International Journal of Cosmetic Science, 2016, 38, 266271
12288
A proposal of a standardized protocol to evaluate waterproof effect
of eyeliner and mascara
M. J. Kim*, Y. K. Seo*, Y. C. Boo and J. S. Koh*
*Dermapro LTD., Skin Research Center, Seoul, Korea and Department of Molecular Medicine and Cell and Matrix Research Institute, Kyungpook
National University School of Medicine, Daegu, Korea
Received 27 July 2015, Accepted 6 October 2015
Keywords: colour cosmetics, colour measurement, image analysis, percentage waterproof ratio (%WPR), waterproof effect
Abstract
OBJECTIVE: Eye make-up products must have waterproofing prop-
erties to make sure that their colours do not smudge or wash away
easily and remain intact despite water or perspiration. Until now,
most research has focused on composition and components of
make-up products and not on the level of waterproof. This study
aimed to find methods to assess the waterproof degree of eyeliners
and mascaras and determine the suitability of these methods.
METHODS: Twenty female subjects were selected to test the
waterproof of eyeliners, whereas 20 sets of false eyelashes were
used to evaluate the waterproof of mascaras. For evaluating water-
resistant properties, after test sites where eyeliners and mascaras
were applied were immersed in water and natural drying for over
20 min (not artificial drying by drier etc.), L* value of the eyeliners
applied on the forearm before and after the immersions, and inten-
sity analysis values of mascaras applied on the false eyelashes were
used to calculate the mean percentage waterproof removal ratio (%
WPR). A product was hypothesized to be water resistant if the
value for the mean %WPR was 50%.
RESULTS: The non-waterproof eyeliners were not waterproof if
their mean %WPR was >50%, whereas the waterproof eyeliners
were waterproof if their mean %WPR was <50%.
For mascaras, the mean %WPR was <50% after 1- to 2-h marks
after immersion in water for both non-waterproof and waterproof
products. After 34 h, the mean %WPR for the non-waterproof
mascaras was >50%, rendering them not waterproof, whereas the
mean %WPR for the waterproof mascaras was <50%, making them
waterproof.
CONCLUSION: We have evaluated the waterproof properties by
analysing photographed images of the test sites where eyeliners
and mascaras were applied. Results of the comparison between
non-waterproof and waterproof eyeliners and mascaras, and the
methods used, in particular, will be found useful in evaluating
waterproof of other make-up products.
Re
sume

OBJECTIF: Les produits de maquillage des yeux doivent avoir des
 leau pour faire en sorte que leurs
propri
et
es de r
esistance a
couleurs ne migrent ni se d
etachent facilement et restent intacts,
Correspondence: Min Ji Kim, Dermapro LTD., Skin Research Center, 4F
Jiho B/D, Bangbaejoongang-ro 30, Seocho-gu, Seoul 137-843, Korea.
Tel.: +82 2 597 5434; fax: +82 2 597 5430; e-mail: minji-cos@
hanmail.net
266 2015 Society of Cosmetic Scientists and the Soci
et
e Francaise de Cosm
etologie
doi: 10.1111/ics.
malgr
e un contact avec de leau ou de la transpiration. Jusqu a
pr
esent, la plupart des recherches ont port
e sur la composition et
les composants de produits de maquillage, et non sur le niveau de
imperm
eabilit
e. Cette
etude vise a  trouver des m
ethodes pour

evaluer le degr
e de r
esistance a leau des liners et mascaras et de
d
eterminer la pertinence de ces m
ethodes.


METHODES: Vingt sujets f
eminins ont
et
e s
electionn
es pour tester
la
etanch
eit
e des eye-liners, tandis que 20 ensembles de faux cils
ont
et
e utilis
es pour
evaluer l
etanch
eit
e de mascaras. Pour
evaluer
les propri
et
es de r
esistance a leau, les sites dessai ou les eye-liners
et mascaras ont
et
e appliqu
es ont
et
e immerg
es dans leau et au
s
echage naturel pendant plus de 20 min (pas de s
echage artificielle
par s
echoir, etc.). Les valeurs L * des eye-liners appliqu
es sur
lavant-bras avant et apres la immersions et les valeurs danalyse
dintensit
e de mascaras appliqu
es sur les faux cils ont
et
e utilis
ees
pour calculer le taux d
elimination moyen en pourcentage (WPR
%). Un produit a
et
e estim
e ^etre r
esistant a  leau si la valeur de la
moyenne du WPR%
etait inf
erieure ou
egal a 50%.


