International Journal of Cosmetic Science, 2016, 38, 389–398
12302
Comparison between sensory and instrumental characterization
of topical formulations: impact of thickening agents
M. Estanqueiro, M. H. Amaral and J. M. Sousa Lobo
Laboratory of Pharmaceutical Technology, Department of Drug Sciences, Faculty of Pharmacy, University of Porto, Porto, Portugal
Received 17 September 2015, Accepted 15 December 2015
Keywords: adhesiveness, firmness, rheology, sensorial analysis, spreadability, thickeners
Abstract
OBJECTIVE: Sensorial properties of cutaneous formulations are
important in determining their acceptability by consumers. However,
sensorial analysis is time-consuming and requires an available panel
of trained assessors. Thus, this article aimed to study the impact of
thickening agents on mechanical properties of creams and investi-
gate how these measurements could correlate the sensory attributes
using a combined instrumental–sensorial approach.
METHODS: For this purpose, eight semisolid formulations were
prepared, containing in their composition different thickening
agents at different concentrations. These formulations were firstly
microscopically observed and then assayed through textural, rheo-
logical and spreadability measurements. Textural characterization
and rheological characterization were performed during six months
to assess the physical stability of the studied formulations. Finally,
six sensory attributes, namely firmness, adhesiveness, cohesiveness,
spreadability, consistency and adhesiveness post-application, were
tested by a trained panel.
RESULTS: It was observed that thickening agents influence the
microstructure of semisolid emulsions and also their mechanical
properties. In general, an increase in the concentration of thicken-
ing agents improves the physical stability of formulations over
time. Besides, textural parameters (firmness and adhesiveness), vis-
cosity and difficulty to spread also increase. A good correlation
between mechanical characterization and sensorial analysis was
verified, mainly for spreadability properties.
CONCLUSION: With the obtained results, it is possible to conclude
that the proposed methods for mechanical characterization can be
correlated with sensorial perception obtained from volunteers,
representing a faster and less expensive alternative than sensory
analysis.
Re
sume
problems related with the formulation and production of these
OBJECTIF: Les propri
et
es sensorielles des formulations cutan
ees
sont importantes pour d
eterminer leur acceptabilit
e par les consom-
mateurs. Cependant, l’analyse sensorielle prend beaucoup de temps
et n
ecessite un panel d’
evaluateurs qualifi
es disponibles. Ainsi, ce
travail vise a 
etudier l’impact des agents
epaississants sur les pro-
pri
et
es m
ecaniques de cremes et d’enqu^eter sur la facßon dont ces
mesures pourraient corr
eler avec les attributs sensoriels utilisant
une approche combin
ee instrumentale-sensorielle.
Correspondence: Marilene Estanqueiro, Rua de Jorge Viterbo Ferreira,
n.°228, 4050-313 Porto. Tel.: +351 220 428 500; fax: +351 226
093 390; e-mail: msrestanqueiro@ff.up.pt
© 2015 Society of Cosmetic Scientists and the Soci
et
e Francßaise de Cosm
etologie
doi: 10.1111/ics.
METHODES: A cet effet, huit formulations semi-solides ont
et
e
pr
epar
ees, contenant dans leur composition des agents
epaississants
diff
erents a diff
erentes concentrations. Ces formulations ont d’abord

et
e observ
es au microscope puis
evalu
ees par des mesures de tex-
ture, de rh
eologie et de l’
etalement. Les caract
erisations texturales
et rh
eologiques ont
et
e effectu
ees au cours de six mois afin
d’
evaluer la stabilit
e physique des formulations
etudi
ees. Enfin, six
attributs sensoriels, a savoir, la fermet
e, l’adh
erence, la coh
esion,
l’
etalement, la coh
erence et l’adh
erence apres l’application, ont
et
e
test
es par un panel form
e.
RESULTATS: On a observ
e que des agents
epaississants influencent
la microstructure des
emulsions semi-solides ainsi que leurs pro-
pri
et
es m
ecaniques. En g
en
eral, une augmentation de la concentra-
tion d’agents
epaississants am
eliore la stabilit
e physique dans le
temp des formulations. En outre, les parametres de texture (fermet
e
et adh
erence), de viscosit
e et de difficult
e d’
etalement augmentent

