Colloids and Surfaces A 536 (2018) 38–46

Contents lists available at ScienceDirect

Colloids and Surfaces A

journal homepage: www.elsevier.com/locate/colsurfa

How does composition influence the texture of cosmetic emulsions? T

⁎
Pauline Dubuisson, Celine Picard, Michel Grisel, Geraldine Savary
Normandie Univ, UNIHAVRE, FR 3038 CNRS, URCOM, 76600 Le Havre, France

G RA P H I C A L AB S T R A C T

A R T I C L E I N F O A B S T R A C T

Keywords: Using the Spectrum Descriptive Analysis method, the present work defines a methodology developed in order to
Sensory analysis-texture discriminate and characterize cosmetic oil-in-water emulsions as well as their respective aqueous phases con-
Cosmetic oil-in-water emulsions taining xanthan gum. The objective was to describe and understand how composition parameters govern texture
Xanthan gum perception, through the study of the impact of the amount of (1) xanthan and (2) oil phase. For that purpose,
Oil concentration-aqueous phase
emulsions were developed by varying either their amount of xanthan or oil concentration. Seven texture at-
tributes were selected and defined using precise and strict evaluation protocols and notation scales to set up a
quantitative framework: integrity of shape, penetration force, wetness, ease of spreading, grease, stickiness and gloss.
Results demonstrate the contribution of each parameter to the texture of emulsions and aqueous phases. For
example, increasing the oil phase ratio in emulsion mainly enhances the consistency, grease degree and residual
stickiness of the creams. Moreover, the study establishes consistent linear relationships according to the con-
centration in xanthan in solutions for five attributes: integrity of shape, penetration force, wetness, ease of spreading
and gloss. Interestingly, the effect of xanthan in emulsions is similar but obviously diminished when compared to
polymer solutions.

1. Introduction been led to understand the influence on sensory properties of some of

the ingredients such as: emollients (Goldemberg and De La Rosa, 1971;
Oil-in-water (O/W) emulsions are very commonly used in the food, Parente et al., 2005, 2008 [2,3], moisturizers [4,5] as well as the
pharmaceutical and cosmetic industries [1]. They consist of an oil combination of cross-linked acrylic polymers and emollient esters [6].
phase dispersed as droplets in a continuous aqueous phase. The com- [7] studied the effect of eight distinct texturing agents (natural, semi-
position of an emulsion greatly affects its physical properties which, in synthetic, synthetic) on the skin feel properties of O/W emulsions
turn, impact the product behavior during manufacturing, packaging whereas other authors have studied the sensory properties of cosmetic
and application. Indeed, as an example, the texture of emulsions during emulsions without focusing on the contribution of any particular in-
application is known to be of great importance regarding the con- gredient [8–11]. For all of the above works, the products were eval-
sumers’ preference. The texture of a product is a complex and multi- uated using approaches applicable to both the description and the
dimensional notion that has therefore to be carefully considered. As the quantification of textural properties. These methods were adapted from
texture is linked to the emulsion’s composition, distinct studies have the sensory principles of the food texture profile [12–14]; either

⁎
Corresponding author.
E-mail address: geraldine.savary@univ-lehavre.fr (G. Savary).

http://dx.doi.org/10.1016/j.colsurfa.2017.08.001
Received 12 July 2016; Received in revised form 28 July 2017; Accepted 2 August 2017
Available online 24 August 2017
0927-7757/ © 2017 Elsevier B.V. All rights reserved.
P. Dubuisson et al. Colloids and Surfaces A 536 (2018) 38–46

through consumer research methodologies such as check-all-that-apply 2. Materials and methods

(CATA) questions [15] or through objective sensory analyses using the
Quantitative Descriptive Analysis (QDA) method [16] on the one hand 2.1. Materials
or the Spectrum Descriptive Analysis (SDA) method [17] on the other
hand. 2.1.1. Ingredients
Using the latter methodology, our study focuses on the impact of a Xanthan gum powder (Rhodicare T) from Rhodia was used as tex-
particular natural hydrophilic polymer named xanthan gum. This gum turing agent. Butylene glycol (Acros Organics) was used as humectant,
is an anionic high molecular weight extracellular heteropolysaccharide phenoxyethanol, methylparaben, ethylparaben, propylparaben (Jan
produced by aerobic fermentation of sugars by the microorganism Dekker International) as preservative system (Dekaben MEP), di-
Xanthomonas campestris. Xanthan gum is a non-gelling biopolymer able methicone (Dow Corning), isohexadecane (IMCD), paraffin (Baeriocher
to form highly viscoelastic solutions even at low concentrations because France) and stearic acid (KLK Oleo) as emollients and, finally, steareths
of its semi-rigid conformation stabilized by side chains of mannose and 2 and 21 (Croda) as emulsifying agents.
glucuronic acid [18]. In emulsion, it exhibits a rheological behavior
similar to that in solution: a high viscosity at low shear rates, a strong
2.1.2. Emulsion preparation
non-thixotropic shear-thinning character and a viscoelastic behavior
Six O/W emulsions were formulated, each varying either by the oil
[19].
phase content or by the amount of added xanthan. Emulsions without
For all these reasons, xanthan is widely used in many cosmetic and
xanthan, named Controls, were prepared with 10%, 20% and 30% of oil
food systems. A previous study [7] concluded that the presence of
phase. The content of each oil phase ingredient was multiplied, in
xanthan at 1% in O/W emulsions, in comparison with a gum-free
comparison with the Control with 10% of oil, by, respectively, 2 and 3,
emulsion, does not bring significant gloss, difficulty of spreading or
for the Controls with 20% and 30% of oil, except for the quantity of
absorbency but brings firmness and high degrees of stringiness and
surfactant. Indeed, this parameter remained constant for each of the six
stickiness. To date, the details of the impact of the amount of xanthan
emulsions (4%) and was determined to reach a physicochemical sta-
gum on the perception of emulsions have not been reported, notably
bility of the control emulsion with the highest amount of oil (30%) and
considering both the gum content and the oil/water phase ratio.
without xanthan. An additional objective was to study the influence of
The objectives of this study were thus to adapt a methodology
oil content on size distribution and the organization of the emulsion
previously described by different authors [7,12], composed of defini-
droplets.
tions, evaluation protocols, scales and a quantitative frame of refer-
The aqueous phase of the six emulsions is the same in terms of
ences, in order to evaluate how the xanthan gum amount and the oil
humectant and preservative system contents (%, w/w). They only vary
content contribute to the texture properties of O/W emulsions. The first
by their amount of gum and water: the global content (100%, w/w) is
part of this paper focuses on the sensory characterization of these
adjusted through the quantity of water. For the three emulsions con-
emulsions from the appearance stage to the perception during and after
taining xanthan, the natural polymer was first pre-dispersed in butylene
application on skin. In the second part, solutions containing the same
glycol (4% w/w) at concentrations of 0.3, 0.7 and 1% w/w and then
amounts of xanthan were studied using the same methodology in order
incorporated into emulsions containing 10% of oil phase (Table 1).
to reveal how the texture properties of the aqueous phase may affect the
Those three emulsions are coded E- in the rest of this paper. Batches of
perception of the emulsions. In this study, seven attributes were ex-
200 g were formulated with, for each emulsion, a suitable formulation
amined to properly describe and particularly distinguish the texture of
protocol developed in order to obtain stable emulsions over at least 6
the emulsions and solutions: integrity of shape, penetration force, wetness,
months. The protocol is similar to the one developed in a previous study
ease of spreading, grease, stickiness and gloss. Panelists’ performance was
[7] except for the fact that mechanical stirring speed using a de-
assessed to prove that the sensory panel is reliable and that the meth-
flocculating paddle (Turbotest VMI®) was adapted to the consistency of
odology is suitable to evaluate such xanthan-based products.
each mixture to reach a suitable mixing efficacy.