RESULTATS: Les liners non
etanches ne sont pas
etanches si leur
moyenne WPR%
etait sup
erieur a 50%, tandis que les eye-liners
dits imperm
eables a leau l
etaient si leur moyenne WPR%
etait
inf
erieure a 50%.
Pour les mascaras, le moyen WPR%
etait inf
erieur a  50% apres
1 a 2 h apres immersion dans leau a  la fois pour les produits non

etanches et imperm
eables. Apres 3 a  4 h, la moyenne WPR% pour
mascaras non-
etanches a  leau est sup
erieure a  50%, ce qui les
rend non
etanche, tandis que la moyenne WPR% des mascaras
waterproof est inf
erieure a  50%, ce qui les rend imperm
eable.
CONCLUSION: Nous avons
evalu
e les propri
et
es imperm
eables en
analysant les images photographi
ees avec des sites dessai o u les
eye-liners et mascaras ont
et
e appliqu
es. Les r
esultats de la compa-
raison entre les eye-liners et mascaras non
etanches et imperm
e-
ables, et les m
ethodes utilis
ees, en particulier, seront utiles pour

evaluer imperm
eabilit
e dautres produits de maquillage.
Introduction
Make-up, by definition, refers to activities involved in complementing
and/or modifying undesirable features of ones face or other body
parts, and enhancing features one is proud of with the intention of
beautifying the individual and adding to their personality. It is an
act pursuant to aesthetic values where cosmetics and other tools are
used to accentuate beautiful parts and where weak points and
Evaluation of waterproof effect for eyeliner and mascara
undesirable areas are modified or complemented. Generally, make-up
is divided into base make-up, involving evening out the overall com-
plexion or concealing flaws such as brown spots and freckles, and
spot make-up, where products are selectively applied to areas like the
lips, eyes or cheekbones to brighten the complexion and make them
appear more prominent. Point make-up is further composed of eye
and lip make-up. Among these, eye make-up is used to define the
eyes and leave a strong impression, and eyeliners, in particular, are
used to make the eyes look larger and more elongated, whereas mas-
caras are used to change or complement the shape of the eyes by
making the eyelashes appear longer and fuller [1, 2].
Depending on their composition, eye make-up products currently
available in the market are divided into waterproof (removable
with make-up remover, not with water), water-resistant (easily
washable with warm or soapy water) and non-descript types that
are susceptible to water and can easily be removed.
Eye make-up products, used mostly in summer, require water-
resistant properties as the colours in these products need to remain
adherent and should not smear off or washed away due to aquatic
activities or perspiration.
They should also meet safety and sanitary standards because eye
make-up products come in contact with the eyes. Additionally, they
should not irritate the eyes or cause allergic reactions [3].
To date, not much research has been performed to test the
waterproof of eye make-up products, and those that have have
focused on formulation or ingredients [4, 5], adverse reactions and
safety [69], and methods to test safety [10]. In particular, the
waterproofing composition and the test method for waterproof abil-
ity of mascara have been previously been described, for example in
United States 5 959 009 and WO 1992019215. Procter and Gam-
ble swirled in the pool of water while gently touching the lash
samples and used Max Factor Waterproof Cream Make-up and Max
Factor Whipped Cream Fluid Make-up (non-waterproof) to test
waterproof ability of their composition. In addition, Dempsey et al.
[11], in an attempt to develop semi-permanent mascaras, tested
the waterproof of mascara film by conducting blot tests.
For sun products, there have been a series of research efforts to
evaluate water resistance: the European Cosmetic, Toiletry and Per-
fumery Association (COLIPA) and the Ministry of Food and Drug
Safety (MFDS), Korea, presented a process with which the sun pro-
tection factor of water-resistant sun products was objectively mea-
sured. In this study, after referring to the Guideline for Evaluating
Sun Product Water Resistance (COLIPA, 2005.12) and Guideline
