制样品6170mPa·s有所上升。在48℃放置1月后，样品pH值为4.09，与初始值一致，而粘度为4930mPa·s，相比新制样品小幅下降。复配5％尿素的样品(实施例37)在室温放置1月后，pH值自4.30上升至6.79，粘度从3570mPa·s大幅下降至1100mPa·s。该样品在48℃放置1月后，其粘度明显上升。相比新制样品的粘度3570mPa·s，48℃放置1周、2周及1月的样品的粘度分别为5000mPa·s、9630mPa·s和8280mPa·s。与此同时，样品pH值也从4.30上升至9.16。以上实验结果表明，TA-100复配体系乳化棕榈酸异辛酯后可稳定承载尿素，并且在高温经时稳定性测试中，样品粘度呈上升趋势。
乳化十六酸十六酯ACP的样品(实施例38)在室温放置1月后，其pH值为4.59，相比初始值4.47略微上升；样品粘度为7480mPa·s，相比新制样品6100mPa·s小幅上升。在48℃放置1月后，样品pH值为4.46，相比新制样品几乎没有变化，而粘度为6300mPa·s，相比新制样品略微上升。复配5％尿素的样品(实施例39)在室温放置1月后，pH值自4.87上升至7.40，粘度从3570mPa·s上升至4570mPa·s。该样品在48℃放置1月后，其粘度明显上升。相比新制样品的粘度3570mPa·s，48℃放置1周、2周及1月的样品的粘度分别为12380mPa·s、17330mPa·s和15330mPa·s。与此同时，样品pH值也从4.87上升至8.98。以上实验结果表明，TA-100复配体系乳化十六酸十六酯ACP后可稳定承载尿素，并且在高温经时稳定性测试中，样品粘度呈明显上升趋势。
乳化二甲基硅油(100cst)的样品(实施例40)在室温放置1月后，其pH值为5.04，相比初始值5.08略微下降；样品粘度为9630mPa·s，相比新制样品3250mPa·s明显上升。在48℃放置1月后，样品pH值亦为5.04，而粘度为11230mPa·s，相比新制样品同样粘度明显上升。复配5％尿素的样品(实施例41)在室温放置1月后，样品pH值自5.55上升至7.70，粘度从4820mPa·s下降至2330mPa·s。该样品在48℃放置1月后，其及 1月的样品的粘度分别为8380mPa·s、16650mPa·s和17000mPa·s。与此同时，样品pH值也从5.55上升至9.21。以上实验结果表明，TA-100复配体系乳化二甲基硅油(100cst)后可稳定承载尿素，并且在高温经时稳定性测试中，样品粘度呈明显上升趋势。
乳化多种油脂的样品(实施例42)在室温放置1月后，其pH从值6.10小幅下降至5.86，而粘度为1280mPa·s，相比新制样品858mPa·s小幅上升。在48℃放置1月后，样品pH值自6.10下降至5.46，而粘度为880mPa·s，相比新制样品并无明显变化。复配5％尿素的样品(实施例43)在室温放置1月后，pH值自6.21上升至7.98，而粘度也从858mPa·s小幅上升至1380mPa·s。该样品在48℃放置1月后，其粘度显著上升。相比新制样品的粘度1092mPa·s，48℃放置1周、2周及1月的样品的粘度分别为5025mPa·s、20170mPa·s和11530mPa·s。与此同时，样品pH值也从6.21上升至9.02。以上实验结果表明，TA-100复配体系乳化复合油脂后仍可稳定承载尿素，并且在高温经时稳定性测试中，样品粘度同样呈显著上升趋势。
综合上述实验结果可归纳出以下结论：尽管因油脂性质不同，实施例34-43样品的性质略有差异。但总体而言，所有样品均表现出以下与实施例1-2一致的共性：所有实施例均可稳定承载尿素，并且复配尿素后在高温经时稳定性测试中样品的粘度上升。表明TA-100复配乳化体系复配尿素后，具有广泛的油脂选择空间，有利于本发明所报道的技术在化妆品中的实际应用。
实施例44-53固定油脂为白凡士林，考察了油脂添加量对TA-100复配乳化体系性质的影响。实施例44-45、实施例46-47、实施例48-49、实施例1-2、实施例50-51和实施例52-53的油脂添加量依次为0％、1％、3％、6％、10％和20％。
未复配油脂样品(实施例44)在室温放置1月后，其pH值为4.97，相比初始值5.29小幅下降；样品粘度为2150mPa·s，相比新制样品1700mPa·s小幅上升。在48℃放置1月后，样品pH值为4.88，而粘度为1280 mPa·s，相比新制样品粘度有所下降。复配5％尿素的样品(实施例45)在室温放置1月后，pH值自5.27上升至7.14，粘度从1270mPa·s下降至258mPa·s。该样品在48℃放置1月后，其粘度显著上升。相比新制样品的粘度1270mPa·s，48℃放置1周、2周及1月的样品的粘度分别为4250mPa·s、14500mPa·s和14750mPa·s。与此同时，样品pH值也从5.27上升至9.24。以上实验结果表明，TA-100复配乳化体系在未复配油脂的情况下即具有良好的尿素承载性，且相关样品性质相较实施例1-2无明显差异。