2.1.3. Xanthan solution preparation

200 g of aqueous solutions, coded S-, were prepared with 0.3, 0.7, 1
and 2% (w/w) of xanthan in order to compare the gum impact and
behavior in both solution and emulsion. For that purpose, xanthan
powder was first pre-dispersed in butylene glycol (4% w/w), and then

Table 1
List of ingredients (INCI name) used into the o/w emulsions and physicochemical properties of emulsions.

Control10% E-XG0.3% E-XG0.7% E-XG1% Control20% Control30%

Aqueous phase Distilled water QS QS QS QS QS QS

Butylene glycol 4.0 4.0 4.0 4.0 4.0 4.0
Xanthan gum 0.0 0.3 0.7 1.0 0.0 0.0
Preservatives 0.5 0.5 0.5 0.5 0.5 0.5
Oil phase Dimethicone 1.0 1.0 1.0 1.0 2.0 3.0
Isohexadecane 7.0 7.0 7.0 7.0 14.0 21.0
Paraffin 1.5 1.5 1.5 1.5 3.0 4.5
Stearic acid 0.5 0.5 0.5 0.5 1.0 1.5
Steareth 2 2.4 2.4 2.4 2.4 2.4 2.4
Steareth 21 1.6 1.6 1.6 1.6 1.6 1.6
Droplets size distribution d2 (μm) 0.32 0.31 0.42 0.40 0.15 0.16
d50 (μm) 3.92 5.23 2.70 2.28 12.6 17.9
d98 (μm) 39.6 50.0 37.5 32.2 65.9 66.3
Viscoelastic parameters G' (Pa) 80.4 76.3 72.3 81.5 236 362
G” (Pa) 18.5 26.5 21.5 23.4 44.0 85.0

INCI, International Nomenclature of Cosmetic Ingredients.

39
P. Dubuisson et al. Colloids and Surfaces A 536 (2018) 38–46

Table 2
Evaluation protocols of five out of the seven attributes.

Evaluation protocols

Rub-out:
Wetness Evaluate the wetness of the product during the first five rounds.
Ease of spreading Keep on applying and evaluate the product ease of spreading between the first round and the tenth.
Grease After having evaluated the product ease of spreading, evaluate its grease between the tenth and the twentieth round.

After-feel:
Stickiness In the same way as for the protocol evaluation for the rub-out phase, draw three circles on the inner surface of each forearm. After spreading the product for 50
strokes, start a timer. After 30 s, strongly press edge of the opposite hand over the application site and then remove it slowly. Repeat three times and evaluate
the product stickiness.
Gloss Turn on the booth light. 2 min and 30 s after having evaluated the stickiness, bring the forearm on which the product has been applied closer to the light, 41 cm
away from the edge of the booth desk. Slightly incline the forearm to catch reflection and evaluate gloss.

