CN108802231A - Method that is a kind of while measuring 19 kinds of sun-screening agents in cosmetics - Google Patents
Method that is a kind of while measuring 19 kinds of sun-screening agents in cosmetics Download PDFInfo
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- CN108802231A CN108802231A CN201810685610.8A CN201810685610A CN108802231A CN 108802231 A CN108802231 A CN 108802231A CN 201810685610 A CN201810685610 A CN 201810685610A CN 108802231 A CN108802231 A CN 108802231A
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- cosmetics
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- 239000000516 sunscreening agent Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000002537 cosmetic Substances 0.000 title claims abstract description 32
- 239000012086 standard solution Substances 0.000 claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 239000012085 test solution Substances 0.000 claims abstract description 20
- 238000001514 detection method Methods 0.000 claims abstract description 16
- 239000012452 mother liquor Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000011002 quantification Methods 0.000 claims abstract description 5
- 230000004044 response Effects 0.000 claims abstract description 5
- 230000014759 maintenance of location Effects 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 129
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 66
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 48
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 24
- 235000019253 formic acid Nutrition 0.000 claims description 24
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 19
- -1 Diethylhexyl butamido Chemical group 0.000 claims description 15
- ALYNCZNDIQEVRV-UHFFFAOYSA-N 4-aminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1 ALYNCZNDIQEVRV-UHFFFAOYSA-N 0.000 claims description 14
- 229960000655 ensulizole Drugs 0.000 claims description 14
- UVCJGUGAGLDPAA-UHFFFAOYSA-N ensulizole Chemical compound N1C2=CC(S(=O)(=O)O)=CC=C2N=C1C1=CC=CC=C1 UVCJGUGAGLDPAA-UHFFFAOYSA-N 0.000 claims description 14
- KJCLYACXIWMFCC-UHFFFAOYSA-M sodium;5-benzoyl-4-hydroxy-2-methoxybenzenesulfonate Chemical compound [Na+].C1=C(S([O-])(=O)=O)C(OC)=CC(O)=C1C(=O)C1=CC=CC=C1 KJCLYACXIWMFCC-UHFFFAOYSA-M 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 9
- WSSJONWNBBTCMG-UHFFFAOYSA-N 2-hydroxybenzoic acid (3,3,5-trimethylcyclohexyl) ester Chemical compound C1C(C)(C)CC(C)CC1OC(=O)C1=CC=CC=C1O WSSJONWNBBTCMG-UHFFFAOYSA-N 0.000 claims description 8
- 125000006181 4-methyl benzyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1C([H])([H])[H])C([H])([H])* 0.000 claims description 7
- 241000723346 Cinnamomum camphora Species 0.000 claims description 7
- 229940111759 benzophenone-2 Drugs 0.000 claims description 7
- WXNRYSGJLQFHBR-UHFFFAOYSA-N bis(2,4-dihydroxyphenyl)methanone Chemical compound OC1=CC(O)=CC=C1C(=O)C1=CC=C(O)C=C1O WXNRYSGJLQFHBR-UHFFFAOYSA-N 0.000 claims description 7
- 238000010790 dilution Methods 0.000 claims description 7
- 239000012895 dilution Substances 0.000 claims description 7
- 229960004881 homosalate Drugs 0.000 claims description 7
- FMRHJJZUHUTGKE-UHFFFAOYSA-N Ethylhexyl salicylate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1O FMRHJJZUHUTGKE-UHFFFAOYSA-N 0.000 claims description 6
- 229930008380 camphor Natural products 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims description 5
- KKJKXQYVUVWWJP-JLHYYAGUSA-N 4-[(e)-(4,7,7-trimethyl-3-oxo-2-bicyclo[2.2.1]heptanylidene)methyl]benzenesulfonic acid Chemical compound CC1(C)C2CCC1(C)C(=O)\C2=C\C1=CC=C(S(O)(=O)=O)C=C1 KKJKXQYVUVWWJP-JLHYYAGUSA-N 0.000 claims description 5
- YBGZDTIWKVFICR-JLHYYAGUSA-N Octyl 4-methoxycinnamic acid Chemical compound CCCCC(CC)COC(=O)\C=C\C1=CC=C(OC)C=C1 YBGZDTIWKVFICR-JLHYYAGUSA-N 0.000 claims description 5
- 229960004050 aminobenzoic acid Drugs 0.000 claims description 5
- 229960000846 camphor Drugs 0.000 claims description 5
- 239000006071 cream Substances 0.000 claims description 5
- 229940068171 ethyl hexyl salicylate Drugs 0.000 claims description 5
- 229960001679 octinoxate Drugs 0.000 claims description 5
- DXGLGDHPHMLXJC-UHFFFAOYSA-N oxybenzone Chemical compound OC1=CC(OC)=CC=C1C(=O)C1=CC=CC=C1 DXGLGDHPHMLXJC-UHFFFAOYSA-N 0.000 claims description 5
- 229960001173 oxybenzone Drugs 0.000 claims description 5
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 claims description 4
- JGUMTYWKIBJSTN-UHFFFAOYSA-N 2-ethylhexyl 4-[[4,6-bis[4-(2-ethylhexoxycarbonyl)anilino]-1,3,5-triazin-2-yl]amino]benzoate Chemical compound C1=CC(C(=O)OCC(CC)CCCC)=CC=C1NC1=NC(NC=2C=CC(=CC=2)C(=O)OCC(CC)CCCC)=NC(NC=2C=CC(=CC=2)C(=O)OCC(CC)CCCC)=N1 JGUMTYWKIBJSTN-UHFFFAOYSA-N 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000005374 membrane filtration Methods 0.000 claims description 4