for Evaluating Sunscreen Product Water Resistance (KFDA,
2007.05), a method to test the waterproof of eyeliners and
mascaras was devised, and waterproof was evaluated by measuring
colour changes of eyeliners (L* value) and analysing colours of
mascaras (intensity value) generated from photographed images. In
addition, based on the scanning electron microscopy (SEM) study
on mascara films by Dempsey et al. [11] and Camacho-Bragado
et al. [12], SEM images were taken to compare the film surface of
mascaras before and after immersion in water. With the results,
the author tried to establish a method to evaluate the waterproof
of the eye make-up products concerned and assess its suitability.
Materials and methods
Subjects and materials
The study was conducted in accordance with the intent and pur-
pose of good clinical practice regulations, as described in Korean
2015 Society of Cosmetic Scientists and the Soci
et
e Francaise de Cosm
etologie
International Journal of Cosmetic Science, 38, 266271
M. J. Kim et al.
Good Clinical Practice (KGCP) and/or the Declaration of Helsinki,
as appropriate. All participants provided written informed consent
before the study initiation. All procedures for recruitment, selection
and inclusion of subjects in the study were established to provide
the participants with clear and precise information on the project
aims and the consequences of their consent.
Eyeliner is applied in a bilateral oculomucocutaneous manner in
the eyelid area, and mascara is applied to eyelashes. It is difficult to
be completely submerge the application sites in water. This study
included a total of 20 healthy Korean females aged 2143 (average
31.75
6.79) to evaluate the waterproof effect of eyeliner (applied
on the inner forearm skin). Exclusion criteria were as follows: (i)
subjects with any active skin disease, (ii) medication or past medi-
cal history that may affect skin response, (iii) pregnant or nursing
mothers, (iv) immunosuppression treatment within 3 months prior
(v) serious renal disorder or hepatic dysfunction and (vi) subjects
with aesthetic procedure (filler, botulinum toxin, laser).
We used 20 sets of false eyelashes (Clear Brown No. 7 Dolly eye,
ARITAUM, Korea) to evaluate the waterproof effect of mascaras.
We compared non-waterproof and waterproof eye make-up
products, to demonstrate that the methods fit the evaluations. The
products were selected from currently marketed eyeliners (1 non-
waterproof and 1 waterproof) and mascaras (1 non-waterproof and
1 waterproof). The comparative products were listed in Table I.
Methods
Water immersion procedure to evaluate waterproof effect: Water-
proof effect evaluation for eyeliners was with immersion using the
Whirlpool Model 4848C maintained at 28
2C. The test sites
were immersed in water for 20 min and dried for 20 min and the
process was repeated twice, to evaluate the waterproof effect of the
test product.
Waterproof effect evaluation for mascaras was with immersion
using the WiseCircu WBC-22 that circulated water at a constant
flow (5 L min1). The water temperature was maintained at 30C
and 40C during the experiment. For mascaras, the test sites were
immersed in water for 1, 2, 3 and 4 h and dried for 20 min.
Evaluation for waterproof effect of eyeliner: Randomization was
used to determine where the products were applied, and the inner
forearm of the subjects was rinsed and towel-dried. Twenty minutes
later, the products in question were applied on the test sites at
1.5 cm2 in dimension three times in a row. The eyeliner was
applied on the subjects inner forearm (1.5 cm2), and the applica-
tion was repeated thrice. The skin colour (L* value) was measured
by Spectrophotometer CM-2500d before, after application (drying
for 15 min) and after immersion (for 20 min twice) and natural
drying of eyeliners.
Table I Comparative eyeliner and mascara products
Manufacturer Product name Type
(a) Eyeliner
INNISFREE (Korea) Eco blush pen eyeliner Non-waterproof
INNISFREE (Korea) Powerproof blush liner Waterproof
(b) Mascara
MAYBELLINE (U.S.A.) Great lash lots of lashes Non-waterproof, Washable
MAYBELLINE (U.S.A.) Great lash Waterproof
267
Evaluation of waterproof effect for eyeliner and mascara M. J. Kim et al.