复配1％白凡士林样品(实施例46)在室温放置1月后，其pH值为5.01，相比初始值5.25小幅下降；样品粘度为1980mPa·s，相比新制样品1720mPa·s小幅上升。在48℃放置1月后，样品pH值为4.84，而粘度为1330mPa·s，相比新制样品粘度有所下降。复配5％尿素的样品(实施例47)在室温放置1月后，pH值自5.75上升至7.27，粘度从1320mPa·s下降至300mPa·s。该样品在48℃放置1月后，其粘度显著上升。相比新制样品的粘度1320mPa·s，48℃放置1周、2周及1月的样品的粘度分别为3450mPa·s、13670mPa·s和14830mPa·s。与此同时，样品pH也从5.75上升至9.23。以上实验结果表明，TA-100复配乳化体系在复配1％白凡士林时具有良好的尿素承载性，且相关样品性质相较实施例1-2无明显差异。
复配3％白凡士林样品(实施例48)在室温放置1月后，其pH值为4.97，相比初始值5.29小幅下降；样品粘度为2120mPa·s，相比新制样品1900mPa·s小幅上升。在48℃放置1月后，样品pH值为4.88，而粘度为1330mPa·s，相比新制样品粘度有所下降。复配5％尿素的样品(实施例49)在室温放置1月后，pH值自5.76上升至7.41，粘度从1530mPa·s下降至333mPa·s。该样品在48℃放置1月后，其粘度显著上升。相比新制样品的粘度1530mPa·s，48℃放置1周、2周及1月的样品的粘度分别为5800mPa·s、16080mPa·s和1650mPa·s。与此同时，样品pH值也从5.76上升至9.26。以上实验结果表明，TA-100复配乳化体系在复配3％白凡士林时具有良好的尿素承载性，且相关样品性质相较实施例1-2无明显 差异。
复配10％白凡士林样品(实施例50)在室温放置1月后，其pH值为5.09，相比初始值5.29小幅下降；样品粘度为2670mPa·s，相比新制样品2200mPa·s小幅上升。在48℃放置1月后，样品pH值为5.20，而粘度为1620mPa·s，相比新制样品粘度有所下降。复配5％尿素的样品(实施例51)在室温放置1月后，样品pH值自5.78上升至7.43，粘度从1770mPa·s下降至392mPa·s。该样品在48℃放置1月后，其粘度显著上升。相比新制样品的粘度1770mPa·s，48℃放置1周、2周及1月的样品的粘度分别为8680mPa·s、18750mPa·s和21500mPa·s。与此同时，样品pH值也从5.78上升至9.28。以上实验结果表明，TA-100复配乳化体系在复配10％白凡士林时具有良好的尿素承载性，且相关样品性质相较实施例1-2无明显差异。
复配20％白凡士林的样品(实施例52)在室温放置1月后，其pH值为5.00，相比初始值5.40有所下降；样品粘度为10630mPa·s，相比新制样品7020mPa·s小幅上升。48℃放置1月后，样品pH值为4.95，而粘度为4820mPa·s，相比新制样品粘度有所下降。复配5％尿素的样品(实施例53)在室温放置1月后，pH值自5.76上升至7.55，粘度从2380mPa·s下降至800mPa·s。该样品在48℃放置1月后，其粘度显著上升。相比新制样品的粘度2380mPa·s，48℃放置1周、2周及1月的样品的粘度分别为14230mPa·s、18170mPa·s和19500mPa·s。与此同时，样品pH值也从5.76上升至9.23。以上实验结果表明，TA-100复配乳化体系在复配20％白凡士林时具有良好的尿素承载性，且相关样品性质相较实施例1-2无明显差异。
综合实施例44-53的实验结果，我们发现随白凡士林复配量的上升，TA-100复配乳化体系的粘度逐渐上升。在白凡士林复配量在0-20％的范围内，TA-100复配乳化体系均可稳定承载尿素，且样品性质相比实施例1-2基本一致。实施例34-53的实验结果证明，TA-100复配乳化体系在上述所有测试条件下均具有良好的尿素承载力，具备广泛油脂添加量和复配种类的调整空间，有利于本发明所报道的技术在化妆品工业中的实际应用。
实施例54-62：不同尿素添加量及尿素组合物或衍生物的TA-100复配乳化体系样品的制备。
按表6所示在三个烧杯中称取适量A相、B相及C相，分别于90℃水浴锅中加热30min。之后使用台式均质机以5000rpm均质A相2min使之分散均匀；此后保持5000rpm均质并趁热加入B相，加完后保持均质2min；继续保持5000rpm均质，趁热将C相加入混合样品，加完C相后保持均质5min。此后使用PE膜将烧杯封口后将样品于室温静置过夜。次日加入D相，室温再次使用台式均质机以5000rpm均质3min使样品混合均匀，再用PE膜将烧杯封口，保留样品待用。