- FMJSMJQBSVNSBF-UHFFFAOYSA-N octocrylene Chemical compound C=1C=CC=CC=1C(=C(C#N)C(=O)OCC(CC)CCCC)C1=CC=CC=C1 FMJSMJQBSVNSBF-UHFFFAOYSA-N 0.000 claims description 4
- 229960000601 octocrylene Drugs 0.000 claims description 4
- 235000012459 muffins Nutrition 0.000 claims description 3
- QMNWYGTWTXOQTP-UHFFFAOYSA-N 1h-triazin-6-one Chemical compound O=C1C=CN=NN1 QMNWYGTWTXOQTP-UHFFFAOYSA-N 0.000 claims description 2
- UUGLJVMIFJNVFH-UHFFFAOYSA-N Hexyl benzoate Chemical compound CCCCCCOC(=O)C1=CC=CC=C1 UUGLJVMIFJNVFH-UHFFFAOYSA-N 0.000 claims 2
- 150000002240 furans Chemical class 0.000 claims 2
- JFHCDEYLWGVZMX-CMDGGOBGSA-N Isoamyl cinnamate Chemical compound CC(C)CCOC(=O)\C=C\C1=CC=CC=C1 JFHCDEYLWGVZMX-CMDGGOBGSA-N 0.000 claims 1
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 claims 1
- 125000002252 acyl group Chemical group 0.000 claims 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- JBIASUUIWKZOJM-UHFFFAOYSA-N n-ethyl-n-phenoxyethanamine Chemical compound CCN(CC)OC1=CC=CC=C1 JBIASUUIWKZOJM-UHFFFAOYSA-N 0.000 claims 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 8
- 150000002148 esters Chemical class 0.000 description 7
- KGNFCMBVSSCAGC-UHFFFAOYSA-N C(=O)OC(C1=CC=CC=C1)=O.C(C)N(OC1=CC=CC=C1)CC Chemical compound C(=O)OC(C1=CC=CC=C1)=O.C(C)N(OC1=CC=CC=C1)CC KGNFCMBVSSCAGC-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- TYYHDKOVFSVWON-UHFFFAOYSA-N 2-butyl-2-methoxy-1,3-diphenylpropane-1,3-dione Chemical compound C=1C=CC=CC=1C(=O)C(OC)(CCCC)C(=O)C1=CC=CC=C1 TYYHDKOVFSVWON-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000003556 assay Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 229960005193 avobenzone Drugs 0.000 description 3
- 239000012964 benzotriazole Substances 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- ASLNDVUAZOHADR-UHFFFAOYSA-N 2-butyl-3-methylphenol Chemical compound CCCCC1=C(C)C=CC=C1O ASLNDVUAZOHADR-UHFFFAOYSA-N 0.000 description 2
- WXESYIUTJXKGCE-UHFFFAOYSA-N C(CCCC)(=O)OCCC(C)C.COC(C(=O)O)=CC1=CC=CC=C1 Chemical compound C(CCCC)(=O)OCCC(C)C.COC(C(=O)O)=CC1=CC=CC=C1 WXESYIUTJXKGCE-UHFFFAOYSA-N 0.000 description 2
- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000004696 Poly ether ether ketone Substances 0.000 description 2
- 206010042496 Sunburn Diseases 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 2
- 239000012965 benzophenone Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 208000014674 injury Diseases 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 229920002530 polyetherether ketone Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- MIOPJNTWMNEORI-GMSGAONNSA-N (S)-camphorsulfonic acid Chemical compound C1C[C@@]2(CS(O)(=O)=O)C(=O)C[C@@H]1C2(C)C MIOPJNTWMNEORI-GMSGAONNSA-N 0.000 description 1
- NCIAZCLIFWUDPR-UHFFFAOYSA-N 2-butyl-3,4,5,6-tetramethylphenol Chemical compound CCCCC1=C(C)C(C)=C(C)C(C)=C1O NCIAZCLIFWUDPR-UHFFFAOYSA-N 0.000 description 1
- HIPQTCQUXOFTFI-UHFFFAOYSA-N 2-methoxy-1,3-diphenylpropane-1,3-dione Chemical class C=1C=CC=CC=1C(=O)C(OC)C(=O)C1=CC=CC=C1 HIPQTCQUXOFTFI-UHFFFAOYSA-N 0.000 description 1
- ZDHRAACDPXUCHC-UHFFFAOYSA-N 3,4-diethyl-2-hexoxyphenol;5-methoxy-4-phenyltriazine Chemical compound COC1=CN=NN=C1C1=CC=CC=C1.CCCCCCOC1=C(O)C=CC(CC)=C1CC ZDHRAACDPXUCHC-UHFFFAOYSA-N 0.000 description 1
- ANJLMAHUPYCFQY-UHFFFAOYSA-N 4-phenyl-1h-benzimidazole-2-sulfonic acid Chemical class C=12NC(S(=O)(=O)O)=NC2=CC=CC=1C1=CC=CC=C1 ANJLMAHUPYCFQY-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 201000009030 Carcinoma Diseases 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 206010015150 Erythema Diseases 0.000 description 1
- 238000010268 HPLC based assay Methods 0.000 description 1
- 102000011782 Keratins Human genes 0.000 description 1
- 108010076876 Keratins Proteins 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 208000002193 Pain Diseases 0.000 description 1
- 206010057249 Phagocytosis Diseases 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- UBNYRXMKIIGMKK-RMKNXTFCSA-N amiloxate Chemical compound COC1=CC=C(\C=C\C(=O)OCCC(C)C)C=C1 UBNYRXMKIIGMKK-RMKNXTFCSA-N 0.000 description 1
- 150000003851 azoles Chemical class 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- FQUNFJULCYSSOP-UHFFFAOYSA-N bisoctrizole Chemical compound N1=C2C=CC=CC2=NN1C1=CC(C(C)(C)CC(C)(C)C)=CC(CC=2C(=C(C=C(C=2)C(C)(C)CC(C)(C)C)N2N=C3C=CC=CC3=N2)O)=C1O FQUNFJULCYSSOP-UHFFFAOYSA-N 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 231100000321 erythema Toxicity 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- CLJDBQVBSMXSTP-UHFFFAOYSA-N octan-3-yl 2-hydroxybenzoate Chemical class CCCCCC(CC)OC(=O)C1=CC=CC=C1O CLJDBQVBSMXSTP-UHFFFAOYSA-N 0.000 description 1