added to the distilled water mixed with Dekaben MEP (0.5% w/w). notation scales, developed using the procedure described by [25],
using mainly commercial cosmetic products.
2.1.4. Reference solution preparation • The final step consisted of four periods of 30 min during which some
Solutions were prepared to be used as references as part of the of the products were evaluated, the results discussed and the whole
sensory analysis attributes scale, as explained in 2.2.1.1. methodology validated.
A solution of polymers with 0.4% w/w of Carbomer (Carbopol
Ultrez 10, Lubrizol), 4.0% w/w of methylpropanediol (Dub diol, In the end, seven sensory texture attributes were selected by con-
Stéarinerie Dubois), 0.4% w/w of xanthan gum (Kelco CG, Kelco), 1.5% sensus to characterize the ten products properly: integrity of shape was
w/w of phenoxyethanol (Jan Dekker) and distilled water was for- evaluated during the “appearance phase,” penetration force during the
mulated and neutralized with 0.40 g of TEA (pH = 6.07). “pick-up phase,” wetness, ease of spreading and grease during the “rub-
Aqueous solutions of xanthan gum (Rhodia) composed of 0.7% and out phase” and stickiness as well as gloss during the “residual appearance
1% of xanthan gum (w/w) dispersed in distilled water, in the presence phase.” The attributes integrity of shape, penetration force and stickiness
of 0.5% (w/w) of preservative Dekaben MEP were produced. are described in a previous study [7]. The corresponding definitions of
the other attributes are:
2.1.5. Stability and microbiological contamination
Once prepared, all emulsions and solutions were stored at 4 °C in • Wetness: perceived amount of water while applying the product
5 mL plastic jars. Physical stability over time was checked by optical • Ease of spreading: required force to move product over skin
microscopy observations as well as pH, particle sizing and rheological • Grease: perceived amount of grease while applying the product
measurements (results not shown) to ensure absence of aging. Prior to (rich, thick and butter-like feeling)
any sensory analysis, a microbiological test was performed (ACM, • Gloss: Amount of reflected light from product once absorbed on skin
Bellegarde, France) to make sure that each product was in accordance
with the cosmetic criteria for bacterial contamination (< 100 UFC/g Integrity of shape and penetration force were evaluated the same way
or/ml) for both the search of aerophilic mesophilic bacteria [20] and as described elsewhere [7]. Protocols for the other five attributes are
the enumeration of yeasts and molds [21]. detailed in Table 2. However, prior to the evaluation of those attributes
the panelists had to:
2.2. Methods
• Using a skin scribe and a template, draw two symmetrical circles
2.2.1. Sensory analysis (5.4 cm diameter) on the inner surface of each forearm with 1.5 cm
Based on the SDA method, through the use of absolute scales, a valid between each circle.
and reliable sensory evaluation method discriminating and describing • With a positive displacement pipette equipped with a capillary
the diversity of creams and solutions in terms of texture properties was piston (Microman M250, GILSON, Middleton, WI), deliver 50 μL of
developed, all taking into account rheological principles and physical product to the center of the circle on the suitable forearm as in-
characteristics of the products. structed by a random function.
• Spread the entire amount of product within the whole circle using
2.2.1.1. Terminology development. The lexicon only focuses on the opposite forefinger by making a clockwise circular motion at a
appearance and texture attributes. The development of the rate of one and a half rounds per second (a metronome is set to mark
terminology for all the products tested (six emulsions and four time at 90 rpm). Adapt the force with which the product is spread so
solutions) was based on previous studies [22,7,23,13]. The conditions that it can be applied for 50 strokes.
for the test (environment, sample handling and panelists’ skin
conditioning) were determined by the Standard Practice for For each of the seven attributes, 0–9 scales with 0.5 increments
Descriptive Skinfeel Analysis of Creams and Lotions given by the were used, 0 being the minimum and 9 the maximum. As an example,
ASTM [24]. for gloss, 0 stands for the product being matt and 9 for the product being
The methodology was structured through a three-step process led by highly glossy. Each attribute scale consisted of four or five references
a group of experts: covering different levels of intensity, as listed in Table 3. Products are
commercial creams, lotions or gels, ingredients (water, vaseline…) or
• Six preliminary sessions (2 h each) were required to review all prepared polymers solutions. Products were specifically chosen for this
samples and to select the most pertinent attributes from the litera- study in order to well discriminate our ten systems. Some products were
ture in order to discriminate the texture and appearance of all already used in other studies in particular to define the scores for in-
creams and solutions. tegrity of shape, penetration force, ease of spreading [7]. The choice
• Thirteen more sessions of 2 h were essential to develop a common and the positioning of each product on the scale were done during a
terminology with precise evaluation procedures and accurate preliminary study with the sensory panel. Such physical references

