23 - 02 - 14 Latest Developments in Claim Substantiation Methods Ver 1 - OCR

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LATEST DEVELOPMENTS
HAIR CONDITIONING TESTS
IN HAIR CLAIM
Dr. Paul Cornwell
SUBSTANTIATION
Business Development Director, TRI Princeton

METHODS
Paul Cornwell and Eleanor Lehman, TRI Princeton

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TRI Princeton IFSCC
~
TRI Princeton is a world-leading research institute focused
on hair and skin testing for cosmetics, dermatology, and a
wide range of other applications

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Look out for
learning
resources
available in TRI
Library

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Team effort IFSCC
~
Contributors to this presentation

¨ David Graham, President


¨ Ernesta Malinauskyte, Dir. Hair Research
¨ Samuel Gourion-Arsiquaud, Dir. Skin and
Biosubstrates
¨ Trefor Evans, Institute Fellow
¨ Plus many others!

Pictured (l-r) are Xuzi Kang, Muriel Mason, Vanessa Castro, Amy Jarosz, David Graham (TRI President),
Ernesta Malinasukyte, Matt Jarosz, Alison Robinson, Jessica Turner, Guilherme Fratassi, Marcella
Gabarra

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Outline IFSCC
~

¨ Introduction to hair product evaluation and claims


¨ New thinking
¨ New protocols
¨ Method validation
¨ Conclusion

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Hair and scalp care - $80 billion category IFSCC
~

No.1
Bond Multiplier.
OLAPLEX
UGIHHIHG THE REIUllDING
RESTORE•
This concentroted first so Ion step rebuilds HAIR SERUM
StRUMPO<,R
broken disulfide bonds and begins the CfiEVEUX
process of preventing damage and REPARA110••
BR/l(ANCE
repairing hair.
JOml/1.011.~

~
co

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Hair product evaluation IFSCC
~
¨ Product evaluation: “assessment of one
or more of the attributes, characteristics
or qualities of a product”1

¨ Uses;
• New product development
• Formulation changes
• Performance versus competitors
• Validation of product claims

1. Principle of Product Evaluation: Objective Sensory Methods. IFSCC Monograph Number 1.


https://ifscc.org/monographs/monograph-no-1-principles-of-product-evaluation-objective-sensory-methods/

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General procedure for objective evaluation1 IFSCC
~
1. Objective
New thinking

2. Outline considerations

3. Detailed protocol New protocols

4. Operation

5. Validity Method validation

6. Conclusions

1. Principle of Product Evaluation: Objective Sensory Methods. IFSCC Monograph Number 1.


https://ifscc.org/monographs/monograph-no-1-principles-of-product-evaluation-objective-sensory-methods/

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The art of translation for instrumental testing ~
IFSCC
~
Consumer Scientific

• Build up • Fibre diameter


• Conditioning • Surface friction
• Moisturisation • Water isotherms
• Shine • Light scatter
• Softness • Modulus
• Strength • SEM images
• Volume • IR Spectrum
• Etc etc
Consumer language…may not match technical
understanding2,3
2. Evans, T. (2012) Hair Care Product Claims. In: Practical Modern Hair Science (Evans, T. and Wickett, R.R. (Eds.) Allured !Bi
Library
Business Media, Ch 15, pp 498-531
3. Evans, T. (2020) Practical Aspects of Shampoo and Conditioner Testing. In: Practical Aspects of Cosmetic Testing 2nd Edition
(Fluhr, J.W., Ed.), Springer-Verlag, Ch 19, pp 207-227
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Types of hair tests IFSCC
~

Consumer Fibre
(sensory) Array tests Fibre tests composition
tests tests

Perception claims Performance claims Mechanism claims Mechanism claims


(e.g. 80% of women (e.g. damaged hair (e.g. reverses the (e.g. replaces the
thought it made their was made 2x effects of damage lipids lost from
damaged hair softer smoother) on the structure of damaged hair)
to touch) internal hair
proteins)

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Selecting your claims test – at TRI Princeton IFSCC
~