- 238000001543 one-way ANOVA Methods 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000008782 phagocytosis Effects 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 238000000611 regression analysis Methods 0.000 description 1
- 238000004366 reverse phase liquid chromatography Methods 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000012109 statistical procedure Methods 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 230000000475 sunscreen effect Effects 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Cosmetics (AREA)
Abstract
The present invention relates to analysis and detection technique fields, and in particular to a kind of while method that measures 19 kinds of sun-screening agents in cosmetics.This method includes：Single mark mother liquor；Mixed standard solution preparation；Serial mixed standard solution preparation；The preparation of test solution and liquid chromatogram measuring.The response of serial mixed standard solution and test solution should all be detected in instrument within the scope of line style, qualitative according to peak retention time, according to peak area quantification.Advantage of the present invention：Sample treatment is simple, effective；Realize in C18 chromatographic columns 19 kinds of sun-screening agents of separation detection simultaneously；The easy environmental protection of method, accuracy are high；Reproducibility and good tolerance.
Description
Technical field
The present invention relates to analysis and detection technique fields, and in particular to a kind of while measuring in cosmetics 19 kinds of sun-screening agents
Method.
Background technology
Industrial pollution causes atmospheric ozone layer to be seriously damaged so that the amount of ultraviolet that ground is injected in sunlight constantly increases
Add, excessive ultraviolet radiation can cause major injury to human skin.Ultraviolet B radiation UVB (280~320nm) makes skin exist
Sunburn, turn to red because of sun burn in short time；Long wave ultraviolet UVA (320~400nm) penetration capacity is stronger, can go deep into corium with undertissue,
Collagen is destroyed, accelerates melanin to be formed, cutaneum carcinoma can be caused when serious.
Sun-screening agent can protect the skin from the injury of ultraviolet light, be often added in cosmetics and sun care preparations is made,
Sun-screening agent can be divided into physical sunscreen agent and chemical sun.Physical sunscreen agent be by reflection or scattering process stop ultraviolet light from
And reach sun-proof purpose, mainly there are titanium dioxide and zinc oxide；Chemical sun is also known as ultra-violet absorber, and the mechanism of action is
One of ultraviolet light phagocytosis barrier is formed by other film forming substances in skin surface to be absorbed, this process is happened at skin
Inside, and removed by body metabolism.This kind of chemical sun has skin certain irritation, easily causes various skins not
Suitable symptom, such as skin is made to generate erythema, make skin keratin aging and various burning pain senses.
It is newly executed from 31 days December in 2016《Cosmetics safety technical specification》The makeup of (version in 2015) clear stipulaties
The use type and limit of mutatis mutandis sun-screening agent in product.According to《Specification》Regulation, the chemical sun that can be used in limitation range
There are 25 kinds, but only 19 kinds of sun-screening agents list detection method, and respectively 5 groups different HPLC methods, including limits the use of component
The measurement of 15 kinds of components such as Phenylbenzimidazolesulfonic acid, the own ester of diethylamino oxybenzene formylbenzoate, Diethylhexyl butamido
3 kinds of base triazinone, benzylidene camphor sulfonic acid components measure respectively, and disabling component benzophenone -2 detection method, when check fee
Arduously, operability is not good enough.Through experimental study,《Specification》The assay method of 15 kinds of ingredients such as middle Phenylbenzimidazolesulfonic acid is in reality
There are certain limitations in the inspection work of border, not only have to many polyether-ether-ketones of reversed-phase liquid chromatography instrument (PEEK) component materials
Corrosivity, the repeatability of retention time can also decline when high-volume is run, while having to experimenter and injuring and to environment
There is pollution.
