防晒配方开发
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SPF 50+ ，PA++++防晒配方开发技巧
2016 Merck 研讨会
Agenda
1 2 3 4
防晒配方开发基本原则及SPF 指数增效手段
SPF 50+/PA++++配方解析
In Vivo SPF VS In Vitro SPF 测试
配方实例
2
防晒产品开发 Warning –防晒产品是难度“最大”的化妆品配方开发 Formulation 配方 Preservation 防腐体系 Stability 稳定性 Aesthetics 感官评价 Balancing Act –杰出的防晒产品是“平衡艺术”
Always back up plan
0.18% Microcare MTB (Methylisothiazolinone and Polyaminopropyl Biguanide) + 1% Sensiva SC10 (Ethylhexylglycerin & Caprylyl Glycol)
1% Dermosoft Octiol H (Caprylyl Glycol & Hinokitiol) but expensive Optiphen 1% (Phenoxyethanol & Caprylyl Glycol) + 0.1% Neolone 950 (Methylisothiazolinone)
14
SPF 增效途径 II
Functional filler are king: 功能填料是防晒体系最重要的肤感调节剂和SPF增效剂 LF-2000, Soft Sphere, BN, LDP white, Silica – Good for after feel, cushion and spread – Powders are very good at stopping greasiness and improving after feel: – Watchout for compatibility with TiO2 – LDP WHITE 人体法 SPF 增效结果（MERCK 专利 2015） O/W 有机无机防晒体系SPF 可以增效 21%(in vitro SPF，3.0% LDP WHITE）
Cetiol CC, ININ Abil Wax 9801 (Cetyl Dimethicone)
小技巧：如何初判固体防晒剂稳定性测试是否不易结晶析出： Make oil phase and place in at 5 C overnight to check for crystalization
W/O 体系， SPF增效达 42.5% (in vivo SPF，3.0% LDP WHITE）
15
I.
Results Impact within a O/W formulation containing organic and inorganic UV-filters, in vitro
40.00 35.00 30.00
in vivo SPF
37.5 28.7
29.7
10 1.7 0 Base 3% RonaFlair® LDP White without UV-filter 3% RonaFlair® Extender W 3% RonaFlair® Flawless 3% RonaFlair® LDP White
9
o
Emulsifiers 乳化剂的选择 使用主，辅乳化剂 平衡肤感和 乳化剂用量的 关系
STABILITY
AESTHETICS
10
O/W 防晒体系主，辅乳化剂搭配（尤其是因为无机防晒剂可能吸附乳化剂的效应） 主乳化剂 Amphisol K (Potassium Cetyl Phospate, DEA-Cetyl Phosphate) Arlacel 165 (Glyceryl Stearate and PEG-100 Stearate) Lanette 16 (Cetyl Alcohol) Brij 56/72/721 (Cetech 10/Steareth-2/Steareth-21) Ceralution ES, H, S，POLYGLYCERYL-10 OLEATE（喷雾） 带有乳化功能的 辅乳化剂 Pemulen TR-2 (Acrylates/C10-30 Alkyl Acrylate Crosspolymer) Sepiplus 400 (Polyacrylate-13 & Polyisobutene & Polysorbate 20)
Base containing UV filters: 2% Eusolex® T-AVO 10% Eusolex® OCR 3% Eusolex® 9020
In vitro SPF
25.00 20.00 15.00 10.00 26.54 28.02 32.10
5.00
0.00 Base 3% RonaFlair® Flawless 3% RonaFlair® LDP White
配方原型 注册（特殊类申报，及人体SPF) 中试和 大试 理化稳定性和防腐挑战性试验
4
防晒剂的选择
专利含防晒剂搭配 –光稳定系统 A product with 2% BMDBM and 10% OCR named “BULLFROG” has been published in Australia in the “Prescription Products Guide 1989” and was free prior art as early as February 1989 EP 0514491 from L’Oréal has been revoked in EU due to this prior art in Australia Other L’Oréal patents dealing also with the combination of OCR/BMDBM are US 5576354, US 5587150, JP 2975682B2, AU 652742B2, FR 2658075
13
SPF 增效途径 I
SPF 增效剂 和 成膜剂选择
Common Boosters: Eusolex 232 Eusolex UV-PEARL OMC and OB-S T-2000 dispersion in different phase Tinosorb S
Film Formers: Lexfilm Sun, spray (Inolex Chemical), KP-545 (Shin-Etsu), and DC593 good film forming/aesthetics
O
h *
O
O
O
t-Butyl
Avobenzone
h O *
O
cleavage
O
derived Photoproducts
•
HO
•
O PhOCH3 COOC8H17
t-Butyl
OMC+Avobenzone 不可逆光降解
7 Presentation title in footer | 26 May 2012
All priority dates of the above mentioned patents are after the February 2009.