表6显示了实施例54-62的各原料的投料量。
表6
实施例54-62的乳化体系与实施例1-2相同，固定为5％TA-100复配2％H-MY。各样品配制量均为200g，样品配制工艺亦采用了与实施例1-2一致的浓缩水相法。其中，实施例54-61均复配6％白凡士林，在此基础上，考察了尿素添加量、尿素衍生物及尿素组合物对样品性质的影响。实施例62乳化了5种油脂(油脂配比同实施例42)，并复配尿素组合物。
测试例3：实施例54-62的稳定性测试
测定新制实施例54-62样品的pH及粘度后，将各样品平分装入2个150ml透明PET瓶，盖紧旋盖后将样品分别置入25℃恒温箱和48℃恒温箱。定期将样品从恒温箱中取出，静置6h待其冷却至室温后测定样品的pH和粘度并观察样品性状，测定完毕后再将样品放回恒温箱。
表7显示了实施例54-62在各测试时间点的pH值和粘度(列入实施例1-2和实施例42-43作为对比)。
表7
表7汇总了实施例54-62在各个测试时间点的pH值及粘度，并列入了实施例1-2和实施例42-43的数据作为对比。其中，实施例1-2和实施例54-59考察了8种不同尿素添加量对复配乳化体系性质的影响，根据尿素添加量的顺序依次为：0％(实施例1)、0.1％(实施例54)、0.2％(实施例55)、0.5％(实施例56)、1％(实施例57)、2％(实施例58)、5％(实施例2)和10％(实施例59)。实施例60和实施例61和上述实施例基质相同，但分别复配了尿素组合物(5％尿素+5％甘氨酸+0.5％柠檬酸三乙酯)和尿素衍生物(5％羟乙基脲)。实施例62复配了多种油脂(所乳化油脂同实施例42)，并复配尿素组合物，以模拟接近化妆品实际配方的复杂体系。
复配0.1％尿素的样品(实施例54)在室温放置1月后，其pH值从4.92 略微上升至6.19，样品粘度为2730mPa·s，相比新制样品1750mPa·s小幅上升。在48℃放置1月后，样品pH值自4.92上升至7.98。48℃放置1周、2周及1月的样品的粘度分别为1020mPa·s、850mPa·s和608mPa·s，相比新制样品的1750mPa·s呈逐步下降趋势。
复配0.2％尿素的样品(实施例55)在室温放置1月后，其pH值从5.09略微上升至5.20，样品粘度为2630mPa·s，相比新制样品1780mPa·s有所上升。在48℃放置1月后，样品pH值自5.09上升至8.50。48℃放置1周、2周及1月的样品的粘度分别为780mPa·s、580mPa·s和408mPa·s，相比新制样品的1750mPa·s呈逐步下降趋势。
复配0.5％尿素的样品(实施例56)在室温放置1月后，其pH值从5.04上升至5.66，样品粘度为2170mPa·s，相比新制样品1950mPa·s略微上升。在48℃放置1月后，样品pH值自5.04上升至8.82。48℃放置1周、2周和1月的样品的粘度分别为530mPa·s、750mPa·s和2142mPa·s，相比新制样品的1950mPa·s呈先下降后上升的趋势。
复配1％尿素的样品(实施例57)在室温放置1月后，其pH值从5.09上升至6.20，样品粘度为1620mPa·s，相比新制样品1900mPa·s小幅下降。在48℃放置1月后，样品pH值自5.09上升至8.97。48℃放置1周、2周和1月的样品的粘度分别为520mPa·s、1050mPa·s和10830mPa·s，相比新制样品的1900mPa·s呈先下降后大幅上升的趋势。
复配2％尿素的样品(实施例58)在室温放置1月后，其pH值从5.13上升至6.71，样品粘度为1030mPa·s，相比新制样品1180mPa·s小幅下降。在48℃放置1月后，样品pH值自5.13上升至9.08。48℃放置1周、2周和1月的样品的粘度分别为1270mPa·s、6920mPa·s和16250mPa·s，相比新制样品的1180mPa·s呈逐步上升的趋势。
复配10％尿素的样品(实施例59)在室温放置1月后，其pH值从5.64上升至7.62，样品粘度为600mPa·s，相比新制样品1780mPa·s明显下降。在48℃放置1月后，样品pH值自5.64上升至9.15。48℃放置1周、2周和1月的样品的粘度分别为15630mPa·s、10050mPa·s和11750mPa·s，相比新制样品的1780mPa·s上升明显且基本保持稳定。
复配尿素组合物的样品(实施例60)在室温放置1月后，其pH值从5.59略微下降至5.58，样品粘度为500mPa·s，相比新制样品820mPa·s有所下降。在48℃放置1月后，样品pH值自5.59小幅上升至5.89。48℃放置1周、2周和1月的样品的粘度分别为4330mPa·s、8200mPa·s和13580mPa·s，相比新制样品的820mPa·s呈逐步上升趋势。