egalement. Une bonne corr
elation entre la caract
erisation m
ecani-
que et l’analyse sensorielle a
et
e v
erifi
ee, principalement pour les
propri
et
es d’
etalement.
CONCLUSION: Avec les r
esultats obtenus, il est possible de con-
clure que les m
ethodes propos
ees pour la caract
erisation m
ecanique
peuvent ^etre corr
el
ees avec la perception sensorielle obtenue par
des b
en
evoles, ce qui repr
esente une alternative plus rapide et
moins co^ uteuse que l’analyse sensorielle.
Introduction
The common semisolid formulations for cutaneous application
include ointments, pastes, gels and creams. However, for skin
care, the most used and appreciated formulations are creams,
more precisely, hydrophilic creams. One of the most complicated
preparations is the establishment of reliable techniques for their
characterization, mainly due to the complexity of their physical
structure [1]. Consumer preference for such products depends on
various properties of the product, including, appearance, odour,
extrudability (when applicable), spreadability, adhesiveness and
residual greasiness after application [2]. In summary, the accept-
ability and efficacy of topical products require that they have opti-
mal mechanical properties (firmness), adequate rheological
behaviour (pseudoplastic behaviour with tixotropy) and appropri-
ate adhesion [3].
The sensation produced by the application on the skin is one
of the most important properties of cutaneous products in addition
389
Sensory and instrumental evaluation of creams
to the long-term physical stability and physiological effect [4].
Sensory properties in skin care formulations mainly result from
ingredients such as emollients, rheology modifiers, emulsifiers and
humectants [5].
Sensory profiling of cosmetic products is a powerful tool for the
cosmetic industry as it provides relevant information for the
development and marketing of new products, the reformulation of
existing products and the optimization of manufacturing process.
However, this evaluation is time-consuming and requires an avail-
able and well-trained panel of assessors and sometimes does not
afford clear-cut results [6].
As an alternative to sensory evaluation, objective evaluation
methods by means of instrumental measurements have been stud-
ied [4]. Rheological analysis can be employed to develop a suitable
product for skin application [7]. Rheological evaluation is usually
taken to predict the behaviour of the product in real-time condi-
tions, namely during manufacturing, packaging and skin applica-
tion. Textural analysis can be applied for several purposes;
however, in the field of formulation development, it is mainly used
to characterize the mechanical properties of topical formulations
[8]. In particular, texture properties of a topical formulation during
application are known of great importance because the consumers’
preference is closely connected to the texture properties of the
product [9].
Water dispersible polymers have a remarkable contribution in
texture properties of topical formulations. These hydrophilic poly-
mers, also called texturing agents, are widely used as thickeners
and rheology modifiers, but also as stabilizers [10]. These effects
have been studied as a function of the nature and concentration of
polymers, by various authors [11–15].
A challenge prospect continues to be relate to the instrumental
measurements with the sensorial evaluation, and based on this
idea, some studies were made. Some of these studies have focused
on the effect of lipid components on mechanical and sensorial prop-
erties of creams and emulsions [5, 16, 17]. Other works evaluated
the effect of different thickening agents, but using the same concen-
tration of each one [18, 19].
The aim of this work was to compare instrumental characteriza-
tion with sensorial evaluation of semisolid formulations composed
by different thickening agents used in different concentrations.
Materials and methods
Materials
Raw materials
For the preparation of formulations, the following excipients
commonly used in cosmetic products were used. Sodium car-
boxymethylcellulose, xanthan gum and imidurea were purchased
from Guinama (Spain). Carbopolâ934 and niacin were purchased
from Vaz Pereira (Portugal). Lanetteâ SX (ceteary alcohol, sodium
lauryl sulphate and sodium cetearyl sulphate), jojoba oil and
mineral oil were obtained from Acofarma; and glycerine was
obtained from Fagron (Spain). Carbopolâ 980 and Lipocireâ A SG
(C10–C18 triglycerides) were kindly provided by Lubrizol (U.S.A.)
and Gattefoss
e (France), respectively.
Preparation of the formulations
Carbomers, sodium carboxymethylcellulose and xanthan gum were
the thickening agents studied in this work at different concentra-
tions, namely 0.25%, 0.5% and 1.0% (w/w).
390 © 2015 Society of Cosmetic Scientists and the Soci
et
e Francßaise de Cosm
etologie
M. Estanqueiro et al.
The creams were prepared by varying the thickening agent com-
position and concentration, as shown in Table I. The formulations
FC7, FC8, FC10 and FC11 including in their composition 0.5%
w/w (FC7) and 0.25% w/w (FC8) of xanthan gum and 0.5% w/w
(FC10) and 0.25% w/w (FC11) of sodium carboxymethylcellulose
were also prepared. However, these formulations presented an
extremely fluid consistency and were excluded from this study. Fur-
thermore, formulation FC10 showed phase separation after three
months of preparation.
Methods
Microscopic analysis
All the studied formulations were microscopically observed using
an optic microscope Nikon Eclipse E400 (Tokyo, Japan), with a
magnification of 4009, and images were captured by an attached
Nikon Coolpix MCD camera (Tokyo, Japan).
Rheology
Rheological analysis was performed on a rotational viscometer
HAAKE Viscotester 550 (Thermo Scientific, Germany), with a
coaxial cylinder sensor SV-DIN. The flow behaviour was studied
by continuous shear investigations, which were performed to
evaluate the shear stress (Pa) as a function of shear rate (s
1).
The study started with a shear rate of 1 s
1 up to a maximum
of 500 s
1 and back to 1 s
1, and the resulting shear stress
was measured. To reduce the influence of temperature on the
rheological behaviour, a thermostatic water bath was used to
accurately maintain the sample temperature (20°C) during all
experiments. The rheological analysis was performed one week,
and one, three and six months after the formulations prepara-
tion, to elucidate about the mechanical stability of the creams
with time.
The flow curves were obtained, and Hershey–Berkeley, Cross,
Carreau, Power law, Bingham and Newton models were tested to
describe the flow behaviour. The Carreau model (equation 1)
resulted in better fittings [20]. The quality of fit was evaluated from
the determination coefficient (R2) and from the sum of squared
residues (SSR).
ðg
g1 Þ
gap ¼ g1 þ h 0 iN ð1Þ
_ c_ c Þ2
1 þ ðc=
where gap is the apparent viscosity (Pa.s), g0 and g∞ are the zero-
shear rate and the infinite-shear rate viscosity (Pa.s), c_ is shear rate
(s
1) and c_ c is the critical shear rate (s
1), and N is a dimensionless
constant (zero for Newtonian fluids).
Textural analysis
Textural analysis was performed using a texturometer (Stable
Micro Systems, TA-XT2i, London, U.K.) by carrying out a penetra-
tion test using a load cell of 5 kg, a cylindrical probe with
13 mm diameter, a penetration depth of 3 mm, test speed of
3 mm s
1 and a trigger force of 0.049 N. The texture apparatus
is equipped by a probe connected to an engine that enables verti-
cal probe displacement. After penetrating the sample, the probe
returned to the initial position. From the obtained graph force vs.
distance, the maximum force (firmness) and the negative area
(adhesiveness) were calculated. All the measurements were taken
in triplicate, at room temperature. The textural analysis was
International Journal of Cosmetic Science, 38, 389–398
Sensory and instrumental evaluation of creams M. Estanqueiro et al.