Neutrogena: Heliopan@: Avobenzone+BP-3+ Corapan TQ
check the situation by internal patent experts
17
功能性填料增效SPF研究
机理探究：进一步研究进行中
协同无机形成更 增加紫外线散射 效果
填料本身有纳米 材料包裹 （TiO2/ZnO）
加连续均匀的膜
球状结构比片状
填料更具优势
18
Agenda
1 2 3 4
防晒配方开发基本原则及SPF 指数增效手段
SPF 50+/PA++++配方解析
In Vivo SPF VS In Vitro SPF 测试
12
Preservative选择
Fungi is a major issue Stay away from Parabens – deactivated by many sunscreens
Kill rate is slower for sunscreens. 70% PET is critical
和公司法规部门确认是否涉及专利
5
防晒剂的选择
Bulletproof Sunscreens “防弹级搭配”
Combination of OCR&Avobenzone&T-AVO or T-EASY Combination of OCR&Avobenzone&UV-PEARL OMC or UV-PEARL OB-S Eusolex T , UV-TITAN + UV-PEARL Photostabilizer 光稳定剂 （稳定OMC 和 Avobenzone 防止光降解) Diethylhexyl Syringylidene Malonate(ST Liquid,0.2%) Bis-Ethylhexyl Hydroxydimethoxy Benzylmalonate(Ronacare AP,0.5%)
3
防晒新品开发程序
防晒产品开发时间有限(E.G. Registration
time in China is about 10-12 months. While 3 months is enough for SPF products Regulation in Korea)
很多部门合作 Work closely with IP, MRKING, RA, Analytical team, Engineering team. 主要步骤: Prototyping Registration Pilots & Trial Stability
60
40
20
0
1:0:0
1 : 4.5 : 0
1 : 4.5 : 2.5
Ratio BMDBM : OCR : OMC
8
油脂的选择
极性酯类或者用液体有机防晒剂分散固体防晒剂 选用不同极性和铺展性的油脂来改变防晒配方在皮肤上的铺展和吸收。使用一些 报道有SPF 增效的合成酯类
Finsolv TPP (C12-15 Alkyl Benzoate and Dipropylene Glycol Dibenzoate and PPG-15 Stearyl Ether Benzoate)
MDA-S-121-01
百度文库16
II: Impact within a W/O formulation containing organic UV-filters, in vivo
60
Base containing UV filters:
50 40 30 20 40.9
10% Eusolex® HMS 10% Eusolex® OCR 5% Eusolex® 9020 5% Eusolex® OS
6
防晒剂之间的兼容性 防晒剂之间的兼容性 OMC 不可逆光降解化学反应
OMC
COOC8H17 H3COPh H3COPh COOC8H17
H3COPh
COOC8H17
Dimer
H3COPh COOC8H17
OMC
O
H
O
Photoketonisatio n
t-Butyl
Avobenzone 不可逆光降解
t-ButylPh
Avobenzone
HO t-ButylPh H3COPh
O PhOCH3 COOC8H17
H3COPh
Dimer
O O t-ButylPh H3COPh COOC8H17 PhOCH3
OMC
100
Residual amount of BMDBM [%]
80
after 5 MED
11
W/O 防晒体系乳化剂搭配（高粉含量体系易得）
EM 90, 97（硅油包水）, WE 09（硅油包水） PGPH, TGI,P-135（含有Avobenzone 体系）
W/Si system – KSG 210, KF 6017, KF 6028, KF 6038 – WE 09 – DC 5225C, 3225C – Easy Nov
2016 Merck 研讨会
Agenda
1 2 3 4
防晒配方开发基本原则及SPF 指数增效手段
SPF 50+/PA++++配方解析
In Vivo SPF VS In Vitro SPF 测试
配方实例
2
防晒产品开发 Warning –防晒产品是难度“最大”的化妆品配方开发 Formulation 配方 Preservation 防腐体系 Stability 稳定性 Aesthetics 感官评价 Balancing Act –杰出的防晒产品是“平衡艺术”
Always back up plan
0.18% Microcare MTB (Methylisothiazolinone and Polyaminopropyl Biguanide) + 1% Sensiva SC10 (Ethylhexylglycerin & Caprylyl Glycol)
1% Dermosoft Octiol H (Caprylyl Glycol & Hinokitiol) but expensive Optiphen 1% (Phenoxyethanol & Caprylyl Glycol) + 0.1% Neolone 950 (Methylisothiazolinone)