复配5％羟乙基脲的样品(实施例61)在室温放置1月后，其pH值从8.42略微下降至8.16，样品粘度为6820mPa·s，相比新制样品8330mPa·s小幅下降。在48℃放置1月后，样品pH值自8.42小幅上升至8.92。48℃放置1周、2周和1月的样品的粘度分别为8200mPa·s、10000mPa·s和8120mPa·s，相比新制样品的8330mPa·s有小幅上升。
复配多种油脂及尿素组合物的样品(实施例62)在室温放置1月后，其pH值从6.76小幅下降至6.19，样品粘度为620mPa·s，相比新制样品458mPa·s小幅上升。在48℃放置1月后，样品pH值自6.76下降至5.93。48℃放置1周、2周和1月的样品的粘度分别为5025mPa·s、20170mPa·s和11530mPa·s，相比新制样品的458mPa·s上升显著。
上述实验结果可归纳出下列结论：
(1)TA-100复配乳化体系可以承载不同添加量的尿素、尿素衍生物和尿素组合物，所有样品均未出现分层和破乳问题。
(2)低尿素复配量的样品(0.1％-0.2％，实施例54-55)在高温经时强化测试中粘度呈下降趋势；较低尿素复配量的样品(0.5％-1％，实施例56-57)在高温经时强化测试中粘度先上升后下降；较高尿素复配量的样品(2％-10％，实施例2和实施例58-59)在高温经时强化测试中粘度呈上升趋势。该现象可能来源于尿素分解所产生的水溶性阴离子小分子促进了TA-100胶束的重构。在尿素量较低、分解产物较少的条件下，主要表现为破坏既有胶束结构使料体降粘；但在尿素量较高、分解产物较多的情况下，则促进了新的聚合度更大的胶束的生成，使料体的粘度显著上升。以上实验结果表明TA-100复配乳化体系，在复配较高含量尿素时更易显现其独特性质，在添加功效量尿素的配方中的具有的实用价值。
(3)实施例60和实施例61在实施例1的基础上复配了尿素组合物和 尿素衍生物，以上两实施例均可稳定承载尿素，且性质与其它复配尿素样品相似。需要指出，这两份样品的pH值并未显著上升，表明尿素促进TA-100胶束重构的现象并非仅在强碱性条件下发生。本发明报道的TA-100复配乳化体系可以在满足国家化妆品法规对样品pH监管标准的前提下，展现其独特的性质。
(4)实施例62在实施例60的基础上，复配了多种油脂，该样品在稳定性测试中的表现与后者基本一致。对接近化妆品实际配方的复杂体系，本发明所报道的乳化体系仍具有良好的承载性并表现出独特的增粘性能，表明该复配乳化体系具有广泛的油脂和添加剂放入调整空间，有利于其在化妆品中的应用。
实施例63-88：调节TA-100添加量及长链脂肪醇添加种类和添加量的的TA-100复合乳化体系样品，及相应含尿素样品的制备。
按表8所示在三个烧杯中称取适量A相、B相及C相，分别于90℃水浴锅中加热30min。之后使用台式均质机以5000rpm均质A相2min使之分散均匀；此后保持5000rpm均质并趁热加入B相，加完后继续均质2min；继续保持5000rpm均质，趁热将C相加入混合样品，加完C相后保持均质5min。此后使用PE膜将烧杯封口后将样品室温静置过夜。次日加入D相，室温再次使用台式均质机以5000rpm均质3min使样品混合均匀，再用PE膜将烧杯封口，保留样品待用。
表8显示了实施例63-88中添加的长链脂肪醇的种类及各原料的投料量。
表8
实施例63-88固定工艺为浓缩水相法，油脂添加量为6％白凡士林，各样品配制量均为200g。其中，实施例63-78固定TA-100的添加量为5％，在此基础上，考察了长链脂肪醇添加量及添加种类对料体性质的影响。实施例79-88固定长链脂肪醇为2％H-MY，考察了TA-100添加量对料体性质的影响。每种样品均分别配制基料及含有尿素的实施例各一份，其中含有尿素的实施例的尿素添加量均为5％。
测试例4：实施例63-88的稳定性测试
测定新制实施例63-88样品的pH及粘度后，将各样品平分装入2个150ml透明PET瓶，盖紧旋盖后将样品分别置入25℃恒温箱和48℃恒温箱。定期将样品从恒温箱中取出，静置6h待其冷却至室温后测定样品的pH和粘度并观察样品性状，测定完毕后再将样品放回恒温箱。
表9显示了实施例63-88在各测试时间点的pH值和粘度(列入实施例 1-2)。
表9
表9汇总了实施例63-88在各个测试时间点的pH值及粘度，并列入了实施例1-2的数据作为对比。其中，实施例1-2和实施例63-74考察了7种不同H-MY添加量的影响，根据H-MY添加量的顺序依次为：0％(实施例63-64)、0.5％(实施例65-66、1％(实施例67-68)、2％(实施例1-2)、 3％(实施例69-70)、4％(实施例71-72)和5％(实施例73-74)。实施例75-76和实施例77-78分别复配了2％二十二醇和2％十六醇。