Table I Composition of the developed formulations (%, w/w)

Ingredients FC1 FC2 FC3 FC4 FC5 FC6 FC9 FC12

Oil phase
Cetearyl alcohol, sodium lauryl 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5
sulphate and sodium cetearyl
sulphate
Jojoba oil 7.5 7.5 7.5 7.5 7.5 7.5 7.5 7.5
Mineral oil 7.5 7.5 7.5 7.5 7.5 7.5 7.5 7.5
C10–C18 triglycerides 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0
Aqueous phase
Niacin 3.5 3.5 3.5 3.5 3.5 3.5 3.5 3.5
Glycerine 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0
Carbopolâ980 0.5 0.25 1.0
Carbopolâ 934 0.5 0.25 1.0
Xanthan gum 1.0
Sodium carboxymethylcellulose 1.0
Imidurea 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2
Water q.s.100 q.s.100 q.s.100 q.s.100 q.s.100 q.s.100 q.s.100 q.s.100

performed one week, and one, three and six months after prepara- Table II Description of attributes evaluated in sensorial analysis, by
tion of formulations by the same reason mentioned to the rheol- category
ogy study.
Category Parameter Definition
Spreadability
The spreadability was evaluated according to previous studies [17,
21]. Briefly, 1 g of each formulation was placed at the centre of a Pick-up
glass plate. This plate was covered with another glass plate with Attributes measured by Firmness Force required to fully compress
the same size. Next, a weight of 200 g was carefully applied on the manipulation between product between thumb and index
fingers finger.
upper face of the plate. After one minute, the weight was removed
Adhesiveness Force required to separate fingertips.
and the diameter of the spread area (cm) was measured. The Cohesiveness Amount of sample that strings rather
measurements were taken in triplicate. than breaks when fingers are
separated.
Sensorial analysis During rubbing
A panel of 12 volunteers (average age 22.3  1.7 years old) of Attributes measured by Spreadability Ease of moving the product over
rubbing the product the skin.
both sexes, without dermatological diseases, recruited based on
on the skin Consistency Amount of product felt between
their interest, availability to participate in this study and capability fingertip and skin.
to use rating scales were enrolled, after giving their informed con- After feel
sent. Assessors were first introduced to the general concept of the Attributes of the skin Adhesiveness Degree to which fingers adhere to
study, following a detailed explanation about the test and sensorial surface after the use product residue.
of a product
parameters definition, and for each tested attribute, the procedure
and scale were demonstrated with references. The standard materi-
als as well as the definitions and scales were adapted from the
ASTM E1490 Standard Guide for sensory descriptive analysis of
creams and lotions [22]. measuring the distance from the mark made by the panellist to the
The test was conducted in a room with controlled temperature 0 cm extreme.
and relative humidity and good light conditions. For the pick-up The definitions of the parameters evaluated by category are
category, 0.1 g of each product was compressed between the index presented in the Table II.
finger and thumb and the firmness, adhesiveness and cohesiveness
were evaluated. In the during rubbing category, 0.1 g of the pro- Statistical analysis
duct was gently spread within a circle with 5 cm diameter, marked Whenever applicable, the results were presented as a mean  stan-
in the forearm, at a rate of two strokes per second. The spreadabil- dard deviation. The statistical analysis was performed using the
ity was evaluated after three rubs, and the consistency was evalu- software SPSSâ Statistics version 22.0 (IBMâ Corporation, Armonk,
ated after 12 rubs. In the after feel category, adhesiveness was Westchester, New York, U.S.A.). The results were checked for their
evaluated by soft beats with fingers in the residue of the product normality and homogeneity of variances and then an ANOVA test
previously applied on the forearm. The products to be tested were was applied. Pearson’s correlation coefficients were calculated
evaluated using intensity scales, anchored in the extremes with between mechanical and sensorial parameters. The results were
directional terms (e.g. easy/difficult). Scores were calculated by considered significant when P < 0.05.

