fragrance retention, release and sensory perception from surfactant-rich rinse-off cosmetics

session: sensory evaluation of fats17th AOCS Latin American Congress and Exhibition on Fats, Oils, and Lipids September 11–14, 2017

martin vethamuthu, sergio lira, edwarddiantonio, hani fares and linda foltis

agenda

critical role of fragrance oils in cosmetics

in-vivo instrumental method to evaluate fragrance impacto liquid body wash with polymer technologyo soap bars with polymer technologyo screening polymers for fragrance retention/release

review of innovations: fragrance encapsulation

testing stability and performance of fragrance encapsulateso leakage potential and capsule integrity in formulationso expert performance evaluation

conclusion

solving for efficient delivery of fragrance

pH-4.6 pH-5.6 pH-5.7

pH-4.7 pH-6.8pH-5.5

pH 6.8 pH 5.5 pH 6.5

pH 6.8 pH 6.6 pH 5.5 pH 7.0

pH 10

product sight, smell, touch mood & sensorial experience

fragrance impact vs investment

multisensory perception

consumer satisfaction / repurchase

challenge: very low level of fragrance deposited from rinse-off cosmetics

critical role of fragrance oils in cosmetics

o delivers a pleasing scento masks an unpleasant odoro immediate / lingering scent

provides a hedonic impacto reinforces perception of the

products purpose and efficacy

o fragrances are considered the most effective “value-booster” and “brand differentiators” in cosmetics

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high initial impact out of bottle

long lasting scent

bloom in shower

fragrance deposition from body wash

daily conditioning

body wash is a prototype that

contains a polymeric deposition technology

(GHPTMC)

new method

sampling setup - twister bar

o sample preparation: an area of 18cm2 of the volar forearm was washed with the cleansing formulation for 30 seconds, wait 10 seconds, and rinsed with tap water for 30 seconds then towel dried

o the washed area of the arm was exposed to the twister bar setup for 15 minutes. this step is repeated at 1 hour intervals, three times, for head space extraction

o after extraction the twister bar is removed and placed into clean glass thermal desorption tubes for fragrance analysis

GC/MS with GERSTEL MPS robotic sampler, thermal desorption unit(TDU), and cooled injection system (CIS) option is used tomonitor the fragrance release profile as a function of time

GC/MS with Gerstel MPS robotic sampler TDU-CIS

twister instrumentation

comparison of SPME fiber to twister bar

conditioning polymer enhances fragrance deposition on skin after rinse

Guar hydroxypropyltrimonium chloride (GHPTMC: N-Hance™ CCG45)

results from fragrance evaluator

• 1 – no scent• 2 – Weak• 3 – Medium• 4 – Moderately Strong• 5 - Strong

Formulation with N-Hance CCG-45 (GHPTMC) shows improved initial bloom,

deposition and retention on skin

polymers tested – soap bar study

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ceraphyl™ RMTmaleic anhydride/ castor oil adduct

(1:1)

O OO

OH

O

OOHOH

O

H2CO

HCOH2CO

n-hance™ 3196guar hydroxypropyltrimonium chloride

(GHPTMC)

N-Hance SP-100acrylamidopropyltrimonium

chloride/acrylamide copolymer

benecel™ K200Mhydroxypropylmethylcellulose

superior fragrance deposition and reduced cracking

fragranced soap plus0.5% Benecel K200M

(HPMC)

fragrance control no polymer

all polymers tested significantly enhances dihydro-myrcenol retention on skin

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screening of polymer N-Hance SP100:effect of concentration and no polymer

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0.0E+00

2.0E+06

4.0E+06

6.0E+06

8.0E+06

1.0E+07

1.2E+07

1.4E+07

1.6E+07

GC A

rea

Coun

t

1.5% Fragrance

0.75% Fragrance

0.0E+00

2.0E+06

4.0E+06

6.0E+06

8.0E+06

1.0E+07

1.2E+07

1.4E+07

1.6E+07

GC A

rea

Coun

t

0.5% PolymerNo Polymer

review of innovations - encapsulates

o capture perfume oilso protect & store in formulationo slow and sustained release o triggers- UV light, heat, pH, rubbing,

hydrolysis, enzymes, O2

current technologieso polymeric shell around fragrance oil

composed of melamine resin crosslinked with formaldehyde through interfacial precipitation

o poly-urea based shell crosslinked with isocyanate through interfacial polymerization

new technologyo melamine/formaldehyde and amine

free shell chemistryo more surfactant tolerant shello fragrance loading ~ 30%o size of capsules 5-30 microns

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formulations tested

Standard SLES/CAPB surfactant system tested with 1.0% total fragrance

− 1: 100% Fragrance Oil− 2: 80% Fragrance Oil/20% Encapsulated Fragrance− 3: 50% Fragrance Oil/50% Encapsulated Fragrance− 4: 0% Fragrance Oil/100% Encapsulated Fragrance

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acceptable viscosity over time at 25°C and 45°C