未复配长链脂肪醇的样品(实施例63)在室温放置1月后，其pH值为6.06，相比初始值5.61小幅上升；样品粘度为1042mPa·s，相比新制样品620mPa·s有所上升。48℃放置1月后，样品pH值为5.35，相比初始值小幅下降，而粘度为617mPa·s，与新制样品基本一致。复配5％尿素的样品(实施例64)在室温放置1月后，pH值自5.90上升至7.38，粘度从1030mPa·s小幅下降至783mPa·s。该样品在48℃放置1月后，其粘度明显下降。相比新制样品的粘度1030mPa·s，48℃放置1周、2周和1月的样品的粘度分别为280mPa·s、280mPa·s和280mPa·s。与此同时，样品pH也从5.90上升至8.98。有必要指出，以上样品均出现固块，源于乳化体系稳定性不足，继而导致油脂析出并聚集成块。以上实验结果表明，未复配长链脂肪醇的TA-100乳化体系无法稳定乳化油脂，且同样没有观察到在复配尿素后在高温经时稳定性测试中粘度显著上升的现象，以上实验结果可证明长链脂肪醇在复配乳化体系中起到了关键的作用。
鲸蜡硬脂醇(H-MY)复配量为0.5％的样品(实施例65)在室温放置1月后，其pH值为5.68，相比初始值5.31小幅上升；样品粘度为400mPa·s，相比新制样品380mPa·s略微上升。48℃放置1月后，样品pH值为4.97，相比初始值小幅下降，而粘度为725mPa·s，相比新制样品有所上升。复配5％尿素的样品(实施例66)在室温放置1月后，pH值自5.62上升至7.41，粘度从420mPa·s小幅下降至250mPa·s。该样品在48℃放置1月后，其粘度有所下降。相比新制样品的粘度420mPa·s，48℃放置1周、2周和1月的样品的粘度分别为270mPa·s、280mPa·s和208mPa·s。与此同时，样品pH也从5.62上升至9.00。以上实验结果表明，复配0.5％鲸蜡硬脂醇的TA-100乳化体系可承载尿素，但未观察到在复配尿素后在高温经时稳定性测试中粘度显著上升的现象。可见低长链脂肪醇复配样品的性质相比实施例2有较明显的差异。
鲸蜡硬脂醇(H-MY)复配量为1％的样品(实施例67)在室温放置1月后，其pH值为5.49，相比初始值5.31小幅上升；样品粘度为358mPa·s， 相比新制样品430mPa·s略微下降。48℃放置1月后，样品pH值为4.81，相比初始值有所下降，而粘度为575mPa·s，相比新制样品小幅上升。复配5％尿素的样品(实施例68)在室温放置1月后，pH值自5.65上升至7.46，粘度从670mPa·s下降至267mPa·s。该样品在48℃放置1月后，其粘度呈明显上升趋势。相比新制样品的粘度670mPa·s，48℃放置1周、2周和1月的样品的粘度分别为2880mPa·s、5330mPa·s和7920mPa·s。与此同时，样品pH也从5.65上升至9.00。以上实验结果表明，复配1％鲸蜡硬脂醇的TA-100乳化体系可承载尿素，且其性质相比实施例2基本一致。
鲸蜡硬脂醇(H-MY)复配量为3％的样品(实施例69)在室温放置1月后，其pH值为5.62，相比初始值5.32小幅上升；样品粘度为9630mPa·s，相比新制样品7780mPa·s小幅上升。48℃放置1月后，样品pH值为4.79，相比初始值有所下降，而粘度为8450mPa·s，相比新制样品略微上升。复配5％尿素的样品(实施例70)在室温放置1月后，pH值自5.76上升至7.63，粘度从36420mPa·s小幅下降至31580mPa·s。该样品在48℃放置1月后，其粘度呈小幅下降趋势。相比新制样品的粘度36420mPa·s，48℃放置1周、2周和1月的样品的粘度分别为23580mPa·s、23000mPa·s和21670mPa·s。与此同时，样品pH也从5.76上升至9.06。以上实验结果表明，复配3％鲸蜡硬脂醇的TA-100乳化体系可承载尿素，与实施例2不同的是，在复配尿素后样品即时粘度出现明显上升，且含尿素样品在高温经时测试中粘度略有下降，表明较高添加量的鲸蜡硬脂醇可使TA-100复配乳化体系显现出独特的性质。
鲸蜡硬脂醇(H-MY)复配量为4％的样品(实施例71)在室温放置1月后，其pH值为5.62，相比初始值5.16小幅上升；样品粘度为32580mPa·s，相比新制样品36830mPa·s略微下降。48℃放置1月后，样品pH值为5.79，相比初始值有所上升，而粘度为35330mPa·s，相比新制样品略微下降。复配5％尿素的样品(实施例72)在室温放置1月后，pH值自5.79上升至7.83，粘度为53420mPa·s与新制样品一致。该样品在48℃放置1月后，其粘度呈小幅上升趋势。相比新制样品的粘度53420mPa·s，48℃放置1周、2周和1月的样品的粘度分别为48420mPa·s、59920mPa·s和 65170mPa·s。与此同时，样品pH也从5.79上升至8.94。以上实验结果表明，复配4％鲸蜡硬脂醇的TA-100乳化体系可承载尿素，且含尿素样品在高温经时稳定性测试中呈小幅上升趋势。与实施例2不同的是，在复配尿素后样品即时粘度出现明显上升。