Evaluation for waterproof effect of mascara: The mascara was Table II The mean %WPR of eyeliner waterproof effect evaluation at water
applied on the upper and lower false eyelashes, and the applica- temperature of 28
2C
tion was repeated 30 times for overall application. We took
images of the false eyelashes using the Digital camera D90 Mean
(Nikon, Japan). The acquired images were analysed as intensity percentage
mean by Image-Pro plus before, after application (drying for waterproof d = t-value 3 Mean
15 min) and after immersion (for 1, 2, 3 and 4 h) and natural Type removal SD N t-value S/n %WPR
drying of mascaras.
Observation for surface of mascara films: We used scanning elec-
Non- 88.11 2.85 20 1.729 1.10 87.01
tron microscopy (SEM) to observe the change of mascara films waterproof
applied to false eyelashes. The false eyelashes were allowed to dry Waterproof 0.15 1.45 20 1.729 0.56 0.31
completely after application of mascara. Individual lashes were
adhered to an SEM sample stub with carbon tape. Samples were
lightly coated with gold before observation. We measured SEM
before, after application and after 4-hour immersion and natural
drying.

Percentage waterproof removal ratio (%WPR)

Test product data from subjects or false eyelashes were used in the
calculation of the mean percentage waterproof removal.
Percentage waterproof removal for each subject or false eyelash
was calculated as follows:

ACViw  ACViaa
Percentage Waterproof Removal i  100
ACViba  ACViaa
ACViba = individual analysed colour value before application.
ACViaa = individual analysed colour value after application.
ACViw = individual wet analysed colour value after water
immersion.
The 95% confidence interval for the mean percentage waterproof
removal ratio was calculated as:
[mean Percentage Waterproof Removal d]
mean Percentage Waterproof Removal Ratio (%WPR)
with d calculated as:
tS
d p
n in water for more than three hours to accurately evaluate their
S = standard deviation.
n = total number of subjects or false eyelashes in test.
t = n1 degree of freedom.
ex) n = 20, t = 1.729.
If the value for 95% lower unilateral confidence limit for the
mean %WPR was <50%, we concluded that the test product was
waterproof.
The acceptance criteria for waterproof testing referred the
Guideline for Evaluating Sunscreen Product Water Resistance.
Results
Analysis of skin colour for eyeliner waterproof effect
The result of L* value for non-waterproof eyeliner yielded the mean
%WPR as 87.01% and for waterproof eyeliner as 0.71% (Table II,
Figs 1, 2 ).
The mean %WPR of non-waterproof eyeliner was >50%; hence,
it was not waterproof. The mean %WPR of waterproof eyeliner
was <50% and, hence, was waterproof.
Figure 1 Changes of color (L* value) before, after application and after
immersion for 20 min twice of eyeliner on subjects inner forearm, n = 20.
Analysis of colour for mascara waterproof effect
At temperatures 30C and 40C at the 1- to 2-h marks after
immersion, the mean %WPR (0.0217.26%) for both non-water-
proof and waterproof mascaras was <50%, and from the 3-hour
mark onward, the mean %WPR (54.6857.92%) for non-water-
proof mascaras was >50%; hence, they were not waterproof,
whereas that (0.941.55%) of the waterproof mascaras was <50%
and hence were. This indicates that test sites need to be immersed
waterproof (Table III, Figs 3, 4).
In the meantime, no prominent change in mean %WPR was
noticed between non-waterproof and waterproof mascaras at the
two different temperatures of 30 and 40C.
Observation for surface of mascara films
The SEM image showed that the waterproof mascara film had a
smoother surface than the non-waterproof mascara film. Further-
more, the waterproof mascara film was unchanged without flaking
after 4-h immersion and natural drying, as compared to after appli-
cation. The non-waterproof mascara film had flaking after 4-h
immersion and natural drying (Fig. 5).
Discussion and Conclusion
In this study, we aimed to devise a method to evaluate the water-
proof of eyeliners and mascaras according to the Guideline for
Evaluating Sunscreen Product Water Resistance and checked for its
suitability. Non-waterproof and waterproof products were com-
pared, and with the level of confidence set at 95%, in case the

268 2015 Society of Cosmetic Scientists and the Soci
et
e Francaise de Cosm
etologie
International Journal of Cosmetic Science, 38, 266271
Evaluation of waterproof effect for eyeliner and mascara M. J. Kim et al.