Invention content
The purpose of the present invention is overcoming the deficiencies of existing technologies, a kind of easy method is provided, environmental protection, accuracy height, is reappeared
Property and good tolerance and the method that 19 kinds of sun-screening agents in cosmetics can be measured simultaneously.
To achieve the above object, the technical solution adopted by the present invention is：
Method that is a kind of while measuring 19 kinds of sun-screening agents in cosmetics, described 19 kinds of sun-screening agents are：To methoxycinnamate
Isoamyl valerate, Uvinul T 150, double-ethylhexylphenol anisyl triazine, Diethylhexyl Butamido Triazon,
Benzophenone-3, benzophenone -5, benzophenone -2, PABA ethylhexyls, benzylidene camphor sulfonic acid, diethylamino oxybenzene formylbenzoate
Own ester, p-aminobenzoic acid, Phenylbenzimidazolesulfonic acid, 4- methyl benzyl subunits camphor, butylmethoxydibenzoylmethane,
Octocrilene, ethylhexyl methoxy cinnamate, ethylhexyl salicylate, Homosalate and di-2-ethylhexylphosphine oxide-benzotriazole base four
Methyl butyl phenol；
The method includes：
Single mark mother liquor：Precision is weighed after Phenylbenzimidazolesulfonic acid is completely dissolved with 1mol/L sodium hydroxide solutions and is used
Tetrahydrofuran constant volume；Precision, which weighs, uses tetrahydrofuran constant volume after benzophenone -5 is completely dissolved with methanol；Precision weighs remaining respectively
17 kinds of sun-screening agent standard substances, with the tetrahydrofuran dissolving containing 20% methanol and constant volume；
Mixed standard solution preparation：Precision pipettes each single mark mother liquor and is configured to mix with methanol dilution and constant volume in volumetric flask
Standardization solution；
Serial mixed standard solution preparation：Dilute the serial mixed standard solution of preparation step by step with methanol；
The preparation of test solution：Precision weighs cosmetic sample 0.25g, is placed in 25ml volumetric flasks, be added methanol and
Tetrahydrofuran mixed liquor 20mL is ultrasonically treated 30min, takes out and stands to room temperature, shakes up, constant volume, filters；Filtrate 1.0ml is taken, is used
Methanol dilution is to 10.0ml, and mixing, 0.45 μm of membrane filtration is as test solution；
Test sample measures：Serial mixed standard solution and test solution are subjected to liquid chromatogram measuring respectively.Series is mixed
The response of standardization solution and test solution should all be detected in instrument within the scope of line style, root qualitative according to peak retention time
According to peak area quantification.
Further, the configuration concentration of single mark mother liquor is 1mg/mL.
Further, the chromatographic condition of test sample measurement is：
Chromatographic column：C18 columns；Column temperature：35℃；Mobile phase：A is isopropanol:Methanol solution=1 containing 0.1% formic acid:4v/
V, B are 0.05% aqueous formic acid；Flow velocity：1.2mL/min；Sample size：10μL；Detection wavelength：300nm/350nm；
Gradient elution program：0~5min, mobile phase A 75%, Mobile phase B 25%；5~6min, mobile phase A 75~85%,
Mobile phase B 15~25%；6~10min, mobile phase A 85%, Mobile phase B 15%；10~15min, mobile phase A 85~90%, stream
Dynamic phase B10~15%；15~17min, mobile phase A 90%, Mobile phase B 10%；17~35min, mobile phase A 100%, mobile phase
B0%.
Preferably, chromatographic column is Phenomenex Luna C18,4.6mm × 250mm, 5 μm.
Further, cosmetics include cream kind, oily class and muffin class.
Further, when test solution is prepared, methanol and tetrahydrofuran mixed liquor are methanol:Tetrahydrofuran=1:4v/
v。
Further, precision weighs to be accurate to 0.0001g.
Further, methanol, isopropanol, tetrahydrofuran, formic acid and sodium hydroxide are chromatographically pure, wherein formic acid, diformazan
Base sulfoxide purity >=99%.
Further, formic acid purity >=99%.
In 19 kinds of sun-screening agents, in addition to Phenylbenzimidazolesulfonic acid and benzophenone -5, tetrahydrofuran is dissolved in, therefore with four
Hydrogen furans directly prepares remaining 17 kinds of sun-screening agent list mark mother liquor.And solubility of the Phenylbenzimidazolesulfonic acid in first alcohol and water is equal
It is poor, a small amount of sodium hydroxide solution can be used and make it completely dissolved, then with tetrahydrofuran constant volume.Benzophenone -5 is first added when dissolving
A small amount of methanol after making it completely dissolved, reuses tetrahydrofuran constant volume.
Methanol is 8 with tetrahydrofuran volume ratio:When 2, the sun-screening agent rate of recovery is above 97%.Therefore first is used in this research
Alcohol is 8 with tetrahydrofuran volume ratio:2 are used as sample extraction solvent.
The present invention by method in, using 0.05% formic acid as acid modification agent, 20% isopropanol of strong eluant, eluent
Methanol solution (contain 0.1% formic acid), gradient elution detaches 19 kinds of sun-screening agents, 19 kinds of component energy good separations.