14
SPF 增效途径 II
Functional filler are king: 功能填料是防晒体系最重要的肤感调节剂和SPF增效剂 LF-2000, Soft Sphere, BN, LDP white, Silica – Good for after feel, cushion and spread – Powders are very good at stopping greasiness and improving after feel: – Watchout for compatibility with TiO2 – LDP WHITE 人体法 SPF 增效结果（MERCK 专利 2015） O/W 有机无机防晒体系SPF 可以增效 21%(in vitro SPF，3.0% LDP WHITE）
Cetiol CC, ININ Abil Wax 9801 (Cetyl Dimethicone)
小技巧：如何初判固体防晒剂稳定性测试是否不易结晶析出： Make oil phase and place in at 5 C overnight to check for crystalization
W/O 体系， SPF增效达 42.5% (in vivo SPF，3.0% LDP WHITE）
15
I.
Results Impact within a O/W formulation containing organic and inorganic UV-filters, in vitro
40.00 35.00 30.00
in vivo SPF
37.5 28.7
29.7
10 1.7 0 Base 3% RonaFlair® LDP White without UV-filter 3% RonaFlair® Extender W 3% RonaFlair® Flawless 3% RonaFlair® LDP White
9
o
Emulsifiers 乳化剂的选择 使用主，辅乳化剂 平衡肤感和 乳化剂用量的 关系
STABILITY
AESTHETICS
10
O/W 防晒体系主，辅乳化剂搭配（尤其是因为无机防晒剂可能吸附乳化剂的效应） 主乳化剂 Amphisol K (Potassium Cetyl Phospate, DEA-Cetyl Phosphate) Arlacel 165 (Glyceryl Stearate and PEG-100 Stearate) Lanette 16 (Cetyl Alcohol) Brij 56/72/721 (Cetech 10/Steareth-2/Steareth-21) Ceralution ES, H, S，POLYGLYCERYL-10 OLEATE（喷雾） 带有乳化功能的 辅乳化剂 Pemulen TR-2 (Acrylates/C10-30 Alkyl Acrylate Crosspolymer) Sepiplus 400 (Polyacrylate-13 & Polyisobutene & Polysorbate 20)
Base containing UV filters: 2% Eusolex® T-AVO 10% Eusolex® OCR 3% Eusolex® 9020
In vitro SPF
25.00 20.00 15.00 10.00 26.54 28.02 32.10
5.00
0.00 Base 3% RonaFlair® Flawless 3% RonaFlair® LDP White
配方原型 注册（特殊类申报，及人体SPF) 中试和 大试 理化稳定性和防腐挑战性试验
4
防晒剂的选择
专利含防晒剂搭配 –光稳定系统 A product with 2% BMDBM and 10% OCR named “BULLFROG” has been published in Australia in the “Prescription Products Guide 1989” and was free prior art as early as February 1989 EP 0514491 from L’Oréal has been revoked in EU due to this prior art in Australia Other L’Oréal patents dealing also with the combination of OCR/BMDBM are US 5576354, US 5587150, JP 2975682B2, AU 652742B2, FR 2658075
13
SPF 增效途径 I
SPF 增效剂 和 成膜剂选择
Common Boosters: Eusolex 232 Eusolex UV-PEARL OMC and OB-S T-2000 dispersion in different phase Tinosorb S
Film Formers: Lexfilm Sun, spray (Inolex Chemical), KP-545 (Shin-Etsu), and DC593 good film forming/aesthetics
O
h *
O
O
O
t-Butyl
Avobenzone
h O *
O
cleavage
O
derived Photoproducts
•
HO
•
O PhOCH3 COOC8H17
t-Butyl
OMC+Avobenzone 不可逆光降解
7 Presentation title in footer | 26 May 2012
All priority dates of the above mentioned patents are after the February 2009.