© 2015 Society of Cosmetic Scientists and the Soci
et
e Francßaise de Cosm
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Sensory and instrumental evaluation of creams M. Estanqueiro et al.

monodisperse microstructure of the oil droplets, while the

Results and discussion
Microscopic analysis
Representative optical microphotographs of the eight prepared
creams are presented in Fig. 1.
Regarding the obtained images, it is possible to verify that in
the case of creams containing carbomers, increasing the polymer
concentration there is a decrease in droplets size. Thus, creams
with smaller droplets are FC3 and FC6 that also exhibit
remaining formulations present heterogeneity in terms of droplets
size. The droplet size of multiphasic formulations is strongly
dependent on the emulsifier system. As in this case, the primary
emulsifier is the same in all formulations, and the difference
visualized in internal structure may be caused by the secondary
emulsifiers or thickeners, that is the polymers dispersed in
external phase. Additionally, the droplet size can influence the
physical stability and the mechanical properties of emulsions and
creams [23, 24].

Figure 1 Optical microphotographs of the eight formulations at a magnification of 4009.

392 © 2015 Society of Cosmetic Scientists and the Soci
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International Journal of Cosmetic Science, 38, 389–398
Sensory and instrumental evaluation of creams
Rheology
The knowledge about mechanical properties of topical formulations,
namely the rheological behaviour, is useful to predict their spread-
ing capacity on the skin [25]. Continuous shear experiments mea-
sure the ability of each system to resist to structural breakdown
during its exposure to shear. In the present work, the flow beha-
viour of the eight creams was analysed, during six months, after
their production and shear stress vs. shear rate plots obtained. Fig-
ure 2 presents the rheological behaviour of each formulation dur-
ing the analysis period.
All the formulations exhibited a classical shear-thinning or
pseudoplastic behaviour, which means that increasing the shear
rate, the apparent viscosity decreases. As can be seen in the
plots, the shear rate increases faster than the shear stress, which
results in a concave curve in relation to the horizontal axis. The
pseudoplastic behaviour is preferable for products intended for
cutaneous application and is also the most common, which
means that these can break down to spread easily on the skin
[26, 27]. Marty and co-workers compared the rheological char-
acterization of ointments with patient’s acceptability and found
that those with shear-thinning behaviour are also preferred by
patients [28].
Additionally, some formulations showed thixotropy, a reversible
decrease in viscosity with force application time. The formulations
with higher concentration of carbomer (1%, w/w), that is FC3 and
FC6, and the formulation with 0.5% (w/w) of Carbopolâ 980 (FC1)
exhibited higher thixotropy. Thixotropy is an important feature for
topical application. When the formulation is submitted to a shear
Figure 2 Shear stress as a function of shear rate of each formulation, evaluated after one week (a), one month (b), three months (c) and six months (d) of
storage at 20°C.
© 2015 Society of Cosmetic Scientists and the Soci
et
e Francßaise de Cosm
etologie
International Journal of Cosmetic Science, 38, 389–398
M. Estanqueiro et al.
stress, its network structure breaks down, leading to a gradual
viscosity decrease to spread easily on skin, and when the force is
removed, the viscosity recovers slowly, keeping the formulation on
the skin [29].
Considering the creams containing carbomers in their external
phase, an increase in shear stress values was observed while
increasing the carbomer concentration. For the same concentra-
tion (1%, w/w) of the different polymers, the cream with Car-
bopolâ 980 showed the highest values of shear stress whereas
the formulation with xanthan gum presented the lower values.
It was expected that formulations containing Carbopolâ980
exhibited higher shear stress because these polymers originate
more viscous solutions in comparison with Carbopolâ934,
according to the technical data from manufacturer. Additionally,
in a previous study performed by our group, formulations con-
taining 0.5% (w/w) of Carbopolâ 980 showed higher shear
stress values than similar formulations containing Carbopolâ 934
[30]. According to graphs observation, no substantial changes
with time were observed.
Table III shows the rheological parameters of the Carreau model
for the semisolid formulations, one week and six months after their
preparation.
Viscosity values at zero shear increased while increasing polymer
concentration. FC3 showed a considerable increase in this parame-
ter after six months of storage. For some formulations, the parame-
ter infinite-shear rate viscosity resulted in negative values during
fitting. For all formulations, the obtained values of N are >0,
because we are in the presence of non-Newtonian systems, with
semisolid consistency.
393
Sensory and instrumental evaluation of creams M. Estanqueiro et al.