40
P. Dubuisson et al. Colloids and Surfaces A 536 (2018) 38–46

Table 3 reduce notably both the training time and the evaluation time.
Intensity scale values and reference products.
2.2.1.3. Evaluation of products for each attribute. Prior to each session,
Attributes Scale values Products
all panelists were instructed to wash their hands, and their forearms
Integrity of shape 1 Auchan make-up remover lotion − New when needed, with a hydroalcoholic gel and then to take place in one of
formula the sixteen individual booths of the sensory laboratory. Samples were
3 Nivea express hydration body lotion
placed at room temperature two hours prior to any evaluation. They
5 Nivea sensitive cleansing milk (sensitive skin)
7 Mixa protective hand cream anti-dryness were coded with a three-digit code and provided in the 5 mL plastic jars
9 Nivea creme in randomized order for each judge and each session to avoid any bias
Penetration force 0 Water on rating scores. For each attribute, references were at the panelist’s
3 Barbara Gould integral make-up remover disposal during evaluation. As each evaluation session lasted for around
6 Mixa protective hand cream anti-dryness
30 min, it was often not possible to measure all products in a single day.
9 Nivea creme
Wetness 1 Mixa protective hand cream anti-dryness Indeed, because some of the evaluation protocols were longer or
3 Auchan make-up remover lotion − New because the same emulsion/solution was measured through several
formula attributes in one session, only four products per day could be analyzed
6 Solution of 0.7% of xanthan
for wetness, ease of spreading and grease and eight products a day for
9 Water
Ease of spreading 0 Nivea creme stickiness and gloss. All the products were measured twice for each
3 Mixa protective hand cream anti-dryness attribute.
5 Auchan make-up remover lotion − New Overall, training and evaluation of the ten products on the seven
formula texture attributes lasted for five months at a frequency of one session a
7 Solution of 1% of xanthan
week.
Grease 1 Hydroalcoholic gel Softalind ViscoRub
4 Mixa protective hand cream anti-dryness
6 Nivea smoothing indulgence hand cream 2.2.2. Physicochemical characterizations of emulsions
9 Vaseline 2.2.2.1. Droplets size distribution. The emulsion droplet size distribution
Stickiness 0 Bare skin
was measured by static light scattering using a laser diffraction particle
3 Mixa protective hand cream anti-dryness
5 Solution of polymersa
size analyzer SALD–7500 nano (Shimadzu France, Marne la Vallée,
8 Aderma Intense Repair Hand Cream France) equipped with a violet semiconductor laser (405 nm) and a
Gloss 0 Bare skin reverse Fourier optical system. Emulsions were diluted with deionized
2 Aderma Intense Repair Hand Cream water before measurement. Emulsions were stirred continuously using
4 Auchan make-up remover lotion − New
a stirring plate throughout the measurement in the batch cell (7 cm3). A
formula
7 Nivea essentially enriched body lotion refractive index of 1.45−0.00i was used. Data were analyzed using
software, Wing SALD II. The values of d2, d50 (median diameter) and d98
a
See 2.1.4. were acquired and correspond to the maximum emulsion droplet size
below which 2%, 50% and 98% of the sample volume exist. Values are
were used in order to reduce variability and subjectivity among pane- reported as the average of three readings made on each sample.
lists’ ratings.
As previously mentioned, the present lexicon has obviously some 2.2.2.2. Rheological behavior. Rheological tests were performed with a
similarities with previous terminologies developed for creams and lo- controlled stress rheometer (HR-1, TA Instruments) at 25 °C with a
tions but some definitions, protocols and/or scales were notably im- cone-plate aluminum device (1°59′38′’ cone angle, 40 mm diameter,
proved so that bias and individual differences in the evaluation would 47 μm gap). Measurements were carried out in duplicate. A solvent trap
be avoided. was used. Once loaded, samples relaxed and acclimatized for 2 min
prior to measurement. Logarithmic oscillations strain sweep tests were
2.2.1.2. Recruitment −training. In order to evaluate the products on a carried out at a frequency of 1 Hz with strain increasing from 0.01 to
relatively homogeneous panel in terms of skin, the panelists were 300%. Through those experiments, the storage (G’) and loss (G”)
selected among 20–50 year-old women with Caucasian skin type. moduli on the linear viscoelastic region were acquired for each sample.
Indeed, women’s skin is thinner than men’s [26] and they are,
generally, more regular cosmetics consumer, which makes it easier to 2.2.3. Statistical analysis
train them and keep them interested throughout the whole duration of The panel’s objectives are to discriminate between products, to give
the study. Moreover, since structural skin differences exist, notably in repeatable and reproducible results; thus, it is considered to be a real
terms of thickness as well as water and lipid contents [27] according to instrumental tool. As such, statistical analyses were performed using
the different racial groups (Caucasoid, Negroid, Mongoloid, Australoid XLSTAT software from Addinsoft (version 14.1.01, Paris, France) on the
and Capoid races) and in terms of elasticity, hydration and thickness panel’s collected data. For each attribute, a two-way analysis of var-
according to age, it was important to recruit women below 50 years old iance (ANOVA) with interaction products X assessors was conducted.
with the same skin type. In the end, eighteen panelists respecting all the The effects of each factor (product and assessor) and their interaction in
above criteria were selected among volunteers according to their terms of probabilities are P values. Differences between the products
motivation, availability and their ability to describe and score were analyzed using Tukey’s method for multiple comparisons of means
selected skin feel properties. when factor effects were significant (P ≤ 0.05). The model used is the
The training period was conducted separately for each attribute or same as in [7]. It takes into account five parts: the sample’s mean value,
phase, for the rub-out and residual appearance phases. Depending on the product effect, the assessor effect, the product-assessor interaction
the attribute, one or two training sessions were performed to ensure and, lastly, a part that mainly includes the repetition effect. The pa-
panel reliability with respect to the definition, the evaluation protocols nelists’ repeatability was evaluated through the value of root mean
and the rating scales using the appropriate references. At the end of the square error (RMSE). This parameter measures the differences between
training period, four samples were evaluated by the panelists in order to the values predicted by the model and the observed values. It takes into
confirm the validity of their responses. The evaluation of the ten pro- account missing factors in the ANOVA model, such as the effect of re-
ducts was carried out once a consensus was reached, before focusing on petitions. The panel’s repeatability was evaluated through a direct
another attribute or group of attributes. This procedure was efficient to comparison of the RMSE value for each attribute since the scale ranges

