Dsm Influence Tio2 Dispersion on Wr in Cosmetics 2010 Westenfelder[1]

In-Cosmetics 13-15 April 2010

0

Influence of Titanium DioxideDispersions on Water Resistance ofSun Care Products

Presentation at In-Cosmetics 13-15 April 2010

Horst Westenfelder, Dr. Thomas Satzinger


CONTENT OF PRESENTATION

111 COLIPA Guideline for Evaluating Sun Products onWater ResistanceCOLIPA Guideline for Evaluating Sun Products onCOLIPA Guideline for Evaluating Sun Products onWater ResistanceWater Resistance

222 Factors Influencing Water Resistance§ Emulsifiers§ Polymers§ Formulation Requirements§ Influence of UV Filters

Factors Influencing Water ResistanceFactors Influencing Water Resistance§§ EmulsifiersEmulsifiers§§ PolymersPolymers§§ Formulation RequirementsFormulation Requirements§§ Influence of UV FiltersInfluence of UV Filters

333 Influence of Different Particulate UV-Filters onWater Resistance§ In-vitro Test System to Analyze Water Resistance§ Test Results

Influence of Different Particulate UVInfluence of Different Particulate UV--Filters onFilters onWater ResistanceWater Resistance§§ InIn--vitro Test System to Analyze Water Resistancevitro Test System to Analyze Water Resistance§§ Test ResultsTest Results




222 Factors Influencing on Water Resistance§ Emulsifiers§ Polymers§ Formulation Requirements§ Influence of UV Filters

Factors Influencing on Water ResistanceFactors Influencing on Water Resistance§§ EmulsifiersEmulsifiers§§ PolymersPolymers§§ Formulation RequirementsFormulation Requirements§§ Influence of UV FiltersInfluence of UV Filters




3COLIPA Guidelines to Test Water Resistance

§§ 2mg/cm2mg/cm22 of product has to be applied and the SPF has to beof product has to be applied and the SPF has to betested according the standard way of SPF testing.tested according the standard way of SPF testing.

§§ 10 to 12 persons are required to run a full study10 to 12 persons are required to run a full study

§§ The people are immersed for 20 minutes after that step theyThe people are immersed for 20 minutes after that step theyhave to leave the bath and allow to dry for 15 minuteshave to leave the bath and allow to dry for 15 minutes

§§ The use of towels is not recommended air drying is preferredThe use of towels is not recommended air drying is preferred

§§ After 15 to 30 minutes of drying time the volunteers have to doAfter 15 to 30 minutes of drying time the volunteers have to do aasecond run of 20 minutes of immersionsecond run of 20 minutes of immersion

§§ Drying step of 15 minutes without using towelsDrying step of 15 minutes without using towels

§§ After that the SPF has to be tested again according the COLIPAAfter that the SPF has to be tested again according the COLIPAstandardstandard

§§ Calculation of the SPF the next dayCalculation of the SPF the next day


4COLIPA Guidelines to Test VERY Water-Resistance

§§ 2mg/cm2 of product has to be applied and the SPF has to be2mg/cm2 of product has to be applied and the SPF has to betested according the standard way of SPF testing.tested according the standard way of SPF testing.

§§ 10 to 12 people are required to run a full study10 to 12 people are required to run a full study

§§ Same procedure as for waterSame procedure as for water--resistant but 2 more immersionresistant but 2 more immersionsteps of 20 minutes are requiredsteps of 20 minutes are required

§§ After that step the SPF has to be tested again according theAfter that step the SPF has to be tested again according theCOLIPA standardCOLIPA standard

§§ Calculation of the SPF the next dayCalculation of the SPF the next day


GNPD Research of Sunscreen Product Launchessince 2005

4.500

500

4.000

1.500

3.0002.5002.000

3.500

1.000

0Waterproof

823

Water Resistant

297

UV Protection

4.101

Hypoallergenic

1.379

AMPHISOLCetyl PegGlycerine StearateGlyceryl Stearate Citrate

ØØ AMPHISOLAMPHISOL®® is the Emulsifier of choice for all kind of Sun Careis the Emulsifier of choice for all kind of Sun CareProductsProducts

9%

25%

25%

41%

12%

23%

23%

43%

0%15%

15%

70%

17%

15%

15%

53%


7Influence of Emulsifiers on Water Resistance

§§ Reason for that is AMPHISOLReason for that is AMPHISOL®® K can not be easily washed offK can not be easily washed offafter the volatile part of the formulation is evaporatedafter the volatile part of the formulation is evaporated