Benzophenone -2, the own ester of diethylamino oxybenzene formylbenzoate and butyl methoxy dibenzoyl base in 19 kinds of sun-screening agents
Methane has maximal ultraviolet absorption peak at 350nm, has maximal ultraviolet absorption peak at 300nm in 16 type sun-screening agents.Therefore
The chromatogram that 19 kinds of sun-screening agents are carried out using two channels 300nm and 350nm is measured.
Compared with prior art, provided by the invention while the advantages of measure the method for 19 kinds of sun-screening agents in cosmetics：
(1) sample treatment is simple, effective.
(2) methanol/isopropanol/water gradient elution system, double UV check is used to realize in C18 chromatographic columns simultaneously
19 kinds of sun-screening agents of separation detection.
(3) it not only avoids and makees mobile phase using the contour corrosive solvent of tetrahydrofuran and perchloric acid, and by 5 prescriptions
Method is optimized for one group of HPLC assay method, and the easy environmental protection of method, accuracy are high.
(4) reproducibility and good tolerance can be used for 19 kinds of sun-screening agents in cosmetics while measuring.
Description of the drawings
Fig. 1 is Phenomenon Luna C18300nm absorbs sun-screening agent chromatogram.
Fig. 2 is Phenomenon Luna C18350nm absorbs sun-screening agent chromatogram.
In figure, corresponding peak number is：1. p-aminobenzoic acid, 2. Phenylbenzimidazolesulfonic acids, 3. benzophenone -5,4. benzals
Camphorsulfonic acid, 5. benzophenone-3,6.PABA ethylhexyls, 7. pairs of methoxy dibenzoylmethanes, 8.4- methyl benzyl subunit camphor trees
Brain, 9. Octocrilenes, 10. ethylhexyl methoxy cinnamates, 11. Homosalate isomers, 12. ethylhexyl salicylates, 13.
Homosalate, the own oxygen butyrylamino triazinone of 14. diethyl, 15. Uvinul T 150s, 16. di-2-ethylhexylphosphine oxides-benzotriazole base
Tetramethyl butyl phenol, 17. bis-ethylhexoxyphenol methoxyphenyl triazine, 18 benzophenone -2,19. diethylamino hydroxyl Benzoylbenzenes
Hexyl formate, 20. butylmethoxydibenzoylmethanes.
Specific implementation mode
To make those skilled in the art more fully understand technical scheme of the present invention, work of the following embodiment to the present invention
It is described in further detail, following embodiment is merely to illustrate invention, but is not limited to the scope of the present invention.
Method that is a kind of while measuring 19 kinds of sun-screening agents in cosmetics, described 19 kinds of sun-screening agents are：To methoxycinnamate
Isoamyl valerate, Uvinul T 150, double-ethylhexylphenol anisyl triazine, Diethylhexyl Butamido Triazon,
Benzophenone-3, benzophenone -5, benzophenone -2, PABA ethylhexyls, benzylidene camphor sulfonic acid, diethylamino oxybenzene formylbenzoate
Own ester, p-aminobenzoic acid, Phenylbenzimidazolesulfonic acid, 4- methyl benzyl subunits camphor, butylmethoxydibenzoylmethane,
Octocrilene, ethylhexyl methoxy cinnamate, ethylhexyl salicylate, Homosalate and di-2-ethylhexylphosphine oxide-benzotriazole base four
Methyl butyl phenol；
The method includes：
Single mark mother liquor：Precision is weighed after Phenylbenzimidazolesulfonic acid is completely dissolved with 1mol/L sodium hydroxide solutions and is used
Tetrahydrofuran constant volume；Precision, which weighs, uses tetrahydrofuran constant volume after benzophenone -5 is completely dissolved with methanol；Precision weighs remaining respectively
17 kinds of sun-screening agent standard substances, with the tetrahydrofuran dissolving containing 20% methanol and constant volume；The configuration concentration of single mark mother liquor is 1mg/
mL。
Mixed standard solution preparation：Precision pipettes each single mark mother liquor and is configured to mix with methanol dilution and constant volume in volumetric flask
Standardization solution；
Serial mixed standard solution preparation：Dilute the serial mixed standard solution of preparation step by step with methanol；
The preparation of test solution：Precision weighs cosmetic sample 0.25g (being accurate to 0.0001g), is placed in 25ml capacity
In bottle, methanol is added:Tetrahydrofuran=1:4v/v mixed liquor 20mL are ultrasonically treated 30min, take out and stand to room temperature, shake up, fixed
Hold, filtering；Filtrate 1.0ml is taken, with methanol dilution to 10.0ml, mixing, 0.45 μm of membrane filtration is as test solution；
Test sample measures：Serial mixed standard solution and test solution are subjected to liquid chromatogram measuring respectively.Chromatographic column
For Phenomenex Luna C18,4.6mm × 250mm, 5 μm.Test sample measure chromatographic condition be：Chromatographic column：C18 columns；Column
Temperature：35℃；Mobile phase：A is isopropanol:Methanol solution=1 containing 0.1% formic acid:4v/v, B are 0.05% aqueous formic acid；Stream
Speed：1.2mL/min；Sample size：10μL；Detection wavelength：300nm/350nm；Gradient elution program：0~5min, mobile phase
A75%, Mobile phase B 25%；5~6min, mobile phase A 75~85%, Mobile phase B 15~25%；6~10min, mobile phase
A85%, Mobile phase B 15%；10~15min, mobile phase A 85~90%, Mobile phase B 10~15%；15~17min, mobile phase
A90%, Mobile phase B 10%；17~35min, mobile phase A 100%, Mobile phase B 0%.