41
P. Dubuisson et al. Colloids and Surfaces A 536 (2018) 38–46

are similar for each of them. Table 4

For some of the attributes (penetration force, wetness, ease of Results of ANOVAs in terms of probability, RMSE and number of groups of emulsions for
each attribute.
spreading and gloss), one panelist could not manage to apprehend the
attribute definition or its evaluation scale the same way as the other ANOVAs Assessor X product
panelists. In such cases, the results obtained by this assessor were re-
moved from the statistical analysis in order to lower the variability Attributes P (product) P (assessor) P (interaction) RMSE Number of
among the panelists’ ratings. This made it possible to increase the sig- groups
Integrity of < 0.0001 < 0.0001 0.728 0.780 4
nificance of the differences between products. shape
Principal component analysis (PCA) was also performed on centered Penetration < 0.0001 < 0.0001 0.570 0.873 4
as well as auto-scaled mean data in order to highlight the relationships force
between products and attributes. Wetness < 0.0001 0.0370 0.843 1.146 3
Ease of < 0.0001 0.0030 0.045 0.968 3
spreading
3. Results Grease 0.0010 < 0.0001 0.701 1.210 2
Stickiness < 0.0001 < 0.0001 0.379 1.783 3
Gloss 0.0300 < 0.0001 0.704 1.530 2
In this study, the texture properties of cosmetic emulsions were
analyzed in order to understand the effect of the oil phase level as well
as the impact of the amount of xanthan gum in the aqueous phase. In sources of variation for the scoring. It takes into account the disagree-
the first part, results focus on the sensory characterization of these ments in the strict sense of the word, i.e. the assessors rank the products
emulsions. In the second part, solutions containing the ingredients of differently, and the differences in dispersion of the scaled-scores which
the aqueous phase of the previous emulsions were studied using the means that the assessors classify the products the same way but do not
same methodology. Seven attributes were examined to properly de- perceive the same variances between the products Stone et al., 2012.
scribe and particularly distinguish the texture of the emulsions and Hence, a non-significant interaction implies that the panelists perceive
solutions of this study: integrity of shape, penetration force, wetness, ease the same differences between the products, meaning that a consensus
of spreading, grease, stickiness and gloss. between the judges was obtained for the assessment of six out of seven
attributes. Consequently, the panel was reproducible in its judgment.
3.1. Texture properties of oil-in-water emulsions Table 4 also illustrates the panel’s repeatability through the RMSE
for each attribute. Considering that, on a scale ranging from 0 to 9, an
3.1.1. Panel performance results error of 15% in notation is acceptable, the RMSE below which the panel
To this purpose, a two-way ANOVA for each attribute was con- can be considered as rather repeatable is 1.35. Therefore, the panel is
ducted on data in order to evaluate the influence of the different factors repeatable for integrity of shape, penetration force, wetness, ease of
(product and assessor) and their interaction. spreading and grease for which the RMSE varies between 0.780 and
The model used was as followed (Eq. (1)) with i the product, j the 1.210. The higher RMSE values for stickiness and gloss illustrate the
assessor and k the repetition: complexity to evaluate these attributes, in relation with the residual
film, which appear quite impacted by absorbency and skin variability.
yijk = μ + αi + βj + γij + εijk (Eq. (1)) To sum up, all the above results show a high product discrimination,
a great consensus between assessors and good repeatability reached
Each score (yijk) is composed of five different parts: the first one char-
through an intensive training and the use of appropriate references.
acterizes the mean value (μ of the sample, the second one corresponds
These statistical analyses prove that the sensory panel is reliable on the
to the product effect (αi), the third one is the assessor effect (βj), the
one hand, and that the methodology is suitable to evaluate such xan-
fourth one identifies the product-assessor interaction (γij), and the final
than-based products, on the other hand.
one (εijk) conveys both the uncertainty of the measurement and the
inadequacy with the model; this last parameter mainly includes re-
petition effect. 3.1.2. Influence of emulsion parameters on texture properties
The effects of each parameter in terms of ANOVA test probability, Table 5 summarizes each emulsion mean score for each attribute
RMSE and Tukey’s number of groups of products for the seven oil-in- (all assessors and repetitions put together). For integrity of shape and
water emulsions are presented in Table 4. First of all, the product effect penetration force attributes, creams are well-differentiated and can be
(αi) is significant (P < 0.05) for grease and gloss and highly significant classified in four different groups based on Tukey’s test. Results exhibit
(P < 0.0001) for all the other attributes. This parameter depends on a large diversity of products with scores ranging from 2.69 to 6.82 and
the choice of the samples, the selection of relevant and accurate texture 1.87–5.70 for integrity of shape and penetration force, respectively. Both
attributes and panel performances. Thus, a significant product effect attributes display similar product rankings regarding their mean values:
demonstrates that the panelists are capable of discriminating between Control10% is evaluated with the lowest intensity, then emulsions
the emulsions for all seven attributes. XG0.3%, XG0.7% and XG1% with increasing intermediate scores,
The assessor effect (βj) is significant for both wetness and ease of Control20% and lastly, Control30% with the highest intensities. Thus,
spreading (P = 0.0370 and P = 0.0030 respectively) and highly sig- those consistency parameters increase with both xanthan and oil
nificant for the other attributes. A significant assessor effect means that amounts. Wetness and ease of spreading each exhibit different behaviors
the global means (all products and repetitions put together) are not among products: Control30% is rated as the lowest, then Control20%,
homogeneous among the judges. This may be the consequence of dif- and afterwards the emulsions with decreasing amount of xanthan and
ferences among the panel in the way of evaluating the products, the use Control10% have the highest values. Both attributes exhibit a sig-
of the scales or differences in skin types. This assessor effect is generally nificant difference between Control10% and Control20% but not be-
significant, persistent even with an intensive training but does not bring tween the latter and Control30% and values that tend to decrease when
real information on panelists’ performance. the amount of xanthan increases. For grease, assessors gave close scores
The panel performance is characterized rather through the product for all emulsions, ranging from 3.25 to 4.36. The grease feature of
X assessor interaction [28]. The P values for this interaction are not emulsions tends to increase with the amount of xanthan. Indeed, the
significant (P > 0.05) for every attribute (P = 0.379 to 0.843) except emulsion XG0.7% is evaluated with the same score as Control20%.
for ease of spreading (P = 0.045). This parameter is often interpreted as Stickiness also displays distinctive groups of products: the mean values
a way of measuring the disagreement between assessors through two lean towards an increase when the amounts of xanthan as well as oil

42
P. Dubuisson et al. Colloids and Surfaces A 536 (2018) 38–46

Table 5
Mean intensity scores for the descriptive analysis data of emulsions.