鲸蜡硬脂醇(H-MY)复配量为5％的样品(实施例73)在室温放置1月后，其pH值为5.57，相比初始值5.05小幅上升；样品粘度为32580mPa·s，相比新制样品45250mPa·s有所下降。48℃放置1月后，样品pH值为5.90，相比初始值有所上升，而粘度为35000mPa·s，相比新制样品有所下降。5％尿素的样品(实施例74)在室温放置1月后，pH值自5.79上升至7.99，粘度从为53420mPa·s上升至66250mPa·s。该样品在48℃放置1月后，其粘度呈上升趋势。相比新制样品的粘度53420mPa·s，48℃放置1周、2周和1月的样品的粘度分别为48420mPa·s、61630mPa·s和73080mPa·s。与此同时，样品pH也从5.79上升至8.96。以上实验结果表明，复配5％鲸蜡硬脂醇的TA-100乳化体系可承载尿素，且与实施例2一致，含尿素样品在高温经时稳定性测试中呈上升趋势。
复配2％山嵛醇(即二十二醇)的样品(实施例75)在室温放置1月后，其pH值为5.28，相比初始值4.88小幅上升；样品粘度为8250mPa·s，相比新制样品13580mPa·s有所下降。48℃放置1月后，样品pH值为5.12，相比初始值有所上升，而粘度为10500mPa·s，相比新制样品小幅下降。复配5％尿素的样品后(实施例76)在室温放置1月后，pH值自5.54上升至7.67，粘度从为14170mPa·s下降至7500mPa·s。该样品在48℃放置1月后，其粘度呈上升趋势。相比新制样品的粘度14170mPa·s，48℃放置1周、2周和1月的样品的粘度分别为15670mPa·s、26080mPa·s和27250mPa·s。与此同时，样品pH也从5.54上升至9.06。以上实验结果表明，复配2％山嵛醇的TA-100乳化体系可承载尿素，含尿素样品在高温经时稳定性测试中呈上升趋势。然相应样品的初始粘度相比实施例1和实施例2更高，表明山嵛醇的更长碳链有助于配方粘度的形成。
复配2％鲸蜡醇的样品(实施例77)在室温放置1月后，其pH值为5.68，相比初始值5.42小幅上升；样品粘度为2325mPa·s，相比新制样品 1700mPa·s有所上升。48℃放置1月后，样品pH值为6.70，相比初始值有所上升，而粘度为750mPa·s，相比新制样品明显下降。复配5％尿素的样品(实施例78)在室温放置1月后，pH值自5.92上升至7.27，粘度从2920mPa·s上升至5258mPa·s。该样品在48℃放置1月后，其粘度呈上升趋势。相比新制样品的2920mPa·s，48℃放置1周、2周和1月的样品的粘度分别为10880mPa·s、16170mPa·s和15670mPa·s。与此同时，样品pH也从5.92上升至9.26。以上实验结果表明，复配2％鲸蜡醇的TA-100乳化体系可承载尿素，且相关样品性质基本与实施例1-2一致。
以上实验结果标明，TA-100在复配合适种类及添加量的长链脂肪醇后，所制备的样品可稳定承载尿素。但是，随着脂肪醇复配量和种类不同，在实验中发现以下特性：
(1)未复配长链脂肪醇的样品乳化体系稳定星较差，在稳定性测试中因破乳导致油相聚集而产生油块。
(2)复配低含量的长链脂肪醇样品(0.5％，实施例65-67)在复配尿素后，在高温经时稳定性测试中未出现粘度显著上升趋势。
(3)复配高含量的长链脂肪醇样品(＞3％，实施例69-74)在复配尿素后，即时粘度即明显上升。
(4)复配山嵛醇的样品(实施例76-77)对比复配相同含量的鲸蜡硬脂醇和鲸蜡醇的样品，前者粘度偏高明显。
以上实验表明，TA-100复配乳化体系在长链脂肪醇的种类和复配量的选择上具有广阔的空间。可通过调节长链脂肪醇的添加种类和添加量对料体粘度进行调节，以适应不同机型的化妆品配方粘度的要求，有利于本发明在化妆品工业中的实际应用。此外，在长链脂肪醇复配量较高时，添加尿素后的样品粘度即出现显著上升，表明本发明报道的复配乳化体系在膏霜或高粘乳液中的应用中更具优势。
实施例1-2和实施例79-88考察了6种不同TA-100添加量的影响，根据TA-100添加量的顺序依次为：0％(实施例79-80)、0.5％(实施例81-82)、2.5％(实施例83-84)、5％(实施例1-2)、7.5％(实施例85-86)和10％ (实施例87-88)。
未添加TA-100的样品(实施例79)在室温放置一月后，pH值从4.88略微下降至4.62；此外，因为配方乳化能力和悬浮力过低，各个测试时间点均发现料体分层及破乳。48℃放置1月后，样品在各个时间点同样分层和破乳，稳定性测试后样品pH值为4.57，相比初始值小幅下降。复配5％尿素的样品(实施例80)在室温放置1月后，pH值自6.13上升至8.29，且样品在各时间点均出现分层和破乳现象。该样品在48℃放置1月后，样品pH从上升至9.17，同样在各个测试时间点样品均分层及破乳。以上实验结果表明，未复配TA-100的样品不具有乳化和支撑料体的能力，亦不能稳定承载尿素，证明了TA-100在复配乳化体系中的核心作用。