(a)

(b)

Figure 2 Skin color images of eyeliner on subjects inner forearm (from left, before, after application and after immersion for 20 min twice) (a) non-waterproof
eyeliner, (b) waterproof eyeliner.

Table III The mean %WPR of mascara waterproof effect evaluation

Mean percentage
Type Time waterproof removal SD N t-value d = t-value 3 S/n Mean %WPR

(a) At water temperature of 30C

Non-waterproof 1H 4.63 9.74 20 1.729 3.77 0.86
2H 27.74 27.10 20 1.729 10.48 17.26
3H 59.10 11.44 20 1.729 4.42 54.68
4H 60.79 12.78 20 1.729 4.94 55.84
Waterproof 1H 1.24 3.14 20 1.729 1.22 0.02
2H 1.87 3.72 20 1.729 1.44 0.43
3H 1.69 1.92 20 1.729 0.74 0.94
4H 2.07 2.16 20 1.729 0.84 1.23

(b) At water temperature of 40C

Non-waterproof 1H 40.04 5.19 20 1.729 2.01 38.03
2H 43.49 3.88 20 1.729 1.50 41.99
3H 57.24 3.83 20 1.729 1.48 55.76
4H 58.18 0.68 20 1.729 0.26 57.92
Waterproof 1H 1.56 3.05 20 1.729 1.18 0.38
2H 3.62 6.76 20 1.729 2.61 1.01
3H 1.66 0.42 20 1.729 0.16 1.50
4H 3.12 4.06 20 1.729 1.57 1.55

mean %WPR was <50%, the products concerned were considered

waterproof. The acceptance criteria for waterproof testing referred
the guideline by KFDA.
The results indicate that after two consecutive immersions for
20 min at 28
2C, there were discrepancies in eyeliner mean %
WPR between waterproof and non-waterproof products, whereas no
discrepancy in mascara was exhibited between waterproof and non-
waterproof products when they were immersed for 20 min consecu-
tively at 30C (data not presented). This may be due to the fact that
most commercial non-waterproof mascaras are splash resistant and
washable, making them unlikely to be removed with room tempera-
ture water, but with soapy or lukewarm water instead. Taking this
into consideration, additional tests on the same mascaras were con- Figure 3 Changes of color (Intensity) before, after application and after 1,
ducted at 30 and 40C at 1-, 2-, 3- and 4-h marks. 2, 3 and 4 h immersion of false eyelashes with mascara, n = 20.

2015 Society of Cosmetic Scientists and the Soci
et
e Francaise de Cosm
etologie 269
International Journal of Cosmetic Science, 38, 266271
Evaluation of waterproof effect for eyeliner and mascara M. J. Kim et al.

(a)

(b)

Figure 4 False eyelash color images of mascara with casmatch at 30C (from left, before, after application, after 1, 2, 3 and 4 h immersion) (a) non-water-
proof mascara, (b) waterproof mascara.

(a)

(b)

Figure 5 SEM images of mascara films with false eyelashes at 30C (from left, before, after application, after 4 h immersion) (a) non-waterproof mascara, (b)
waterproof mascara.