Products Attributes

Integrity of shape Penetration force Wetness Ease of spreading Grease Stickiness Gloss
Control10% 2.69 d 1.87 d 3.77 a 5.04 a 3.25 b 3.21 c 3.79 b
E-XG0.3% 2.77 d 2.43cd 3.31 ab 4.88 ab 3.81 ab 4.71 ab 4.23 ab
E-XG0.7% 3.36 c 2.46cd 2.64 bc 4.57 abc 4.21 a 4.87 a 4.18 ab
E-XG1% 4.67 b 3.00 c 2.55 bc 4.18 c 4.32 a 5.03 a 4.95 a
Control20% 6.60 a 3.73 b 2.40 c 4.28 bc 4.19 a 3.57 bc 4.60ab
Control30% 6.82 a 5.70 a 2.35 c 3.96 c 4.36 a 4.81 a 4.74 ab

a−d
In each column, products with means displaying the same letter are not significantly different from one another (P < 0.05) for this specific attribute.

phase increase. Like grease, gloss only presents two groups of products corresponding loading plot of the variables is presented in Fig. 2. It
with significant differences between means. Differences between the illustrates that the vectors of variables are well-represented since they
products were fairly low. The products ranked from Control10% to are close to the correlation circle. F1 is positively related to four at-
emulsion XG1%, the lowest and the highest values, respectively, and tributes: integrity of shape, penetration force, grease and gloss with a high
the emulsions XG0.7%, XG0.3%, Control20% and Control30% with correlation (correlation coefficients between attributes and F1 ranging
increasing intermediate values. from 0.884 to 0.969). Moreover, wetness and ease of spreading are ne-
gatively loaded on F1 and highly correlated as well to this first com-
3.1.3. Physicochemical characteristics of emulsions ponent (correlation coefficients between attributes and F1 of −0.962
Droplets size distributions and viscoelastic parameters of each for wetness and −0.908 for ease of spreading). Besides, stickiness is po-
emulsion were also measured (Table 1). Regarding the three control sitively loaded on F2.
emulsions containing 10%, 20% and 30% of oil phase, one can observe Fig. 3 presents the loading plot for the ten products, thus allowing a
that the median droplet size (d50) and the sizes distribution (d2 and d98) global comparison of the effect of xanthan in both emulsion and aqu-
increase as the volume fraction of oil increases. Both viscoelastic eous phase. First of all, products appear well distributed on the loading
modulus (G’ and G”) show a rise with the oil content revealing firmer plot along F1 and F2. It can be observed that the six emulsions and the
emulsions. four solutions are divided in two distinct clusters. The emulsions are
Concerning the xanthan-based emulsions, results from static light characterized by the highest degrees of penetration force, integrity of
scattering and rheology exhibit a less significant effect. Droplets size shape, grease and gloss while the solutions are characterized by their
distributions are similar with d50 ranging from 2.28 μm for E-XG1% to higher degrees of ease of spreading and wetness.
5.23 μm for E-XG0.3%. Values of G’ and G” on the linear viscoelastic
region are almost the same whatever the content of xanthan. 4. Discussion
The impact of the oil phase on the physicochemical properties is
thus more important than the xanthan amount present in the aqueous The previous results highlight that the amounts of both the xanthan
phase. and the oil phase impact the textural properties of emulsions as well as
solutions. The contribution of these two parameters in both media is
3.2. Texture properties of aqueous phases compared. Now let’s discuss these results.

Fig. 1 shows the panel’s mean scores for the aqueous solutions with 4.1. Influence of emulsion parameters on texture properties
increasing concentrations of xanthan gum. Each graph corresponds to
one attribute and represents the mean assessors’ score as a function of Regarding the influence of emulsion parameters on integrity of shape
the amounts of xanthan from 0.3 to 2%. Standard deviations were and penetration force, it can be observed that, on the whole, the effect of
calculated on the assessor’s scores. A linear regression was performed the oil phase content is greater than the effect of the amount of xanthan.
for each attribute. When the calculated coefficient of determination R2 However, this observation actually depends on the attribute. Indeed,
was higher than 0.90, we assumed that the relationship was highly the increase in the oil phase content induces an increase for both at-
reliable; the corresponding regression equation was then indicated tributes with a significant effect for penetration force whereas the in-
below the graph. The linear equation was expressed as followed: crease in the xanthan content also induces an increase for both attri-
y = ax + b except for penetration force, expressed as: y = ax, since the butes but with a significant effect for integrity of shape. These two
reference for penetration force = 0 was water on its own (Table 3). attributes are both related to the cream consistency either at rest (in-
On the one hand, for integrity of shape, penetration force, wetness and tegrity of shape) or during pick-up (penetration force). The higher the oil
gloss, solutions were well discriminated by assessors. In these cases, phase content, the more consistent the emulsion in accordance with
each attribute varies linearly with xanthan content. On the other hand, higher viscoelastic modulus (Table 1). While more xanthan induces an
results were less significant for the other attributes. Furthermore, for increase in consistency at rest but not during pick-up, probably because
grease as well as stickiness, one can observe that the values tend to a of its well-known shear thinning behavior [19]. Wetness was studied in
maximal mean score since no significant differences were evidenced the present work because we assumed that the perception of wetness
between 1 and 2% of xanthan. during application might be modified by the quantity of water in the
product. This assumption is indeed verified through the results because
3.3. Comparison of the texture properties of emulsions and aqueous wetness decreases when the oil phase ratio increases and tends to de-
solutions crease as well when the xanthan amount increases, thus when the
quantity of water decreases in terms of the global content of the
A PCA was carried out on all of the data for the emulsions and so- emulsion. Regarding ease of spreading, our aim was to evaluate the ef-
lutions. This analysis enables a better evidencing of the differences fect of xanthan gum, which is often used to improve the application of
among the products and a possible generalization of relationships be- creams onto skin. Nevertheless, it probably depends on its concentra-
tween attributes. The first two principal components account for tion, since above 0.3% the ease of spreading of the cream declines. We
91.58% of the total variance (73.25% for F1 and 18.33% for F2). The assumed that ease of spreading is influenced rather by the consistency.

43
P. Dubuisson et al. Colloids and Surfaces A 536 (2018) 38–46

Fig. 1. Representation of the impact of the amount

of xanthan on the panel mean score for each attri-
bute for xanthan solutions.