Consumer Fibre
(sensory) Array tests Fibre tests composition
tests tests

1. Repeated grooming 1. Single fibre tensile 1. Hair/sebum lipids


2. Ease of combing 2. Single fibre fatigue 2. Hair proteins
3. Hair colour fade 3. Single fibre torsion 3. Delivery – spectroscopy
4. Style retention 4. Raman - disulphide (FTIR/Raman)
5. Frizz control bonds 4. Delivery - fluorescence
6. Volume 5. SEM imaging
…..etc 6. Thermal analysis (DSC)
…..etc
For details visit www.triprinceton.org
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New thinking – Bond Builders IFSCC
~
¨ New definition: “a treatment that is able to penetrate into the hair and to
improve or restore the internal structure of hair, giving rise to an
improvement in hair mechanical properties”4,5
Figure 1- The Growth of Bond-Building Claims In Hair Care

450
400
350
No.1
BondMultipt,e,. i
cl:
300
250
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co
0
200
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E
:, 150
z
b ' 100
._......
p-oceacl ~rl:rgcbnagear.d
50
0
2012 2013 2014 2015 2016 2017 2018 2019 2020 2021
Yeot

• Search on Mintel GNPDfrom 2012 • 2021, searching for shampoos, conditioners, hair styling products and
hair treatments containing the term 'bond' OR 'bonds' ond A D NOT 'bonding' In the product description.
Excludes co/oront$.

4. Cornwell, P.A., Marsh, J. (2023) Bond Builders: Do They Really Repair Hair? Cosmetics & Toiletries Magazine, in press
5. Cornwell, P.A. (2022, Oct 12) Do bond builders really repair the hair? TRI Talks 2023, Presented live and on-line on October 12th !Bi
Library

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New Thinking – Bond Builders IFSCC
~
¨ Proposed approach for claims: (i) active penetration, (ii) improvement or
restoration of internal hair structures, and (iii) improvements in mechanical
properties 4
(i) (ii) (iii)
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4. Cornwell, P.A., Marsh, J. (2023) Bond Builders: Do They Really Repair Hair? Cosmetics & Toiletries Magazine, in press
6. Figure (i) from - Malinauskyte, E., Shrestha, R., Cornwell, P.A., Gourion-Arsiquaud, S., Hindley, M. (2021) Penetration of different
molecular weight hydrolysed keratins into hair fibers and their effects on the physical properties of textured hair. Int J Cosmet Sci 43(1)
26-37
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New Thinking – Hair Porosity IFSCC
~
¨ New methods for investigating the lateral diffusion of water and actives in
single hair fibres5

D2 0 Diffusion in Virgin Hair


.a

Control O 0.5 1.5 2.5 3.5 an

I , .
I ., 11 C ~
I ' •I

u [
I
; ·, "> 'i I ' C

5. Senak, L. (2022, Dec 7) Innovative method to evaluate hair structure and chemistry by investigating the diffusion of actives.
Presentation at TRI Talks, live and on-line Dec 7th
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New Thinking – Hair Porosity IFSCC
~
¨ New methods for investigating the lateral diffusion of water and actives in
single hair fibres5
Rhodamine Bin D2OWater (48-hours) - CROSS-
SECTIONS
Guillotine Soak - 9% bleached MB hair

0 cm 0.5 cm 1 cm 1.5 cm 2 cm

0 0
5. Senak, L. (2022, Dec 7) Innovative method to evaluate hair structure and chemistry by investigating the diffusion of actives.
Presentation at TRI Talks, live and on-line Dec 7th
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New Protocols – Repeated Grooming + IA IFSCC
~
¨ Existing repeated grooming protocol is used to measure hair breakage6,7
I Scope Assesses the number of hairs in a tress
-
NEVPANTENE
-· that break during repeated
brushing/combing strokes. Any anti-
breakage benefits of using hair care
products can be evaluated by the
reduction in the number of broken hair
fibers.
- -
Hair 8”/3g tresses, flat crimped, treated +
THICKER dried and equilibrated at 60% R.H.,
- STRONGER
HAIR
IN hair types selected
140A '
Method Evaluate hair breakage by counting
broken fibers on floor of instrument
after every 200 brushes/combs to the
_L maximum of 2000 brushes/combs
Measurement Broken hairs collected
parameters
I I I