TA-100复配量为0.5％的的复配乳化体系(实施例81)在室温放置一月后，样品pH值从5.38略微下降至4.87；样品在各个时间点均分层。48℃放置1月后，样品在各个时间点仍因粘度过低而分层，稳定性测试后样品pH值为4.85，相比初始值小幅下降。复配5％尿素的样品(实施例82)在室温放置1月后，pH值自6.18上升至8.23，样品仍在各时间点均出现分层。然而实施例82在48℃高温经时测试中却表现出了独特的性质，48℃放置1周、2周和1月的样品的粘度分别为1350mPa·s、4458mPa·s和18250mPa·s，相比初始值出现了显著上升的趋势。以上实验结果表明，TA-100复配量为0.5％的复配乳化体系，即显现出在高温经时测试中粘度显著上升的现象。该发现意味着，可以使用较低浓度的TA-100与其它表面活性剂复配，即可能提升后者的尿素承载力，使原本无法稳定承载尿素的配方能够满足国家法规对化妆品稳定性的监管要求，在化妆品工业的实际应用中具有很高的价值。
TA-100复配量为2.5％的样品(实施例83)在室温放置1月后，其pH为4.97，相比初始值5.60有所下降；样品粘度为383mPa·s，相比新制样品370mPa·s略微上升。48℃放置1月后，样品pH值为4.85，相比初始值有所下降，而粘度为542mPa·s，相比新制样品有所上升。复配5％尿素的样品(实施例84)在室温放置1月后，pH值自6.13上升至8.17，粘度从420mPa·s略微下降至383mPa·s。该样品在48℃放置1月后，其粘度 呈显著上升趋势。相比新制样品的粘度420mPa·s，48℃放置1周、2周和1月的样品的粘度分别为24200mPa·s、23500mPa·s和63920mPa·s。与此同时，样品pH也从6.13上升至9.24。以上实验结果表明，TA-100添加量为2.5％的复配乳化体系可承载尿素，且相关样品性质与实施例1-2基本一致。
TA-100复配量为7.5％的样品(实施例85)在室温放置1月后，其pH为4.89，相比初始值5.23小幅下降；样品粘度为28170mPa·s，相比新制样品27000mPa·s略微上升。48℃放置1月后，样品pH值为4.79，相比初始值小幅下降，而粘度为23670mPa·s，相比新制样品亦小幅下降。复配5％尿素的样品(实施例86)在室温放置1月后，pH值自6.15上升至7.67，粘度从41420mPa·s下降至25500mPa·s。该样品在48℃放置1月后，其粘度呈先下降再上升的趋势。相比新制样品的粘度41420mPa·s，48℃放置1周、2周和1月的样品的粘度分别为12930mPa·s、25670mPa·s和55300mPa·s。与此同时，样品pH也从6.15上升至9.14。以上实验结果表明，TA-100添加量为7.5％的复配乳化体系可承载尿素，且相关样品性质与实施例1-2基本一致。
TA-100复配量为10％的样品(实施例87)在室温放置1月后，其pH为4.97，相比初始值5.08略微下降；样品粘度为30420mPa·s，相比新制样品29080mPa·s略微上升。在48℃放置1月后，样品pH值为4.90，相比初始值小幅下降，而粘度为28330mPa·s，相比新制样品略微下降。复配5％尿素的样品(实施例88)在室温放置1月后，pH值自5.58上升至7.47，粘度从49180mPa·s下降至23920mPa·s。该样品在48℃放置1月后，其粘度呈先下降再上升的趋势。相比新制样品的粘度49180mPa·s，48℃放置1周、2周和1月的样品的粘度分别为16270mPa·s、45500mPa·s和85700mPa·s。与此同时，样品pH也从5.58上升至9.24。以上实验结果表明，TA-100添加量为10％的复配乳化体系可承载尿素，且相关样品性质与实施例1-2基本一致。
以上实验结果表明，固定长链脂肪醇的用量和种类后，在较宽的TA-100复配范围内，所制备的复配乳化体系均可稳定承载尿素。但是，根 据TA-100复配量不同，在实验中发现以下特性：
(1)未复配TA-100的样品(实施例79-80)不具备油脂乳化能力和结构支撑能力，在所有测试条件下均出现分层和破乳的问题。且并未显现复配尿素后在高温经时测试中增粘的现象，证明了TA-100在复配体系中的关键作用。
(2)复配低含量TA-100(0.5％，实施例81)的样品，本身因悬浮力不足而分层；但复配尿素后(实施例82)，在高温经时稳定性测试中料体粘度显著提升，证明较低TA-100添加量的样品在复配尿素后即具有高温增粘的特性。该发现解释了一条全新的配方设计思路，将少量TA-100与其它乳化体系的复配使用，有助于提升后者的尿素承载力，使之满足国家法对化妆品稳定性的要求。