The response of serial mixed standard solution and test solution should all be detected in instrument within the scope of line style, be protected according to peak
Stay the time qualitative, according to peak area quantification.
Methanol, isopropanol, tetrahydrofuran, formic acid and sodium hydroxide are chromatographically pure, wherein formic acid, dimethyl sulfoxide (DMSO) purity
>=99%, formic acid purity >=99%.
In 19 kinds of sun-screening agents, in addition to Phenylbenzimidazolesulfonic acid and benzophenone -5, tetrahydrofuran is dissolved in, therefore with four
Hydrogen furans directly prepares remaining 17 kinds of sun-screening agent list mark mother liquor.And solubility of the Phenylbenzimidazolesulfonic acid in first alcohol and water is equal
It is poor, a small amount of sodium hydroxide solution can be used and make it completely dissolved, then with tetrahydrofuran constant volume.Benzophenone -5 is first added when dissolving
A small amount of methanol after making it completely dissolved, reuses tetrahydrofuran constant volume.
Methanol is 8 with tetrahydrofuran volume ratio:When 2, the sun-screening agent rate of recovery is above 97%.Therefore first is used in this research
Alcohol is 8 with tetrahydrofuran volume ratio:2 are used as sample extraction solvent.
The present invention by method in, using 0.05% formic acid as acid modification agent, 20% isopropanol of strong eluant, eluent
Methanol solution (contain 0.1% formic acid), gradient elution detaches 19 kinds of sun-screening agents, 19 kinds of component energy good separations.
Benzophenone -2, the own ester of diethylamino oxybenzene formylbenzoate and butyl methoxy dibenzoyl base in 19 kinds of sun-screening agents
Methane has maximal ultraviolet absorption peak at 350nm, has maximal ultraviolet absorption peak at 300nm in 16 type sun-screening agents.Therefore
The chromatogram that 19 kinds of sun-screening agents are carried out using two channels 300nm and 350nm is measured.
Embodiment 1
It is a kind of to measure Neo Heliopan E1000 in cosmetics, Uvinul T 150, double-ethylhexyl benzene simultaneously
Phenol anisyl triazine, Diethylhexyl Butamido Triazon, benzophenone-3, benzophenone -5, benzophenone -2, PABA ethyl hexyls
Ester, benzylidene camphor sulfonic acid, the own ester of diethylamino oxybenzene formylbenzoate, p-aminobenzoic acid, Phenylbenzimidazolesulfonic acid, 4-
Methyl benzyl subunit camphor, butylmethoxydibenzoylmethane, Octocrilene, ethylhexyl methoxy cinnamate, salicylic acid
The method of 19 kinds of sun-screening agents such as ethylhexyl, Homosalate and methylene bis-benzotriazolyl tetramethyl butyl phenol：
Methanol, isopropanol, tetrahydrofuran, formic acid and sodium hydroxide used are chromatographically pure, wherein formic acid, dimethyl sulfoxide (DMSO)
Purity >=99%, formic acid purity >=99%.
Single mark mother liquor：Precision is weighed after Phenylbenzimidazolesulfonic acid is completely dissolved with 1mol/L sodium hydroxide solutions and is used
Tetrahydrofuran constant volume；Precision, which weighs, uses tetrahydrofuran constant volume after benzophenone -5 is completely dissolved with methanol；Precision weighs remaining respectively
17 kinds of sun-screening agent standard substances, with the tetrahydrofuran dissolving containing 20% methanol and constant volume；The configuration concentration of single mark mother liquor is 1mg/
mL。
Mixed standard solution preparation：Precision pipettes each single mark mother liquor and is configured to mix with methanol dilution and constant volume in volumetric flask
Standardization solution.
Each standard substance sample weighting amount, constant volume and mixing Stock concentrations are as shown in table 1.
1 hybrid standard Stock concentrations of table
Serial mixed standard solution preparation：Dilute the serial mixed standard solution of preparation step by step with methanol；
The preparation of test solution：Precision weighs cosmetic sample (commercially available cream, oily and each 2 kinds of muffin class) 0.25g,
It is accurate to 0.0001g, is placed in 25ml volumetric flasks, methanol is added:Tetrahydrofuran=1:4v/v mixed liquor 20mL are ultrasonically treated
30min takes out and stands to room temperature, shakes up, constant volume, filters；Filtrate 1.0ml is taken, with methanol dilution to 10.0ml, mixing, 0.45 μ
M membrane filtrations are as test solution；
Test sample measures：Serial mixed standard solution and test solution are subjected to liquid chromatogram measuring respectively.Chromatographic column
For Phenomenex Luna C18,4.6mm × 250mm, 5 μm.Test sample measure chromatographic condition be：Chromatographic column：C18 columns；Column
Temperature：35℃；Mobile phase：A is isopropanol:Methanol solution=1 containing 0.1% formic acid:4v/v, B are 0.05% aqueous formic acid；Stream
Speed：1.2mL/min；Sample size：10μL；Detection wavelength：300nm/350nm；Gradient elution program：0~5min, mobile phase
A75%, Mobile phase B 25%；5~6min, mobile phase A 75~85%, Mobile phase B 15~25%；6~10min, mobile phase
A85%, Mobile phase B 15%；10~15min, mobile phase A 85~90%, Mobile phase B 10~15%；15~17min, mobile phase
A90%, Mobile phase B 10%；17~35min, mobile phase A 100%, Mobile phase B 0%.Gradient elution program is shown in Table 2.