6. Evans, T.A., and Park, K. (2010) A statistical analysis of hair breakage. II. Repeated grooming experiments. Journal of Cosmetic Science
61(November/December), 439-455
7. Evans, T. (2014) Measuring Hair Strength, Part II: Fiber Breakage. Cosmetics & Toiletries Magazine, Vol. 128, 12(December), 854-859
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New Protocols – Repeated Grooming + IA IFSCC
~
¨ New protocol and apparatus developed together with Newtone uses IA to
measure number and lengths of broken hairs
Correlation between manual and instrument counts of broken hairs (n=300 trays)
250

Number of broken hairs counted by image analysis


200
y = 1.1993x
R² = 0.9786

150

100

50

0
0 20 40 60 80 100 120 140 160 180 200

Number of broken hairs counted manually

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New Protocols – Repeated Grooming + IA IFSCC
~
¨ Hair lengths are not normally distributed and need Log conversion


-
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New Protocols – Repeated Grooming + IA IFSCC
~
¨ Measurement of broken hair lengths creates new possibilities

¨ Advantages: Treatment effects on length of broken fibres


(geometric means +/- s.d.)
• Increased sensitivity - The large replicate numbers in 14

Mean fibre length (geo. mean)


hair length data vs hair number data (n=1000+ vs 12

n=10) mean that there is better discrimination 10

8
between treatments – a second ‘bite at the cherry’ if --
6
numbers of broken hairs show no difference 4

• Magnification of effects – The cumulative lengths of 2

hair lost (equivalent to weight of hair lost) shows 0


Cell 1 SLES Control Cell 2 Shampoo Cell 3 Shampoo +
Conditioner
larger changes than the numbers of hair lost*
Use of logged data gives better discrimination between treatments
Treatment Hair length

* In the data shown here, amount of hair lost by use Log mean Log std dev Geo mean + geo s.d. - geo s.d. Confl.
Groups
Mean s.d. Confl.
Groups
of S+C is 5-fold lower than the control, whereas the (p<0.05) (p<0.05)
Cell 4 SLES Control 0.80 0.32 6.24 6.80 3.25 A 8.20 7.43 A
number of hairs list is reduced only 3-fold Cell 5 Shampoo
Cell 6 Shampoo + Conditioner I
0.71
0.66 I 0.30
0.31 I 5.12
4.53 I 5.14
4.67 I 2.57
2.30 I B
C I 6.58
6.20 I 5.77
9.41 I B
B

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New Protocols – Repeated Grooming + Type 4 Hair IFSCC
~
¨ Manual protocol has been developed for Walker Type 4 hair

¨ Key aspects 90
c Mean
OMearttSE

Focussed on wet combing for this hair


80
I

~
M•anctSD

type, rehydrating hair every 20
: 70
~
0

~ 60
passes to maintain wetness of tress ~
38%·
~ 50

~
I!!
• Hand bound 0.25g mini-tresses •
.0
.: 40 48%·
C
g:i 64%. l
!
(Walker Type 4, L’Oreal Type VII
64%"

~
iii
~
30

hair), pre-damaged and weakened, 20

with special dry combing protocol 10


Suave Cantu Macadamia Macadamia Nexxus
Shampoo Shampoo Shampoo+ Shampoo+ Shampoo+

Advantages
+ LeaveIn Condilloner Mask Conditioner
¨ Treatment

• Now possible to differentiate


breakage following different
treatments on Type 4 Hair

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New Protocols – Shine + Type 4 Hair IFSCC
~
¨ Existing shine protocol is used to measure surface gloss8
Scope The SAMBA system detects the amount of
polarized light that is reflected off the
hair surface, the shine from the hair can
be quantified with some of the well-
established shine equations
Hair 8”/3g tresses, flat crimped, treated +
dried and equilibrated at 60% R.H., hair
types selected as required
Method Switches are mounted, combed and
aligned over a black metal cylinder and
illuminated with polarised light. Images
S of the gloss bands are analysed by
*100% image analysis
Dq 0 Measurement Software calculates Reich-Robbins shine
parameters values.

8. C. Reich and C. R. Robbins (1993) Light Scattering and Shine Measurements of Human Hair: A Sensitive Probe of the Hair
Surface, J. Soc. Cosmet. Chem., 44 (1993), pp. 221-234.