Table III Rheological parameters of the Carreau model, calculated for each formulation after one week and six months of preparation

One week Six months

Code g0 g∞ N R2 SSR g0 g∞ N R2 SSR

FC1 1287.6 0.884 0.425 0.9999 3.510 1287.6 1.030 0.429 0.9997 7.214
FC2 1284.2 0.282 0.431 0.9997 2.092 1284.1
0.132 0.417 0.9996 3.160
FC3 1338.3 1.594 0.432 0.9998 11.626 11259.1 2.621 0.452 0.9994 45.779
FC4 1323.3
0.156 0.403 0.9989 13.118 1315.0
1.507 0.333 0.9944 51.908
FC5 1302.2
0.375 0.351 0.9983 4.416 1293.8
0.710 0.331 0.9949 12.627
FC6 2262.7 2.033 0.456 0.9997 43.959 2259.7 1.070 0.422 0.9999 10.620
FC9 2319.0 0.460 0.429 0.9997 0.890 2318.7 0.365 0.424 0.9995 1.187
FC12 2317.4
1.108 0.321 0.9997 5.584 2326.5
1.989 0.317 0.9995 17.249

Textural analysis spreadability given by the diameter of the spread area after applica-
tion of a weight of 200 g to the upper face of a glass plate.
Textural analysis is a multidisciplinary approach with applicability
From box-plot analysis is possible to see that the formulation
in many different fields; however, cosmetic and pharmaceutical
with better spreadability is FC5, with an average diameter of
application has gained increased attention. Through a force vs.
8.1 cm. FC5 is followed by FC2, FC4, FC1 and FC9. According to
distance graph obtained from the performed penetration test, tex-
the obtained results, the formulations with poor spreadability are
tural parameters such as firmness and adhesiveness can be
FC12, FC6 and FC3. In the case of formulations composed by car-
derived. Firmness is a textural property defined as the necessary
bomers, it is interesting to see that formulations containing higher
force to reach a given deformation and can be related to the ease
concentration of polymer present poor spreadability, and this
of application to the skin. Adhesiveness is the work required to
parameter improves with a decrease in the concentration. Formula-
overcome the attractive forces between the surface of the sample
tions composed by Carbopolâ 934 (FC4, FC5, FC6) showed better
and the surface of the probe. Formulations for cutaneous applica-
spreadability than the corresponding formulations with Carbopolâ
tion should exhibit good firmness and adhesiveness. Figure 3 is a
980 (FC1, FC2, FC3).
graphical representation of the values obtained from textural
analysis performed one week, and one, three and six months after
preparation. Sensorial analysis
Through visual analysis of graphs, it can be seen that the for-
Figure 5 represents the obtained sensorial profile of the eight stud-
mulations that stand out due to their higher values of firmness are
ied formulations.
FC6 and FC3, with 1% (w/w) of Carbopolâ 934 and 980, respec-
Significant differences between the studied formulations were
tively. On the other hand, the formulations with lower values of
observed for all the sensory attributes, with exception of cohesive-
firmness are FC5, with 0.25% of Carbopolâ 934, and FC9 with
ness for which no significant differences were observed. The
1.0% of xanthan gum. Regarding stability, formulations FC1, FC4
formulation FC6 presents higher firmness and is followed by FC1,
and FC9 were the more stable because they do not undergo signifi-
FC3, FC4, FC12 and FC2. The formulations FC9 and FC5 present
cant variations in firmness over six months. FC3, FC5 and FC6
lower firmness; however, statistical differences only exist in relation
have experienced a significant change in firmness after one month;
to FC6. A similar observation is made regarding the adhesiveness
nevertheless, they remain stable during the remaining period of
during pick-up category, as the FC6 and FC3 are the most adhesive
time.
and FC5 is the lowest adhesive. Regarding ‘during rubbing’ cate-
FC12 showed the highest values of adhesiveness, followed by
gory and considering spreadability, volunteers attributed a greater
FC6 and FC3 and, similarly to what happened in the case of firm-
score which means easy spreadability, to FC5 formulation, that is
ness, FC5 and FC9 showed the lower values of this textural param-
statistically significant in comparison with FC3, FC6 and FC12
eter. Only FC4 suffered a small but significant variation in
which present poor spreadability under the skin. Considering
adhesiveness over the six months.
consistency, a significant difference was observed for FC5, which
exhibited lower consistency in comparison with FC6 and FC12,
considered as the most consistent formulations. Regarding after feel
Spreadability
category, FC5 was that with lower scores of adhesiveness, present-
Spreadability indicates the area on which a semisolid formulation ing significant differences in relation to FC3, FC6, FC9 and FC12.
for cutaneous application spreads during application on the skin, These latter provided a greater feeling of adhesiveness after applica-
which means that a greater area corresponds to a better spread- tion on skin.
ability. This feature is of great importance for cutaneous products, As the aim of this study was to compare the instrumental
influencing both efficacy and consumer acceptability. For example, measurements with sensory analysis, the correlation matrix of the
poor spreadability may result in an irregular distribution of the sensory and instrumental values was obtained as reported in
product, affecting the applied dose and for consumers is a weakness Table IV. For these calculations, values of firmness, adhesiveness
of the product [17]. Figure 4 is a box-plot with the results of and viscosity determined after one week were considered.

394 © 2015 Society of Cosmetic Scientists and the Soci
et
e Francßaise de Cosm
etologie
International Journal of Cosmetic Science, 38, 389–398
Sensory and instrumental evaluation of creams M. Estanqueiro et al.