2 gradient elution program of table
| Time (min) | A (%) | B (%) |
| 0~5 | 75 | 25 |
| 5~6 | 75~85 | 25~15 |
| 6~10 | 85 | 15 |
| 10~15 | 85~90 | 15~10 |
| 15~17 | 90 | 10 |
| 17~35 | 100 | 0 |
The response of serial mixed standard solution and test solution should all be detected in instrument within the scope of line style, be protected according to peak
Stay the time qualitative, according to peak area quantification.
Embodiment 2
The range of linearity and detection limit (LOD), quantitative limit (LOQ)：
It takes series standard solution to be measured analysis, is ordinate into line using sun-proof agent concentration as abscissa, peak area
Property regression analysis.
19 kinds of sun-screening agent hybrid standards, which are made, with the dairy products of washing one's face without sun-screening agent adds matrix solution to be diluted step by step,
Measure the detection limit and quantitative limit of this method, sample size when using S/N=3 and S/N=10 is as LOD and LOQ.It the results are shown in Table 3.
The linear result and LOD, LOQ of 3 19 kinds of sun-screening agents of table
Measurement result shows that for all sun-screening agents within the scope of sample introduction, sample introduction concentration is in preferably linear with chromatographic peak area
Relationship, related coefficient are all higher than 0.99.
Embodiment 3
The rate of recovery is measured with precision：
Four kinds of each one kind of different substrates cosmetics such as water, lotion, cream, face cleaning of the selection without sun-screening agent, each takes 9
Part, be separately added into low (60%), in (100%), high (140%) three concentration reference substance, every part of concentration gradient sample does 3
Duplicate Samples carry out sample treatment and measurement according to the method that this research is established, calculate the rate of recovery and RSD, the results are shown in Table 4.
4 hybrid standard Stock concentrations (n=9) of table
In different substrates the sample recovery rate range of each component 96.3%~104.3%, RSD ranging from 0.82~
2.45%, show that method accuracy is good, it is matrixing that selected extracting method adapts to four kinds of water, lotion, cream and face cleaning
Cosmetic.
Embodiment 4
Detection method provided by the invention with《Cosmetics safety technical specification》Method detection as defined in (version in 2015) is anti-
Shine the comparison of agent：
Primary dcreening operation chooses a more sample of type containing sun-screening agent, according to《Specification》The phenyl benzo miaow that version in 2015 is recorded
The assay method that 15 kinds of azoles sulfonic acid etc. carries out assay, and is compared with method determination data provided by the invention, gained 2
Group data are indicated with means standard deviation (± s), using PASW Statistics22.0 versions statistical software to each group of data
Carry out statistical procedures：Small sample is examined using shapiro-wilk, and display each group of data is in normal distribution.Each Sets of Measurement money
Expect that comparison among groups use one-way analysis of variance, Levene homogeneitys test of variance.Through analyzing, assay knot between two groups of data
There are significant difference components 5, respectively benzophenone-3,4- methyl benzyl subunits camphor, methoxy cinnamic acid ethyl hexyl for fruit
Ester, ethylhexyl salicylate and Homosalate show as newly-established method measurement result and are higher than original method result.As a result see
Table 5.
2 method measurement results of 55 kinds of components of table compare (n=2)
| This method content (%) | Standard method content (%) | Conspicuousness | |
| Benzophenone-3 | 1.04±0.06 | 0.90±0.003 | 0.003 |
| 4- methyl benzyl subunit camphors | 0.27±0.02 | 0.25±0.003 | 0.048 |
| Ethylhexyl methoxy cinnamate | 6.01±0.54 | 5.31±0.09 | 0.045 |
| Ethylhexyl salicylate | 7.99±0.40 | 7.03±0.16 | 0.004 |
| Homosalate | 11.10±0.04 | 7.43±0.09 | 0.000 |
Embodiment 5
Cosmetic sample tests and analyzes：
The inspection detection that sun-screening agent is carried out with 70 batch sample of detection method pair (commercially available) provided by the invention, calculates sun-proof
Agent content, and the component result of measurement is compared with Product labelling and official written reply.