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New Protocols – Shine + Type 4 Hair IFSCC
~
¨ New protocol has been developed for Walker Type 4 hair

Key aspects
3000
¨ 2800 0 ~:
SE
!SO
.,...,. f 0

¢
2600

¢ ~
• Custom-made light box 2400 70'II·
.i 2200
• 1g hand bound tresses (Walker Type ja:.. 2000
1800 0.5'11,•t
0
4, L’Oreal Type VII hair) .8 E
1600
1400
1°'6-'l

-l
• Careful control of illumination and 1200
1000
¢471'1·1

camera settings 800


600
Suaveshampoo Canru Cowa.i.

• Image J used to measure the number Dustsebum


Treatment
Cantuco wash• CantuHCC

of reflections per unit area


¨ Advantages
• Now possible to differentiate shine
following different treatments on Type
4 Hair

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New Protocols – Wet Combing + Type 4 Hair IFSCC
~
¨ Existing combing protocol is used to measure wet and dry combability9
Scope Determines the level of wet or dry
conditioning on hair by measuring the
force to drag a wet hair tress
through a comb
Hair 8”/3g tresses, flat crimped, treated
and blotted-dry, hair types selected
as required
WetCombingGraph Method Instron, 10N Load Cell, fine-toothed
comb.
Measurement Peak combing force also known as
parameters ‘maximum load’ (gf)

Extension(irdES)

9. Evans, T. (2013) Evaluating Hair Conditioning with Automated Combing. Cosmetics & Toiletries Magazine, Vol. 126, 8(August), 558-563

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New Protocols – Wet Combing + Type 4 Hair IFSCC
~
¨ New protocol has been developed for Walker Type 4 hair
¨ Key aspects
J
220
o Mean

• Wet comb only


200

180
cp QMoantSe
I MtantSD

• Hand bound and pre-selected 0.25g ':160


~
0
23%"
~
2°140
mini-tresses (Walker Type 4, L’Oreal 25

u~ 47%"
120

Type VII hair) 100


C±J 52%" l 54%"

• Validated, wider-toothed combs 80


~
C±J
60
Suave Cantu Macadamia Mac.edamia NHXUS

• Hair re-wetted regularly Shampoo Shampoo


+ LeaveIn
Shampoo+
CondJUonor
Shampoo+
Masi<
City Shield
Shampoo+
Rlns.d Rinsed Condilklner

Delete comb pattern after each pass


R/Med
• Treatment

¨ Advantages
• Now possible to differentiate combing
forces following different treatments
on Type 4 Hair

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New Protocols – Curl Elongation + Type 4 Hair IFSCC
~
¨ New protocol has been developed for Walker Type 4 hair
~~----------------~--------
¨ Key aspects ~ -a 51.9%. I 55.7%. I
qp
59.0%. l
~
59.0%. I
= @
,..:Sc
Lj:-1
.c -10
ti,
C¥J 38.6%. j 63.8%" t 64.8%. l
• Hand bound 0.25g mini-tresses i -12
_,
.!: -14 ciJ
(Walker Type 4, L’Oreal Type VII 2
& -16
-18
u
hair) -20
-22

• Tresses dried at 60% RH


-24
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Cantu Jane Carter
Curls to Go
• Images taken over 8 h
(/)

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• LabView IA software used to extract


...,
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f a Mean
□ Mean:SE
b

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X
I Mean±SD Treettnenlol CtJ~lype VII 0 25 g Tress
... ...
_,._, Advantages
I
.. tftt ... toll

---- • Now possible to differentiate curl


elongation effects following different
treatments on Type 4 Hair

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New Protocols – Hair Lipid Analysis IFSCC
~
¨ Hair lipid analysis and analysis of hair oil treatments by chromatography

¨ Potential claim areas


• Prevention of damage to lipids for
hair mildness claims
• Supplementation of lipids for hair
strength and damage treatment
claims…for all hair types

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New Protocols – Hair Lipid Analysis IFSCC
~
¨ Hair lipid analysis and analysis of hair oil treatments by chromatography
¨ Key aspects
• Protocols developed for sebum
sampling from the scalp, extraction of
lipids from hair samples and for the
analysis of hair oil products All four stages pooled
Hexane
• HPTLC being used in research projects C:M=2:1
C:M=1:1
to investigate differences in lipids C:M=1:2

Diglycerols

Rest (more non-polar)