§§ This leads in many cases to a water resistant formulationThis leads in many cases to a water resistant formulation

§§ AMPHISOLAMPHISOL®® K can be combined with polymers to improve theK can be combined with polymers to improve thewaterwater--resistance or to achieve the claim very waterresistance or to achieve the claim very water--resistantresistant

ØØ Emulsifiers have a tremendous influence on SPF performanceEmulsifiers have a tremendous influence on SPF performanceand water resistanceand water resistance


8

Local Trends and how they Influence the Compositionof Cosmetic Formulations

§§ Silicone issue started in Canada and is spreading now to FranceSilicone issue started in Canada and is spreading now to Franceand Germanyand Germany

§§ Only volatile Silicone oils are seen as critical, but this becomOnly volatile Silicone oils are seen as critical, but this becomes aes abig influence for using Silicones in generalbig influence for using Silicones in general

§§ Silicone Emulsifiers (W/Si) could be helpful for water resistantSilicone Emulsifiers (W/Si) could be helpful for water resistantformulations but the use is becoming impossible for someformulations but the use is becoming impossible for somecompaniescompanies

ØØ Silicones are very useful to improve water resistance, howeverSilicones are very useful to improve water resistance, howeverdue to upcoming regional safety discussions silicones aredue to upcoming regional safety discussions silicones arebecoming under pressurebecoming under pressure


9

Local Trends and how they Influence the Compositionof Cosmetic Formulations

§§ Light formulations are very importantLight formulations are very important

§§ Water/Oil formulation could be very useful to formulate waterWater/Oil formulation could be very useful to formulate water--resistant and even very waterresistant and even very water--resistant productsresistant products

§§ Consumer expectations are different, many companies areConsumer expectations are different, many companies areforced by their customers to formulate very light and easy toforced by their customers to formulate very light and easy toabsorb productsabsorb products

§§ AMPHISOLAMPHISOL®® K can be an emulsifier of choice because all levelsK can be an emulsifier of choice because all levelsof oil loading are possibleof oil loading are possible


10

Influence of UV filters

§§ Most of the relevant UV filters are oil solubleMost of the relevant UV filters are oil soluble

§§ But there is a certain number of water soluble filters availableBut there is a certain number of water soluble filters availableand used:and used:qq BenzophenoneBenzophenone 44qq PEGPEG--25 PABA25 PABAqq Phenylbenzimidazole sulphonic acidPhenylbenzimidazole sulphonic acid PARSOLPARSOL®® HSHSqq DDisodium phenyl dibenzimidazole tetrasulfonateisodium phenyl dibenzimidazole tetrasulfonateqq Methylene bisMethylene bis--benzotriazolyl tetranethylbutylphenolbenzotriazolyl tetranethylbutylphenol

dispersiondispersion

§§ To achieve water resistance it is crucial that the SPF is notTo achieve water resistance it is crucial that the SPF is notmainly coming from the watermainly coming from the water--soluble UVsoluble UV--filter part of thefilter part of theformulation but it is still useful to have some of these filtersformulation but it is still useful to have some of these filtersin the formulation.in the formulation.

ØØ The use of water soluble UV filters is always critical in waterThe use of water soluble UV filters is always critical in waterresistant formulations and have to be chosen carefullyresistant formulations and have to be chosen carefully


11

PARSOL® SLX High Protection Water ResistantEfficacy Data –Water Resistance

ØØ DSM 6BDSM 6B ––with a PARSOLwith a PARSOL®® HS content of 2%HS content of 2% -- provides waterprovides water--resistance according to the COLIPA method (Spa)resistance according to the COLIPA method (Spa)

0

10

20

30

40

50

60

DSM 6B

55,9

DSM 6A

42,448,0

DSM 6

3.0 %

UV Filter Combination

PARSOL® SLX(Polysilicone-15)PARSOL® HS(Phenylbenzimidazole Sulfonic Acid)PARSOL® 340(Octocrylene)PARSOL® 1789(Butyl Methoxydibenzoylmethane)