(3)复配高含量TA-100(＞5％，实施例85-88)的样品，复配尿素后即时粘度即明显上升，在高温经时稳定性测试中粘度先下降再上升，其原因可能为前文所提到的尿素分解产物促进了TA-100的胶束重构。
综上所述，本发明所报道的复配乳化体系，在较宽的TA-100复配量的范围内，均具有稳定承载尿素的能力。可通过调整TA-100的添加量改变料体的粘度，有利于本发明所报道的技术应用于各类的化妆品剂型之中。
以下是复合体系在皮肤外用剂中的具体应用的实施例，及其这些剂型的配方和制备方法。以下各表中“-”表示无添加。
应用例1：面霜的制备
应用例2：乳液的制备
应用例3：精华液的制备
应用例4：面膜的制备
应用例5：眼霜的制备
应用例6：喷雾的制备
Claims (10)
- 一种承载尿素或其衍生物的稳定组合物，所述组合物包含：(a)油脂；(b)阳离子乳化剂，所述阳离子乳化剂是二硬脂基二甲基氯化铵；(c)长链脂肪醇，所述长链脂肪醇的碳链长度为16-22；(d)水相；其中，所述尿素衍生物是尿素的碳原子数为1-6的羟烷基化物，其中，所述阳离子乳化剂与长链脂肪醇的重量比为10:1至1:4，所述阳离子乳化剂与承载的尿素或其衍生物的重量比为1:10至50:1。
- 如权利要求1所述的组合物，其中，所述油脂选自：非极性固态油脂；非极性液态油脂；极性液态油脂；极性固态油脂；硅油；或它们的混合物。
- 如权利要求1所述的组合物，其中，所述组合物包含0.1-20重量％的油脂。
- 如权利要求1所述的组合物，其中，所述组合物包含2.5-10重量％的阳离子表面活性剂。
- 如权利要求1所述的组合物，其中，所述长链脂肪醇选自：十六醇、鲸蜡硬脂醇、十八醇、二十醇、二十二醇或它们的混合物。
- 如权利要求1所述的组合物，其中，所述组合物包含0.1-10重量％的长链脂肪醇。
- 如权利要求1所述的组合物，其中，所述组合物包含1重量％以上的尿素或其衍生物。
- 如权利要求1所述的组合物，其中，所述组合物包含50重量％以上的水相。
- 如权利要求1-8中任一项所述的组合物，其中，所述阳离子乳化剂与长链脂肪醇的重量比为10:1至1:2，所述阳离子乳化剂与承载的尿素或其衍生物的重量比为1:2至10:1。
- 一种皮肤外用剂，其包含如权利要求1-9中任一项所述的组合物。
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| EP1889602A2 (de) * | 2006-07-24 | 2008-02-20 | Beiersdorf AG | Kosmetische Zubereitungen zur Restrukturierung von Haaren mit besonderen Harnstoffderivaten |
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| CN113648232A (zh) * | 2021-08-19 | 2021-11-16 | 上海家化联合股份有限公司 | 承载尿素或其衍生物的稳定组合物 |
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| CN1778287A (zh) * | 2003-11-26 | 2006-05-31 | 国家淀粉及化学投资控股公司 | 使用羟烷基脲提高增湿功效 |
| JP2005330243A (ja) * | 2004-05-21 | 2005-12-02 | Shiseido Co Ltd | Ｗ／ｏ型エマルジョン製剤 |
| JP2005330242A (ja) * | 2004-05-21 | 2005-12-02 | Shiseido Co Ltd | Ｗ／ｏ型エマルジョン製剤 |
| EP1889602A2 (de) * | 2006-07-24 | 2008-02-20 | Beiersdorf AG | Kosmetische Zubereitungen zur Restrukturierung von Haaren mit besonderen Harnstoffderivaten |
| CN101674800A (zh) * | 2007-05-30 | 2010-03-17 | 荷兰联合利华有限公司 | 具有增强的芳香剂递送的个人护理组合物 |
| CN113648232A (zh) * | 2021-08-19 | 2021-11-16 | 上海家化联合股份有限公司 | 承载尿素或其衍生物的稳定组合物 |
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