Indeed, the higher the consistency, the more difficult the product is to in the case of an increase in oil phase content. Moreover, an addition of
spread. For grease, while there is a significant difference perceived be- 0.3% of xanthan provides more stickiness than 20% of oil and one of
tween Control10% and Control20%, surprisingly there is none between 0.7% or more provides higher degrees of stickiness than 30% of oil.
Control20% and Control30%, whereas we expected that grease would Through the products’ ranking, one can see that mean values seem
be greatly impacted by the oil phase amount. This shows that the re- to indicate that increasing the amounts of both xanthan and oil tends to
lationship between the grease perception and the oil phase content is raise gloss. Unexpectedly, 1% of xanthan shows a higher effect if com-
not linear. In the case of stickiness, the impact of xanthan content seems pared to the emulsion with 30% of oil.
to be predominant over that of the oil ratio on the property of the re- Actually, panelists encountered some difficulties to discriminate
sidual film after application. Indeed, stickiness mean values tend to in- between the emulsions for grease and gloss. This may be due to the fact
crease when both the amounts of xanthan and oil phase increase ran- that:
ging from 3.21 to 5.03 regarding the gum impact and from 3.21 to 4.81

44
P. Dubuisson et al. Colloids and Surfaces A 536 (2018) 38–46

4.2. Texture properties of aqueous phases

The results regarding the texture properties of the aqueous phase

reveal the impact of xanthan in solution. Indeed, this hydrocolloid in-
creases the consistency at rest (integrity of shape) as well as during ap-
plication (penetration force). Furthermore, it diminishes wetness, which
is remarkable in view of the fact that the water content remains above
93% and the xanthan at a low concentration in the solutions. Likewise,
assessors have perceived more grease with an increase in the amount of
xanthan. In this context, xanthan gum is able to bring some of the
properties of a fatty ingredient. Moreover, the polysaccharide enhances
skin stickiness and gloss after application but decreases ease of spreading
during application, as was previously observed with the corresponding
emulsions.
Equations established in Fig. 1 are tools of a practical relevance to
anticipate the texture properties of xanthan solutions, notably within a
0.3-2% content, which corresponds to the common level of use of this
texturing agent in cosmetic products.

Fig. 2. PCA loading plot of the seven attributes. 4.3. Comparison of the texture properties of emulsions and aqueous
solutions

• they found it difficult to evaluate gloss, thus requiring more time to The PCA plot representing all seven attributes underlines the narrow
achieve consistent values during the training sessions,
• grease may be just slightly influenced by the different emulsion relationships between six of them: integrity of shape, penetration force,
grease, gloss, wetness and grease. It confirms the correlation between
parameters. Hence for the panel to be able to discriminate between
integrity of shape and penetration force, both being related to consistency,
the products, it requires a very much higher sensitivity, which could
or firmness [7]. The grease attribute appears negatively correlated with
have been acquired through a longer training period,
• there were disparities among the panelists maybe due to skin types
wetness but is clearly associated with the consistency of the product,
making it possible to understand this ambiguous perception. What is
[27].
interesting is the correlation of ease of spreading with wetness rather than
with the integrity of shape or penetration force (Pearson coefficients be-
In any case, it is interesting to note that both the xanthan and the oil
tween ease of spreading and wetness, integrity of shape and penetration
phase contents influence the texture properties before, during and after
force of 0.967, −0.646 and −0.654 respectively). Indeed, the higher
application through the residual film left on the skin.
the product consistency, the lower its degree of wetness and the more

Fig. 3. PCA loading plot of the six emulsions and four solutions.