4.0 %

3.6 %

4.0 %

3.0 %

3.0 %

6.0 %

4.0 %

3.0 %

2.0 %

8.0 %

4.0 %

Wat

er R

esis

tanc

e


12

PARSOL® SLX High Protection Water ResistantEfficacy Data - Summary

3.0 %

UV Filter Combination

PARSOL® SLX(Polysilicone-15)PARSOL® HS(Phenylbenzimidazole Sulfonic Acid)PARSOL® 340(Octocrylene)PARSOL® 1789(Butyl Methoxydibenzoylmethane)

4.0 %

3.6 %

4.0 %

3.0 %

3.0 %

6.0 %

4.0 %

3.0 %

2.0 %

8.0 %

4.0 %

DSM 6 DSM 6A DSM 6B

35.4In vivo SPF

SPF 95% Cl

In vivo SPF (wet) after 40 min SPApool

Water Resistance (%)

29 - 42

14.5

42.4 %

37.6

31 - 44

18.7

48.0 %

35.8

28 - 44

20.2

55.9 %

WRR 90% Conf. Interval 36 - 49 % 42 - 54 % 47 -64 %

Results


14

Influence of Technical Ingredients on Water Resistancefor example TiO2 / TiO2 Dispersions

§§ Water resistance is a very sensitive test and is influenced byWater resistance is a very sensitive test and is influenced bymany factorsmany factors

§§ In an in vitro study we have analyzed the influence of technicalIn an in vitro study we have analyzed the influence of technicalingredients (Emulsifiers)ingredients (Emulsifiers)

§§ We compared PARSOLWe compared PARSOL®® TX versus PARSOLTX versus PARSOL®® TX50 AB andTX50 AB andalso some other dispersions of particulate organic and inorganicalso some other dispersions of particulate organic and inorganicUV FiltersUV Filters

§§ We analyzed the SPF performance and compared the waterWe analyzed the SPF performance and compared the waterresistance in vitro by using our test systemresistance in vitro by using our test system


15In vitro Set Up to Test Water Resistance

§§ To test waterTo test water--resistance in vivo is very expensiveresistance in vivo is very expensive

§§ We were looking to find an in vitro system which gives us anWe were looking to find an in vitro system which gives us anindication of the water resistanceindication of the water resistance

§§ As starting point we have tested the in vitro SPF by using ourAs starting point we have tested the in vitro SPF by using ourMUT systemMUT system

§§ Apply 0.7mg/cmApply 0.7mg/cm22 on PMMA plateson PMMA plates

§§ Immersion took place in 2L beakers at 29Immersion took place in 2L beakers at 29°°C at moderate stirringC at moderate stirring

§§ Water quality was tap waterWater quality was tap water

§§ SPF test with MUTSPF test with MUT

§§ Two times 20 minutes of immersions by slightly moving the tapTwo times 20 minutes of immersions by slightly moving the tapwaterwater


161.1. Application of productApplication of product 2.2. Homogenous distribution of the productHomogenous distribution of the product

3.3. Water bath 29Water bath 29°°C tap water (C tap water (Water is movedWater is movedcarefullycarefully)

In vitro Set Up to Test Water Resistance


17

Test Formulations for Water Resistance in vitro study

2.00AMPHISOL® KAMPHISOL® K 2.00 2.00 2.002.00

PARSOL®

TX50 ABPARSOL®

TXCompetitor

1Competitor

2Competitor

3

2.00LanetteLanette 2.00 2.00 2.002.00

4.00Cetiol CCetiol C 4.00 4.00 4.004.00

8.00Finsolv TNFinsolv TN 8.00 8.00 8.008.00

5.00Dermofeel BGCDermofeel BGC 8.00 8.00 5.008.00

0.05BHTBHT 0.05 0.05 0.050.05

0.80PhenonipPhenonip 0.80 0.80 0.800.80

PARSOL® 1789/ PARSOL® 340,PARSOL® 5000PARSOL® 1789/ PARSOL® 340,PARSOL® 5000

4.00/ 8.00/4.00

4.00/ 8.00/4.00

4.00/ 8.00/4.00

4.00/ 8.00/4.00

4.00/ 8.00/4.00

PARSOL® TX50 ABPARSOL® TX50 AB 10.00

PARSOL® TXPARSOL® TX 5.00

MBTP Dispersion (50% active)MBTP Dispersion (50% active) 10.00

Titanium Dioxide (TMCS)Titanium Dioxide (TMCS) 5.00

11.10Titanium Dioxide (and) DiethylhexylCarbonate (and) Polyglyceryl-6Polyhydroxystearate (45% active)