Neutrogena: Heliopan@: Avobenzone+BP-3+ Corapan TQ
check the situation by internal patent experts
17
功能性填料增效SPF研究
机理探究：进一步研究进行中
协同无机形成更 增加紫外线散射 效果
填料本身有纳米 材料包裹 （TiO2/ZnO）
加连续均匀的膜
球状结构比片状
填料更具优势
18
Agenda
1 2 3 4
防晒配方开发基本原则及SPF 指数增效手段
SPF 50+/PA++++配方解析
In Vivo SPF VS In Vitro SPF 测试
12
Preservative选择
Fungi is a major issue Stay away from Parabens – deactivated by many sunscreens
Kill rate is slower for sunscreens. 70% PET is critical
和公司法规部门确认是否涉及专利
5
防晒剂的选择
Bulletproof Sunscreens “防弹级搭配”
Combination of OCR&Avobenzone&T-AVO or T-EASY Combination of OCR&Avobenzone&UV-PEARL OMC or UV-PEARL OB-S Eusolex T , UV-TITAN + UV-PEARL Photostabilizer 光稳定剂 （稳定OMC 和 Avobenzone 防止光降解) Diethylhexyl Syringylidene Malonate(ST Liquid,0.2%) Bis-Ethylhexyl Hydroxydimethoxy Benzylmalonate(Ronacare AP,0.5%)
3
防晒新品开发程序
防晒产品开发时间有限(E.G. Registration
time in China is about 10-12 months. While 3 months is enough for SPF products Regulation in Korea)
很多部门合作 Work closely with IP, MRKING, RA, Analytical team, Engineering team. 主要步骤: Prototyping Registration Pilots & Trial Stability
60
40
20
0
1:0:0
1 : 4.5 : 0
1 : 4.5 : 2.5
Ratio BMDBM : OCR : OMC
8
油脂的选择
极性酯类或者用液体有机防晒剂分散固体防晒剂 选用不同极性和铺展性的油脂来改变防晒配方在皮肤上的铺展和吸收。使用一些 报道有SPF 增效的合成酯类
Finsolv TPP (C12-15 Alkyl Benzoate and Dipropylene Glycol Dibenzoate and PPG-15 Stearyl Ether Benzoate)
MDA-S-121-01
百度文库16
II: Impact within a W/O formulation containing organic UV-filters, in vivo
60
Base containing UV filters:
50 40 30 20 40.9
10% Eusolex® HMS 10% Eusolex® OCR 5% Eusolex® 9020 5% Eusolex® OS
6
防晒剂之间的兼容性 防晒剂之间的兼容性 OMC 不可逆光降解化学反应
OMC
COOC8H17 H3COPh H3COPh COOC8H17
H3COPh
COOC8H17
Dimer
H3COPh COOC8H17
OMC
O
H
O
Photoketonisatio n
t-Butyl
Avobenzone 不可逆光降解
t-ButylPh
Avobenzone
HO t-ButylPh H3COPh
O PhOCH3 COOC8H17
H3COPh
Dimer
O O t-ButylPh H3COPh COOC8H17 PhOCH3
OMC
100
Residual amount of BMDBM [%]
80
after 5 MED
11
W/O 防晒体系乳化剂搭配（高粉含量体系易得）
EM 90, 97（硅油包水）, WE 09（硅油包水） PGPH, TGI,P-135（含有Avobenzone 体系）
W/Si system – KSG 210, KF 6017, KF 6028, KF 6038 – WE 09 – DC 5225C, 3225C – Easy Nov