Firmness
0.25

0.2

Fmáx (N) 0.15 One week

0.1 One month

Three months
0.05
Six months
0
FC1 FC2 FC3 FC4 FC5 FC6 FC9 FC12
Formulations

Adhesiveness
0
–0.1 FC1 FC2 FC3 FC4 FC5 FC6 FC9 FC12
–0.2
–0.3 One week
A(–) (N*mm)

–0.4 One month

–0.5
Three months
–0.6
–0.7 Six months
–0.8
–0.9
–1
Formulations
Figure 3 Results of firmness and adhesiveness of the formulations evaluated one week, and one, three and six months after preparation (mean values  SD,
n = 3).

It is possible to observe that the parameter firmness determined

through textural analysis appears to be significantly correlated with
the sensorial attributes of firmness (Pearson coefficient 0.610) and
spreadability (Pearson coefficient
0.843). The obtained values
were expected as firmness can be related to the ease of spreading
and a product with higher firmness is more difficult to spread,
thence the negative correlation coefficient observed in the case of
spreadability. From the obtained results, FC6 showed higher values
of firmness either in textural analysis or in sensorial evaluation,
while FC5 and FC9 showed the lower values in both approaches.
Additionally, the higher the necessary force to reach a given defor-
mation, the poorer the spreadability, and thus, the formulations
with higher firmness exhibited poor spreadability and vice versa.
Although visually it seems to have some similarity between the
results of adhesiveness instrumentally determined and the sensorial
parameters of adhesiveness and adhesiveness post-application, no
statistical correlation were obtained as would be expected. How-
ever, this parameter presented a significant negative correlation
with spreadability (Pearson coefficient
0.617) and a significant
correlation with consistency (Pearson coefficient 0.545), which
means that the higher the attractive forces between the skin and Figure 4 Results of spreadability given by the diameter of the spread area
the formulation, the greater the difficulty in spreading the after applying a mass of 200 g (n = 3).

© 2015 Society of Cosmetic Scientists and the Soci
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Sensory and instrumental evaluation of creams M. Estanqueiro et al.

Firmness
10

Adhesiveness Post - 6 FC1

Adhesiveness
applicaon
4 FC2
FC3
2
FC4
0 FC5
FC6
FC9
FC12
Consistency Cohesiveness

Spreadability

Figure 5 Sensory profile of the eight formulations (mean values).

Table IV Correlation matrix (Pearson coefficients) of the sensory and instrumental values of the studied formulation

FI AI SI VI FS AS CS SS ConsS ApS

Instrumental parameters
Firmness (FI) 1.00 – – – – – – – – –
Adhesiveness (AI) 0.562** 1.00 – – – – – – – –
Spreadability (SI)
0.596**
0.843** 1.00 – – – – – – –
Viscosity at 500s
1 (VI) 0.959** 0.762*
0.682 1.00 – – – – – –
Sensory attributes
Firmness (FS) 0.610** 0.395
0.534** 0.326 1.00 – – – – –
Adhesiveness (AS) 0.239 0.235
0.521** 0.180 0.699** 1.00 – – – –
Cohesiveness (CS)
0.101 0.182
0.455* 0.089 0.280** 0.633** 1.00 – – –
Spreadability (SS)
0.843**
0.617** 0.665**
0.871**
0.514**
0.400**
0.279** 1.00 – –
Consistency (ConsS) 0.392 0.545**
0.565** 0.875** 0.364** 0.426** 0.344**
0.322** 1.00 –
Adhesiveness post-application (ApS) 0.252 0.391
0.673** 0.548 0.323** 0.436** 0.565**
0.434** 0.406** 1.00

*Significance at P < 0.05.

**Significance at P < 0.01.

formulation on the skin, and the greater the amount of formulation
perceived. The mechanical determination of spreadability by the
proposed method, although fallible and not completely simulate the
sensory assessment, showed good correlation with all the sensory
attributes studied. According to the obtained values of Pearson
coefficients, it is possible to conclude that the formulations with
better spreadability (larger diameter of the spreading area) exhibit
lower firmness, adhesiveness, cohesiveness, consistency and adhe-
siveness post-application. Additionally, a positive correlation was
obtained between mechanical and sensorial evaluation of spread-
ability. The formulation which obtained better scores of spreadabil-
ity in both methods was FC5 that also exhibit lower values in all
the sensory attributes evaluated. The values of viscosity are propor-
tional to consistency and, consequently, inversely proportional to
spreadability. Technologically, consistency can be defined as the
capacity of a product to resist to a deformation promoted by a force
or pressure and can be evaluated by viscometry, among other
methods. Thus, the higher the apparent viscosity values, the
greater the consistency and the difficulty in spreading.
In sum, the techniques described to study the mechanical char-
acterization of semisolid formulations showed a good correlation
with the sensory attributes studied, which are important to the
acceptance of a semisolid product. In the work developed by Gilbert
et al., [19] despite being accessed other variables, texture and rheo-
logical analysis were also reported as excellent tools to predict sen-
sory attributes of formulations, as can also be seen in the present
work. Effectively, texture properties and rheological behaviour
constitute two approaches that can be used to characterize topical
formulations, and the obtained results can be correlated with sen-
sory properties important for consumer acceptance. Furthermore,