As a result use the type of sun-screening agent and met using concentration currently in real 70 batch samples《Specification》Requirement,
But has and actually detect sunscreen component and label/inconsistent situation of official written reply information in 9 batch samples.In wherein 4 batch samples
The sun-screening agent (being further verified using LC-MS methods) other than labeled marker has been detected, has prompted have enterprise not by official written reply
The possibility of formula production or fake products；Another 5 batch is that the sun-screening agent of part labels mark is not detected, and prompts have product stabilization
Property it is undesirable, press official written reply formula production or fake products possibility.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail can carry out a variety of transformation to technical scheme of the present invention, these letters within the scope of the technical concept of the present invention
Monotropic type all belongs to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments and step,
In the case of no contradiction, it can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention couple
Various combinations of possible ways no longer separately illustrate.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. method that is a kind of while measuring 19 kinds of sun-screening agents in cosmetics, which is characterized in that 19 kinds of sun-screening agents are：To first
Oxygroup isoamyl cinnamate, Uvinul T 150, double-ethylhexylphenol anisyl triazine, Diethylhexyl butamido
Base triazinone, benzophenone-3, benzophenone -5, benzophenone -2, PABA ethylhexyls, benzylidene camphor sulfonic acid, diethylamino oxybenzene first
Acyl group hexyl-benzoate, p-aminobenzoic acid, Phenylbenzimidazolesulfonic acid, 4- methyl benzyl subunits camphor, butylmethoxy hexichol
Formyl methylmethane, Octocrilene, ethylhexyl methoxy cinnamate, ethylhexyl salicylate, Homosalate and di-2-ethylhexylphosphine oxide-benzene
And triazolyl tetramethyl butyl phenol；
The method includes：
Single mark mother liquor：Precision weighs after Phenylbenzimidazolesulfonic acid is completely dissolved with 1mol/L sodium hydroxide solutions and uses tetrahydrochysene
Furans constant volume；Precision, which weighs, uses tetrahydrofuran constant volume after benzophenone -5 is completely dissolved with methanol；Precision weighs remaining 17 kinds respectively
Sun-screening agent standard substance, with the tetrahydrofuran dissolving containing 20% methanol and constant volume；
Mixed standard solution preparation：Precision pipettes each single mark mother liquor and is configured to mixing mark with methanol dilution and constant volume in volumetric flask
Quasi- solution；
Serial mixed standard solution preparation：Dilute the serial mixed standard solution of preparation step by step with methanol；
The preparation of test solution：Precision weighs cosmetic sample 0.25g, is placed in 25ml volumetric flasks, and methanol and tetrahydrochysene is added
Furans mixed liquor 20mL is ultrasonically treated 30min, takes out and stands to room temperature, shakes up, constant volume, filters；Filtrate 1.0ml is taken, methanol is used
It is diluted to 10.0ml, mixing, 0.45 μm of membrane filtration is as test solution；
Test sample measures：Serial mixed standard solution and test solution are subjected to liquid chromatogram measuring respectively.
2. method that is according to claim 1 a kind of while measuring 19 kinds of sun-screening agents in cosmetics, it is characterised in that：It is described
The configuration concentration of single mark mother liquor be 1mg/mL.
3. method that is according to claim 1 a kind of while measuring 19 kinds of sun-screening agents in cosmetics, it is characterised in that：It is described
Test sample measure chromatographic condition be：
Chromatographic column：C18 columns；
Column temperature：35℃；
Mobile phase：A is isopropanol:Methanol solution=1 containing 0.1% formic acid:4v/v, B are 0.05% aqueous formic acid；
Flow velocity：1.2mL/min；
Sample size：10μL；
Detection wavelength：300nm/350nm；
Gradient elution program：0~5min, mobile phase A 75%, Mobile phase B 25%；5~6min, mobile phase A 75~85%, flowing
Phase B15~25%；6~10min, mobile phase A 85%, Mobile phase B 15%；10~15min, mobile phase A 85~90%, mobile phase
B10~15%；15~17min, mobile phase A 90%, Mobile phase B 10%；17~35min, mobile phase A 100%, mobile phase
B0%.
4. method that is according to claim 3 a kind of while measuring 19 kinds of sun-screening agents in cosmetics, it is characterised in that：It is described
Chromatographic column be Phenomenex Luna C18,4.6mm × 250mm, 5 μm.
5. method that is according to claim 1 a kind of while measuring 19 kinds of sun-screening agents in cosmetics, it is characterised in that：It is described
Cosmetics include cream kind, oily class and muffin class.
6. method that is according to claim 1 a kind of while measuring 19 kinds of sun-screening agents in cosmetics, it is characterised in that：It is described
Test solution when preparing, methanol and tetrahydrofuran mixed liquor are methanol:Tetrahydrofuran=1:4v/v.
7. method that is according to claim 1 a kind of while measuring 19 kinds of sun-screening agents in cosmetics, it is characterised in that：It is described
Precision weigh to be accurate to 0.0001g.
8. a kind of according to claim 1~7 any one while the method for measuring 19 kinds of sun-screening agents in cosmetics, special
Sign is：Methanol, isopropanol, tetrahydrofuran, formic acid and the sodium hydroxide is chromatographically pure, and wherein formic acid, dimethyl are sub-
Sulfone purity >=99%.
9. a kind of according to claim 1~7 any one while the method for measuring 19 kinds of sun-screening agents in cosmetics, special
Sign is：Formic acid purity >=99%.
10. a kind of according to claim 1~7 any one while the method for measuring 19 kinds of sun-screening agents in cosmetics,
It is characterized in that：When measurement, the response of serial mixed standard solution and test solution should all be detected in instrument within the scope of line style,
It is qualitative according to peak retention time, according to peak area quantification.
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Application publication date: 20181113 |