The mean %WPR of waterproof eyeliner was negative value,
and the data result from eyeliner film change by swelling and
shrinking in water. The relation of sample gloss, texture change
and colour has been reported [13, 14].
At 30 and 40C temperatures from the 3-h mark onward in
mascara, the mean %WPR for non-waterproof mascaras was
>50%, whereas that of the waterproof mascaras was <50%. The
acceptance criteria, 50%, accorded with this study, because the
mean % WPR of both types of product changed little after 3-h
mark. For confirming reliability of the study, it requires checking at
additional time points. Also, the study was conducted on limited
make-up products, so it needs supplementary studies using a num-
ber of make-up products and samples.
In conclusion, the mean %WPR for non-waterproof eyeliners
and mascaras after 34 h into immersion was >50%, rendering
them not waterproof, whereas the mean %WPR for waterproof
eyeliners and mascaras was <50%, making them waterproof. In
addition, the non-waterproof products in question are likely to
demonstrate higher mean %WPR if they are immersed in water for
a prolonged period of time.
In this study, the authors came up with a way to evaluate
the waterproof of eyeliners and mascaras, and by comparing
non-waterproof and waterproof products, its method was pro-
ven appropriate. This study is expected to be a useful tool for
evaluating waterproof for a variety of make-up products in the
future with varying immersion durations and water tempera-
tures.
Acknowledgement
This study was sponsored by DERMAPRO LTD., the authors being
full-time employees of the company.

270 2015 Society of Cosmetic Scientists and the Soci
et
e Francaise de Cosm
etologie
International Journal of Cosmetic Science, 38, 266271
Evaluation of waterproof effect for eyeliner and mascara
References
1. Butler, H. Pouchers Perfumes, Cosmetics and
Soaps, 10th edn. Kluwer Academic Publish-
ers 151165, 167216 (2000).
2. Dempsey, J.H., Fabula, A.M., Rabe, T.E.,
Lubbers, J.M. and Ye, M. Development of a
semi-permanent mascara technology. Int. J.
Cosmet. Sci. 34, 2935 (2012).
3. Boughton, P. and Hughes, M.E. The Buyers
Guide to Cosmetics. pp. 5578. Random
House, New York (1981).
4. Bui, H.S., Kanji, M., Li, C. and Bavouzet,
B. Long wear, waterproof mascara compo-
sition with water washability. U.S. Patent
8,597,626 (2013).
5. Bavouzet, B.T., Bui, H.S., Kanji, M. and Li, C.
Long-wear and water resistant mascara com-
position enhancing volume and shine. U.S.
Patent Application 12, 825,599 (2010).
2015 Society of Cosmetic Scientists and the Soci
et
e Francaise de Cosm
etologie
International Journal of Cosmetic Science, 38, 266271
6. Fisher, A.A. Allergic contact dermatitis due
to rosin (colophony) in eyeshadow and mas-
cara. Cutis 42, 507508 (1988).
7. Pascher, F. Adverse reactions to eye area
cosmetics and their management. J. Soc.
Cosmet. Chem. 33, 249 (1982).
8. Ng, A., Evans, K., North, R. and Purslow, C.
Eye cosmetic usage and associated ocular
comfort. Ophthalmic Physiol. Opt. 32, 501
507 (2012).
9. Malik, A. and Claou
e, C. Transport and
interaction of cosmetic product material
within the ocular surface: beauty and
the beastly symptoms of toxic tears. Cont.
Lens and Anterior Eye, 35, 247259
(2012).
10. Thomason, H. and Montagnes, D.J. Devel-
oping a quick and inexpensive in vitro
M. J. Kim et al.
(non-animal) bioassay for mascara irrita-
tion. Int. J. Cosmet. Sci. 36, 134139
(2014).
11. Dempsey, J.H., Fabula, A.M., Rabe, T.E.,
Lubbers, J.M. and Ye, M. Development of a
semi-permanent mascara technology. Int. J.
Cosmet. Sci. 34, 2935 (2012).
12. Camacho-Bragado, G.A., Dixon, F.M. and
Zaluzec, N.J. An ESEM study of the influence
of humidity on the integrity of mascara
films. Microsc. Microanal. 15, 682683
(2009).
13. Edul, N.D. and Kristen, M.N. The effect of
Gloss on Color. Color Res. Appl. 24, 369
376 (1999).
14. Lionel, S. and Mady, E. Color change due to
surface state modification. Color Res. Appl.
28, 4549 (2003).
271