396 © 2015 Society of Cosmetic Scientists and the Soci
et
e Francßaise de Cosm
etologie
International Journal of Cosmetic Science, 38, 389–398
Sensory and instrumental evaluation of creams M. Estanqueiro et al.

to obtain a better correlation with sensorial attributes, these instru-
mental approaches should be used together. Additionally, it is
important to not forget that other components of a formulation,
such as emollients, may influence the sensory properties. However,
these influence should be evaluated independently, as in this case,
were we studied the influence of the thickening agents and there
have verified been significant differences for different agents in dif-
ferent amounts.
Conclusions
The purpose of this study was to correlate mechanical character-
ization of semisolid formulations composed by different thickening
agents at different concentrations with sensorial analysis. A good
correlation was obtained between the textural and rheological
analysis and the sensorial parameters of spreadability and consis-
tency. Additionally, the instrumental method used to predict the
spreadability showed a good correlation with all sensory parame-
ters which is of great interest, as the performed assay did not
need specific equipment. Therefore, these instrumental techniques
can be used industrially to understand the role of different excip-
ients in a formulation and predict the consumers’ acceptance in
a time-saver and less expensive manner.
It is possible to conclude that thickening agents play an important
role on the mechanical properties of semisolid formulations and,
consequently, on the physical stability of creams. An increase in the
amount of thickening agent may positively contribute to the physi-
cal stability of creams. However, the use of higher concentrations of
thickening agents also may result in greater firmness, adhesiveness,
viscosity and difficulty in spreading of these formulations. So, it is
preferable to use lower concentrations of thickening agents and use
other strategies to promote good physical stability over time, such as
change or use different combinations of primary emulsifiers. In this
study, we concluded that lower amounts of carbomers may con-
tribute to obtain a stable formulation with good sensory properties,
such as spreadability, firmness, adhesiveness and consistency. Effec-
tively, the formulation with better scores provided by volunteers was
that with the lower amount (0.25%, w/w) of Carbopolâ 934.
In the future, it could be interesting to evaluate the influence of
mixtures of thickening agents, as the marketed formulations com-
monly have more than one thickening agent.
Acknowledgement
The authors would like to thank the volunteers for their contribu-
tion to the sensorial analysis.

References
1. Tamburic, S., Craig, D.Q.M., Vuleta, G. and
Milic, J. A comparison of electrical and rhe-
ological techniques for the characterisation
of creams. Int. J. Pharm. 137, 243–248
(1996).
2. Barry, B.W. and Grace, A.J. Sensory testing
of spreadability: investigation of rheological
conditions operative during application of
topical preparations. J. Pharm. Sci. 61, 335–
341 (1972).
3. Jones, D.S., Woolfson, A.D. and Brown, A.F.
Textural, viscoelastic and mucoadhesive
properties of pharmaceutical gels composed
of cellulose polymers. Int. J. Pharm. 151,
223–233 (1997).
4. Kusakari, K., Yoshida, M., Matsuzaki, F.,
Yanaki, T., Fukui, H. and Date, M. Evalua-
tion of post-application rheological changes
in cosmetics using a novel measuring
device: relationship to sensory evaluation. J.
Cosmet. Sci. 54, 321–333 (2003).
5. Savary, G., Grisel, M. and Picard, C. Impact
of emollients on the spreading properties of
cosmetic products: a combined sensory and
instrumental characterization. Colloids Surf.
B Biointerfaces 102, 371–378 (2013).
6. Capitani, R.D., Mercurio, D.G., Junior,
F.B.d.C. and Campos, P.M.B.G.M. Stability
and clinical efficacy of moisturizing cosmetic
formulations containing vitamins C and E.
Biomed. Biopharm. Res. 9, 215–224 (2012).
7. Brummer, R. and Godersky, S. Rheological
studies to objectify sensations occurring
when cosmetic emulsions are applied to the
skin. Colloids Surf. A Physicochem. Eng. Asp.
152, 89–94 (1999).
8. Lemaitre-Aghazarian, V., Piccerelle, P.,
Reynier, J.P., Joachim, J., Phan-Tan-Luu, R.
and Sergent, M. Texture optimization of
water-in-oil emulsions. Pharm. Dev. Technol.
9, 125–134 (2004).
9. Gilbert, L., Picard, C., Savary, G. and Grisel,
M. Rheological and textural characterization
of cosmetic emulsions containing natural
and synthetic polymers: relationships
between both data. Colloids Surf. A Physic-
ochem. Eng. Asp. 421, 150–163 (2013).
10. Lochhead, Y.R. The role of polymers in cos-
metics: recent trends. ACS Symp. Ser. 961,
3–56 (2007).
11. Quintana, J.M., Califano, A.N., Zaritzky,
N.E., Partal, P. and Franco, J.M. Linear and
nonlinear viscoelastic behavior of oil-in-
water emulsions stabilized with polysaccha-
rides. J. Texture Stud. 33, 215–236 (2002).
12. Vianna-Filho, R.P., Petkowicz, C.L.O. and
Silveira, J.L.M. Rheological characterization
of O/W emulsions incorporated with neutral
and charged polysaccharides. Carbohydr.
Polym. 93, 266–272 (2013).
13. Bais, D., Trevisan, A., Lapasin, R., Partal, P.
and Gallegos, C. Rheological characteriza-
tion of polysaccharide–surfactant matrices
for cosmetic O/W emulsions. J. Colloid Inter-
face Sci. 290, 546–556 (2005).
14. Ribeiro, H.M., Morais, J.A. and Eccleston,
G.M. Structure and rheology of semisolid o/
w creams containing cetyl alcohol/non-ionic
surfactant mixed emulsifier and different
polymers. Int. J. Cosmet. Sci. 26, 47–59
(2004).
15. Pal, R. Viscoelastic properties of polymer-
thickened oil-in-water emulsions. Chem. Eng.
Sci. 51, 3299–3305 (1996).
16. Lukic, M., Jaksic, I., Krstonosic, V., Dokic, L.
and Savic, S. Effect of small change in oil
phase composition on rheological and textu-
ral properties of w/o emulsion. J. Texture
Stud. 44, 34–44 (2013).
17. Montenegro, L., Rapisarda, L., Ministeri, C.
and Puglisi, G. Effects of lipids and emulsi-
fiers on the physicochemical and sensory
properties of cosmetic emulsions containing
vitamin E. Cosmetics 2, 35–47 (2015).
18. Moravkova, T. and Filip, P. The influence
of thickeners on the rheological and sen-
sory properties of cosmetic lotions. Acta
Polytechnica Hungarica 11, 173–186
(2014).
19. Gilbert, L., Savary, G., Grisel, M. and Picard,
C. Predicting sensory texture properties of
cosmetic emulsions by physical measure-
ments. Chemometr. Intell. Lab. Syst. 124,
21–31 (2013).
20. Carreau, P.J. Rheological equations from
molecular network theories. J. Rheol. 16,
99–127 (1972).
21. Chaudhary, B. and Verma, S. Preparation
and evaluation of novel in situ gels contain-
ing acyclovir for the treatment of oral her-
pes simplex virus infections. Scientific World
J. 2014, 7 (2014).