45
P. Dubuisson et al. Colloids and Surfaces A 536 (2018) 38–46

difficult its spreading. On the other hand, the second principal com- participation and contribution to the experimental work. This work was
ponent could be assimilated to an axis representing the stickiness supported by the Haute-Normandie region.
property of the residual product film. Stickiness appears as clearly un-
related to the other attributes. References
Since the products appear to be well-distributed on the loading plot
along F1 and F2, it can be concluded that the selected attributes of this [1] M. Chappat, Some applications of emulsions, Colloids Surfaces A: Physicochem.
study are relevant to discriminate and characterize the texture prop- Eng. Asp. 91 (1994) 57–77.
[2] B.A. Salka, Choosing emollients, Cosmet. Toilet. 112 (10) (1997) 101–106.
erties of such products. The PCA plot clearly points out the effect of [3] G. Savary, M. Grisel, C. Picard, Impact of emollients on the spreading properties of
xanthan in emulsion as compared to its effect in aqueous phase. The cosmetic products: a combined sensory and instrumental characterization, Colloids
cluster formed by the solutions containing 0.3, 0.7 and 1% of xanthan is Surf. B: Biointerfaces 102 (2013) 371–378.
[4] P. Landa, F. Lam, R. Rothman, D. Howard, A. Gestmann, Glycerin and hydroxyethyl
wider than the one formed by the corresponding emulsions. As a con- urea: comparing two skin moisturizers, Cosmet. Toilet. 119 (10) (2004) 79–88.
sequence, there is a similar but lesser impact of the content of xanthan [5] J.W. Wiechers, Comparing instrumental and sensory measurements of skin moist-
in emulsions in comparison with aqueous phases. Hence, it appears that urization, Cosmet. Toilet. 114 (2) (1999) 29–34.
[6] J.M. Carey, B. Moran, F. Shuster, B. Vondruska, A new formulator’s tool for cus-
when xanthan is present in emulsions, its impact is minimized. It is a
tomizing sensory properties, Cosmetics and Toiletries 123 (7) (2008) 57–66.
quite unforeseen conclusion because one could suppose that the effect [7] L. Gilbert, C. Picard, G. Savary, M. Grisel, Impact of polymers on texture properties
of xanthan in emulsion would be enhanced since the xanthan in of cosmetic emulsions: a methodological approach, J. Sens. Stud. 27 (5) (2012)
392–402.
emulsion is actually more concentrated than in solution (due to the
[8] A.M. Dimuzio, E.S. Abrutyn, M.Y. Cantwell, Correlating sensory perception to the
presence of the oil phase). Indeed, for the emulsion XG1%, for example, rheological parameters of emulsions: a predictive model for future product devel-
its aqueous phase contains 1.11% of xanthan in comparison with the opment? J. Cosmet. Sci. 56 (5) (2005) 356–358.
solution that really contains 1% of xanthan, thus it could be assumed [9] T. Moravkova, P. Stern, Rheological and textural properties of cosmetic emulsions,
App. Rheol. 21 (3) (2011) 35200.
that the textural properties brought by the gum would be greater in the [10] J.W. Wiechers, V.A.L. Wortel, Making sense of sensory data, Cosmet. Toilet. 115 (3)
case of the emulsion. Such a hypothesis was not observed in our study. (2000) 37–45.
[11] V.A.L. Wortel, C. Verboom, J.W. Wiechers, M.-C. Taelman, S. Leonard, T.F. Tadros,
Linking sensory and rheology characteristics, Cosmet. Toilet. 120 (4) (2005) 57–66.
5. Conclusion [12] M. Meilgaard, G.V. Civille, B.T. Carr, Sensory Evaluation Techniques, 4th edition,
CRC Press, Boca Raton, 2006.
A specific terminology, well adapted to the study of cosmetic [13] N.O. Schwartz, Adaptation of the sensory texture profile method to skin care pro-
ducts, J. Texture Stud. 6 (1975) 33–42.
emulsions and solutions containing xanthan gum as texturing agent, [14] A.S. Szczesniak, Classification of textural characteristics, J. Food Sci. 28 (4) (1963)
was developed. The corresponding lexicon, based on physical percep- 385–389.
tions and highly detailed evaluation procedures and notation scales, is [15] M.E. Parente, A.V. Manzoni, G. Ares, External preference mapping of commercial
antiaging creams based on consumers’ responses to a check-all-that-apply question,
an accurate and efficient instrumental tool for sensory analysis that
J. Sens. Stud. 26 (2) (2011) 158–166.
enables reliable evaluations. The methodology was applied to seven oil- [16] H. Stone, J. Sidel, S. Oliver, A. Woolsey, R.C. Singleton, Sensory evaluation by
in-water emulsions containing various amounts of (1) xanthan and (2) quantitative descriptive analysis, Food Technol. 28 (11) (1974) 24–34.
[17] A.M. Muñoz, G.V. Civille, R.C. Hootman (Ed.), The Spectrum Descriptive Analysis
oil phase as well as to five solutions with xanthan gum content varying
Method. In Manual on Descriptive Analysis Testing for Sensory Evaluation, ASTM
from 0.3 to 2%. The results highlighted a high product discrimination, a Press, PA, 1992.
great consensus between assessors and a good repeatability reached [18] I. Capron, Traitement Thermique Des Mouts De Fermentation Et Organisation
through an intensive training and the use of appropriate references. The Moleculaire Du Xanthane, Consequences Rheologiques. PhD Thesis, Université de
Rouen, 1996.
PCA emphasized the sensory contribution of each parameter to the [19] I. Nor Hayati, Y.B. Che Man, C.P. Tan, I. Nor Aini, Droplet characterization and
texture of emulsions and aqueous phases. Increasing the oil phase in stability of soybean oil/palm kernel olein O/W emulsions with the presence of se-
emulsions mainly enhances the consistency, grease degree and residual lected polysaccharides, Food Hydrocoll. 2 (2009) 233–243.
[20] AFNOR, NF EN ISO 21149. Cosmétiques- Microbiologie – Dénombrement et
stickiness of the creams. The amount of xanthan in solutions also greatly détection des bactéries aérobies mésophiles (2009).
influences the attributes before, during and after application on the [21] AFNOR, NF EN ISO 16212. Cosmétiques – Microbiologie – Dénombrement des le-
assessors’ skin. Moreover, the present study establishes consistent linear vures et des moisissures (2011).
[22] G.V. Civille, C.A. Dus, Evaluating tactile properties of skincare products: a de-
relationships according to the concentration in xanthan for five attri- scriptive analysis technique, Cosmet. Toilet. 106 (5) (1991) 83–88.
butes: integrity of shape, penetration force, wetness, ease of spreading and [23] I.S. Lee, H.M. Yang, J.W. Kim, Y.J. Maeng, C.W. Lee, Y.S. Kang, H.Y. Kim,
gloss. Interestingly, the effect of xanthan in emulsions is similar but Terminology development and panel training for sensory evaluation of skin care
products including aqua cream, J. Sens. Stud. 20 (2005) 421–433.
obviously diminished when compared to polymer solutions. Further [24] ASTM Standard E1490-03, Standard Practice for Descriptive Skinfeel Analysis of
research will be carried out to understand better how the emulsion Creams and Lotions (ASTM International). PA: West Conshohocken (2003).
properties govern the textural perception of cosmetic creams especially [25] A.M. Muñoz, G.V. Civille, Universal, product and attribute specific scaling and the
development of common lexicons in descriptive analysis, J. Sens. Stud. 13 (1)
considering the microstructure, the oil droplet size and distribution in
(1998) 57–75.
the continuous aqueous phase. [26] J.A. Close, Men’s skin care, Cosmet. Toilet. 109 (2) (1994) 61–65.
[27] A.V. Rawling, Ethnic skin types: are there differences in skin structure and function?
Acknowledgments Int. J. Cosmet Sci. 28 (2) (2006) 79–93.
[28] T. Couronne, A study of assessors’ performance using graphical methods, Food
Qual. Prefer. 8 (5-6) (1997) 359–365.
The authors would very much like to thank the assessors for their

46