Titanium Dioxide (and) DiethylhexylCarbonate (and) Polyglyceryl-6Polyhydroxystearate (45% active)

Pemulen/ Keltrol/ EDTA/ WasserPemulen/ Keltrol/ EDTA/ Wasser 0.4/ ad 100 0.4/ ad 100 0.4/ ad 100 0.4/ ad 1000.4/ ad 100


18

In vitro Water Resistance of Sunscreens containingIn vitro Water Resistance of Sunscreens containingdifferent Pigment Qualitiesdifferent Pigment Qualities

ØØ Quality of coating and optimized emulsifier system have aQuality of coating and optimized emulsifier system have atremendous influence on water resistance and SPFtremendous influence on water resistance and SPF

0

10

20

30

40

50

60

70

80

53,2

PARSOL®TX50 AB

79,2

PARSOL® TX

76,2

Competitor 1

52,0

Competitor 3 Competitor 2

73,2

MB

TP D

ispe

rsio

n(5

0% a

ctiv

e)

Tita

nium

Dio

xide

(TM

CS)

Tita

nium

Dio

xide

(and

) Die

thyl

hexy

lC

arbo

nate

(and

) Pol

ygly

cery

l-6Po

lyhy

drox

yste

arat

e (4

5% a

ctiv

e)

Tita

nium

Dio

xide

, C12

-15

Alk

yl B

enzo

ate,

Poly

glyc

eryl

-2-D

ipol

yhyd

roxy

stea

rate

,Si

lica,

Dim

ethi

cone

Tita

nium

Dio

xide

, Sili

ca, D

imet

hico

ne


19

Test Results for Water Resistance in vitro study

46.10In vitro SPF initial 48.50 43.10 38.3048.10

PARSOL®TX50 AB

PARSOL®TX

Competitor1

Competitor2

Competitor3

41.00In vitro SPF after 20 minwater immersion 42.10 28.40 30.0026.10

36.70In vitro SPF after 40 minwater immersion 37.20 23.40 28.3025.50

79.16Water resistance (%) after40 min water immersion 76.21 53.21 73.1952.02

ØØ Quality of coating and the composition of the formulation has aQuality of coating and the composition of the formulation has astrong influence on performancestrong influence on performance


20

Conclusions

ØØ Emulsifiers have a tremendous influence on SPF performanceEmulsifiers have a tremendous influence on SPF performanceand water resistanceand water resistance

ØØ AMPHISOLAMPHISOL®® is the Emulsifier of choice for all kind of Sun Careis the Emulsifier of choice for all kind of Sun CareProductsProducts

ØØ Silicones are very useful to improve water resistance, howeverSilicones are very useful to improve water resistance, howeverdue to upcoming regional safety discussions under pressuredue to upcoming regional safety discussions under pressure

ØØ The use of water soluble UV filters is always critical in waterThe use of water soluble UV filters is always critical in waterresistant formulations and have to be chosen carefullyresistant formulations and have to be chosen carefully

ØØ In vitro water resistant tests are useful to give an indicationIn vitro water resistant tests are useful to give an indication ofofformulation performanceformulation performance

ØØ Quality of coating and optimized emulsifier system have aQuality of coating and optimized emulsifier system have atremendous influence on water resistance and SPFtremendous influence on water resistance and SPF

ØØ PARSOLPARSOL®® TX50 AB fulfills all requirements to formulate waterTX50 AB fulfills all requirements to formulate waterresistant formulationsresistant formulations


21Thank You!Thank You!

““We offer a full range of innovative highWe offer a full range of innovative high--performance UVA and UVB filtersperformance UVA and UVB filtersand technical support to meet your sunscreen formulation requireand technical support to meet your sunscreen formulation requirements,ments,

while guaranteeing the highest standardswhile guaranteeing the highest standardsin quality, safety, reliability and compliance.in quality, safety, reliability and compliance.““

Thomas SatzingerThomas SatzingerMarc HentschMarc HentschJJüürgenrgen VollhardtVollhardtChristine MendrokChristine Mendrok--EdingerEdingerAnne JanssenAnne JanssenKarinaKarina RadomskyRadomsky

Dsm Influence Tio2 Dispersion on Wr in Cosmetics 2010 Westenfelder[1]

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