© 2015 Society of Cosmetic Scientists and the Soci
et
e Francßaise de Cosm
etologie 397
International Journal of Cosmetic Science, 38, 389–398
Sensory and instrumental evaluation of creams M. Estanqueiro et al.

22. ASTM International. E1490–11 Standard
Guide for Two Sensory Descriptive Analysis
Approaches for Skin Creams and Lotions. West
Conshohocken, Pennsylvania (2012).
23. Chanamai, R. and McClements, D.J. Depen-
dence of creaming and rheology of monodis-
perse oil-in-water emulsions on droplet size
and concentration. Colloids Surf. A Physic-
ochem. Eng. Asp. 172, 79–86 (2000).
24. Shi, L., Miller, C., Caldwell, K.D. and Valint,
P. Effects of mucin addition on the stability
of oil–water emulsions. Colloids Surf. B
Biointerfaces 15, 303–312 (1999).
25. Van De Kerkhof, P.C.M., Berth-Jones, J.,
Griffiths, C.E.M. et al. Long-term efficacy and
safety of tacalcitol ointment in patients with
chronic plaque psoriasis. Br. J. Dermatol.
146, 414–422 (2002).
26. Gaspar, L.R. and Maia Campos, P.M.B.G.
Rheological behavior and the SPF of
sunscreens. Int. J. Pharm. 250, 35–44
(2003).
27. Corr^ea, N.M., Camargo J
unior, F.B., Ign

acio,
R.F. and Leonardi, G.R. Avaliacßa ~o do com-
portamento reol
ogico de diferentes g
eis
hidrof
ılicos. Rev. Farm. Bioquim. Univ. Sao
Paulo 41, 73–78 (2005).
28. Marty, J.P., Lafforgue, C., Grossiord, J.L.
and Soto, P. Rheological properties of
three different vitamin D ointments and
their clinical perception by patients with
mild to moderate psoriasis. J. Eur. Acad.
Dermatol. Venereol. 19(Suppl 3), 7–10
(2005).
29. Liu, W., Hu, M., Liu, W., Xue, C., Xu, H.
and Yang, X. Investigation of the carbopol
gel of solid lipid nanoparticles for the trans-
dermal iontophoretic delivery of triamci-
nolone acetonide acetate. Int. J. Pharm.
364, 135–141 (2008).
30. Estanqueiro, M., Conceicß~ao, J., Amaral, M.H.
and Sousa Lobo, J.M. Characterization, sen-
sorial evaluation and moisturizing efficacy of
nanolipidgel formulations. Int. J. Cosmet. Sci.
36, 159–166 (2014).

398 © 2015 Society of Cosmetic Scientists and the Soci
et
e Francßaise de Cosm
etologie
International Journal of Cosmetic Science, 38, 389–398