05,000

10,00015,00020,00025,00030,00035,00040,000

Initial 1 week 2 weeks 4 weeks 8 weeks 12 weeks

Viscosity over time 25C formulas

1% Encapsulate 25C 0.5% Encapsulate/0.5% Fragrance 25C

0.2% Encapsulate/0.8% Fragrance 25C 1% Fragrance 25C

Blank

05,000

10,00015,00020,00025,00030,00035,00040,000

Initial 1 week 2 weeks 4 weeks 8 weeks 12 weeks

Viscosity over time 45 C formulas

1% Encapsulate 45C 0.5% Encapsulate/0.5% Fragrance 45C

0.2% Encapsulate/0.8% Fragrance 45C 1% Fragrance 45C

Blank

05,000

10,00015,00020,00025,00030,00035,00040,000

Initial 1 week 2 weeks 4 weeks 8 weeks 12 weeks

1% Encapsulate in 12 Weeks

1% Encapsulate 25C 1% Encapsulate 45C

1% encapsulate in surfactant formulation 45°C & 25°C after 90 days

encapsulates remain intact after 90 days in both temperature conditions40X magnification

GERSTEL MPS as headspace autosampler coupled to agilent technologies GC 7890B with MPS

o 180 samples, 1g eacho critical for all samples to be

filled same timeo samples removed at scheduled

time intervals for measuring GC head space of fragrance notes

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formulation with 1% encapsulates shows greatest protection & lowest leakage of fragrance

-5.0E+05

0.0E+00

5.0E+05

1.0E+06

1.5E+06

2.0E+06

2.5E+06

3.0E+06

3.5E+06

0 1 2 3 4 5 6 7 8 9 10 11 12 13

GC

area

cou

nt

Time (weeks)

Limonene peak at 25 C1% Fragrance 25°C0.2% Encapsulate +0.8% Fragrance 25°C0.5% Encapsulate +0.5% Fragrance 25°C1% Encapsulate 25°C

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at 45°C, the formulations with higher level of neat fragrance shows less protection & higher leakage

0.0E+00

5.0E+05

1.0E+06

1.5E+06

2.0E+06

2.5E+06

3.0E+06

3.5E+06

4.0E+06

4.5E+06

0 1 2 3 4 5 6 7 8 9 10 11 12 13

GC

area

cou

nt

Time (weeks)

Limonene peak at 45C1% Fragrance 45°C0.2% Encapsulate +0.8% Fragrance 45°C0.5% Encapsulate +0.5% Fragrance 45°C1% Encapsulate 45°C

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formulations with encapsulated fragrance options show longer lasting fragrance perception

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

5

Initial After rinse Dry skin 15 min 30 min 1 hour 2 hour 4 hour 8 hour

Eval

uato

ry S

core

1% Fragrance 0.8% Fragrance/0.2% Encaps 0.5% Fragrance/0.5% Encaps 1% Encaps

conclusions

o perfume design and creation of novel fragrance oils are essential steps to satisfy consumer need in cosmetic products

o use of polymeric ingredients can enhance the deposition of fragrances from liquid and bar soap formulations

o encapsulation of fragrance oils can lead to improved fragrance intensity, bloom and longevity

o an In-Vivo instrumental method was used to evaluate and differentiate fragrance impact

o melamine, formaldehyde and amine free fragrance encapsulates with loadings above 30% can be created to protect fragrance oils from leakage with good capsule integrity as demonstrated by testing stability for 12 weeks

o next steps: develop method for evaluating bloom in shower

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acknowledgements

o bradford team: abdul Hussain, kishor mistry, ben sales

o ROA team for soap bars: angelito delos reyes; nilesh dhole; s. ganesh; gwendolyn neoh

o bridgewater fragrance evaluation: linda melilo

o presentation review team: linda foltis; william davis; sang-taekim; jason yearout; carolmarie brown

o robertet team for fragrance design

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thank you

questions?

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disclaimer

The information contained in this presentation and the various products described are intended for use only by persons having technical skill and at their own discretion and risk after they have performed necessary technical investigations, tests and evaluations of the products and their uses. This material is for informational purposes only and describes the scientific support for the use of the products described herein as an ingredient in cosmetic products intended to enhance appearance and other cosmetic benefits or to enhance performance of an end product. Certain end uses of these products may be regulated pursuant to rules governing medical devices or other regulations governing drug uses. It is the purchaser’s responsibility to determine the applicability of such regulations to its products. While the information herein is believed to be reliable, we do not guarantee its accuracy and a purchaser must make its own determination of a product’s suitability for purchaser’s use, for the protection of the environment, and for the health and safety of its employees and the purchasers of its products.

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The testing information (the “Testing Information”) has been gratuitously provided by Ashland. The Testing Information is based on many factors beyond Ashland’s control, including but not limited to, the conditions prevailing when the testing was conducted, and in some cases, is based on data generated with development samples of the Active Ingredient. Although it is intended to be accurate, ASHLAND DISCLAIMS ANY AND ALL LIABILITY, EITHER EXPRESS OR IMPLIED. The Testing Information is confidential or proprietary to Ashland, and may not, except as provided below, be disclosed to any third party. You may not make commercial use of the Testing Information, or make claims with respect to your products based the Testing Information, without the written agreement with Ashland covering such use.

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