Cholesterol sulphate and other polar lipids

Free fatty acids


between panellists and over time

Monoglycerols

Cholesterol
• For the latest data see Ernesta’s TRI
Talk from November10

10. Malinauskyte, E. (2022, Nov 30) What kind of lipids do we seek for hair? Presented at TRI Talks 2022, live and on-line Nov 30th

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Call for sponsors IFSCC
~

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New Protocols – Scalp Imaging System IFSCC
~
¨ In-situ analysis of scalp scaling and skin redness

¨ Potential claim areas


• Anti-dandruff
• Sensitive scalp

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New Protocols – Scalp Imaging System IFSCC
~
¨ In-situ analysis of scalp scaling and skin redness Validation tests showed that Majority of panelists
identified as having dandruff by dermatologists also had
scales identified by the image analysis (P<0.05, Chi-
¨ Key aspects squared)
70

• The Scalp and Dandruff Image 60

Number of panellists
50
Analysis System developed by 40

Newtone allows us to use the 30

images recorded with a macro 20

10
imaging system (SkinCamTM) to 0
Yes No
visualise and characterise scalp
scaling and skin colour changes Validation tests also showed that the number of scales
recorded related well with dermatologist defined dandruff
associated with inflammation severity (n=150)
700

• SDAIS allows us to detect hair 600

500

fibres and remove them from the

Number of scales
400

region of interest. This just leaves 300

the exposed scalp skin for analysis


200

100

++
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New Protocols – Scalp Imaging System IFSCC
~
¨ In-situ analysis of scalp scaling and skin redness
Increased skin darkness in subjects with scalp
¨ Key aspects scaling (p<0.05 for all hair types)

• IA can also detect changes in scalp


No Scales
skin colour 60

With scales
50
• Recent studies showed that scaling
was associated with a darkening

Mean L value
40

of surrounding skin areas, 30

presumably through increased 20


blood flow
10
• For more data, come to the Multi-
0
Ethnic Hair and Scalp Care Hair Type 2 Hair Type 3 Hair Type 4

Symposium (live and on-line, June Hair Type No scales With scales Two tailed T-test, equal
5-6, Redbank, NJ) Hair Type 2
Number
45
Mean
47.45
Std Dev
7.12
Number
35
Mean
43.60
Std Dev
9.24
variances (p value)
0.0382
Hair Type 3
Hair Type 4
29
19 I 44.95
31.10 I 8.57
11.60
49
66 I 37.59
22.82 I 8.84
10.10
0.0006
0.0031

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Method validation IFSCC
~
¨ Repeated grooming and hair damage

¨ Increased bleaching times give higher


Bleached Asian and Chinese Hair Tresses
breakage – validating the accuracy of - RPGData Combined
the repeated grooming method 350
Asian Hair •
~ 300
.c Chinese Hair •
~ 250
¨ Non-linear relationship suggest that C
QI
~ 200
peroxide damage accelerates as the ai
0 150
hair becomes more damaged ] 100
E
~ so
0 ....................... .···········••"'' ·············••••••••••••
0 20 40 60 80 100
Total Bleached Minutes - TBMs

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~
Method validation IFSCC
~
¨ Repeated grooming and hair damage
Cysteic Creation after Bleaching Asian and Chinese Hair
Tresses- Combined Data
¨ ATR-FTIR measurement of cysteic acid 0.250
;:;--
levels suggested that damage levels 41

.
C

correlate, in a linear fashion, to bleach ! 0.200 Chinese Hair •


........
··•····
Asian Hair •
...•···.
exposure times
~ ,
·.:;
ct 0.150
.iu
+ 0.0476
~ 0.100
y = 0.00lBx

t,.
....•··•·····
~ 0.050 ••
41
>
·.:;
{l 0.000
~ 0 20 40 60 80
Total Bleached Minutes - TBMs

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~
Conclusions & next steps IFSCC
~
¨ “If you can not measure it, you can not improve it” Lord Kelvin (1824-1907)

¨ In order to make new or stronger claims, you always need better measurement
techniques

¨ Future work in TRI include:


• Development of more lipid and protein analysis capabilities
• Miniaturisation and automation of tests
• Further cross-validation of assays to ensure reliability

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From: TRI Princeton (library.triprinceton.org)

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