cosmetics

Article
Multi-Response Optimization in the Formulation of a
Topical Cream from Natural Ingredients
Gertrude Eleonore DJIOBIE TCHIENOU 1, *, Roli Karole TSATSOP TSAGUE 1 ,
Therese Florence MBAM PEGA 1 , Vera BAMA 1 , Albert BAMSECK 2 ,
Selestin DONGMO SOKENG 2 and Martin Benoît NGASSOUM 1
1 Department of Applied Chemistry, National School of Agro-Industrial Sciences, University of Ngaoundere,
P.O. Box 455 Ngaoundere, Cameroon; rolitsatsop@[Link] (R.K.T.T.); mbam@[Link] (T.F.M.P.);
verabama@[Link] (V.B.); ngassoum@[Link] (M.B.N.)
2 Department of Biological Sciences, Faculty of Sciences, Ngaoundere University,
P.O. Box 454 Ngaoundere, Cameroon; sedrickbamseck@[Link] (A.B.); dsokeng@[Link] (S.D.S.)
* Correspondence: djiobie@[Link]

Received: 1 November 2017; Accepted: 29 December 2017; Published: 5 January 2018

Abstract: The aim of this research was to study the effect of local raw materials on the formulation
of a base cream formulation and determine the optimum proportion of each material that gives
the required properties. Physicochemical properties of cream formulations can be affected by their
viscosity, spreadability, and particle size. The quality of the base cream is directly linked to the basic
material used in the formulation. Screening of independent factors, namely oil phase (sesame oil,
soybean oil, and liquid paraffin), aqueous phase (Aloe vera gel, propylene glycol, and glycerol), and
surfactant (soy lecithin, tween, and soy lecithin/tween) was done to choose the best raw material
required for the preparation of the base cream. Based on the screening criteria, sesame oil, Aloe vera
gel, and soy lecithin were chosen as the best local raw materials. Using a multi-response optimization,
the mixing fractions of sesame oil, Aloe vera gel, and soy lecithin were found to be 24%, 28%, and 10%,
respectively. This base cream can be used as a suitable matrix for formulation in the cosmetic and
pharmaceutical industries.

Keywords: local raw materials; formulation; base cream; multi-response optimization

1. Introduction
Topical products are liquid or semisolid preparations, such as ointments, lotions, gels, and
creams [1]. Creams are usually emulsions, which are thermodynamically unstable and consist either
of two-phase systems (oil in water or water in oil), in which one is dispersed in the form of small
droplets throughout the other [2]. To produce commercial products with sufficiently long shelf
lives to environmental stresses, it is necessary to incorporate stabilizers, such as thickening agents,
gelling agents, weighting agents, ripening inhibitors, and emulsifiers [3]. The emulsifying agent
possesses hydrophilic and hydrophobic groups [4], adsorbed at the interface of water and oil, and
reduces the interfacial tension. Emulsifiers are particularly important ingredients for forming stable
emulsions with appropriate shelf lives and functional attributes. Most industrial emulsifiers, currently
used to stabilize oil-in-water emulsions, are synthetic surfactants (such as Tweens and Spans [5]) or
animal-based emulsifiers (such as gelatin, egg protein, whey protein, and caseinate [6]). However,
there is an increasing consumer demand for more natural, environmentally friendly, and sustainable
commercial products [7]. Many manufacturers are reformulating their products to replace the synthetic
surfactants with more label-friendly natural alternatives [8] or to replace animal proteins from with
plant proteins [9,10]. Generally, manufacturers would often like to create new products entirely from
natural ingredients so that they can make “all-natural” claims on their labels. On the other hand, the

Cosmetics 2018, 5, 7; doi:10.3390/cosmetics5010007 [Link]/journal/cosmetics

Cosmetics 2018, 5, 7 2 of 14

physical stability of emulsions is an important factor when pharmaceutical formulations are considered
as drug delivery concepts.
In recent years, the interest in the use of natural polymers in pharmaceutical, nutraceutical,
and cosmetic formulations has markedly increased [11]. Lowering interfacial tension eases droplet
break-up, and interfacial viscosity provides stability. Silva et al. and Alvarez Lorenzo et al. have
reported the use of protein-based emulsion hydrogels [12,13], while Tang et al. have used soy protein
isolate for stabilizing emulsion hydrogels [14].
Lecithin is a naturally occurring zwitterionic phospholipid-based liquid surfactant (extracted
from egg and soybean). It has been extensively studied as a structuring agent for food, pharmaceutical,
and cosmetic applications [15]. Lecithin derived from soybean has been reported to be biocompatible
and has been used for transdermal drug delivery applications. Lecithin based on organogels has been
reported by many researchers [16], but emulsion hydrogels have not been explored much yet.
Aloe vera Burm (liliaceae family) is an imperative functional ingredient exhibiting remarkable
biological efficacy to the cosmetic, pharmaceutical, and food industries. For centuries, this plant has
been used for its medicinal and therapeutic functions without scientific analysis for its health, beauty,
and skin care properties. The leaf consists of pericyclic cells and the inner central area of the leaf (i.e.,
the gel) along with the leaf extract, juice, and polysaccharides. Aloe vera gel is used as a base in many
cosmetic formulations.
Emulsions are widely used for the treatment of dry skin and emollient applications. A cosmetic
formulation including the active principle of strictly natural origin is designed to protect the skin
against exogenous or endogenous harmful agents. Due to the importance of soy lecithin and the
skin care benefits of Aloe vera, the purpose of this study was to develop a stable cream emulsion with
local raw materials. The effects of different factors of each phase on the stability and viscosity of the
emulsion were analyzed. A multi-response optimization was done to obtain a combined optimum
proportion of local materials in each phase. In this methodology, the study of an ingredient’s effect
on viscosity, particle size, and spreadability is an attempt to find the formulation that produces the
best response.

2. Materials and Methods

2.1. Materials
Sesame and soybean oil were extracted by the soxhlet method. Lecithin was obtained by ethanolic
extraction from soy residue after the defatting of soy powder with hexane. Matured Aloe vera
leaves were purchased from the local market of Bini-dang, Ngaoundere, Cameroon. All of the
other reagents, such as liquid paraffin, glycerol, Tween 80, and propylene glycol, were purchased from
VWR International Co (VWR).

2.2. Methods

2.2.1. Preparation of local materials for formulation

Extraction of sesame and soybeans oil: Sesame and soybean seeds were purchased from a local
market of Bini-dang, Ngaoundere. The seeds were sorted to eliminate damaged grains and dirt. Seeds in
good condition were washed thoroughly with clean water and sun dried in the open. All apparatus
were washed and oven dried, and the soxhlet apparatus was set up in readiness for the experiment.
The seeds were grounded mechanically, while soybean seeds were de-husked before grinding. Five
hundred grams of each powdered sample was placed in a thimble made from thick filter paper and
inserted into the center of the extractor. The soxhlet (1 L capacity) equipped with a condenser was
placed onto a flask containing the hexane. The soxhlet was heated to 65 ◦ C and allowed to reflux
for about 8 h. It was then removed from the tube, dried in the oven, cooled in the desiccators, and
weighed again to determine the amount of oil extracted [17].
Cosmetics 2018, 5, 7 3 of 14

For lecithin: Lecithin was obtained by ethanolic extraction from soy residue after the defatting of soy
powder with hexane. The soxhlet was heated to 80 ◦ C and allowed to reflux for about 24 h.

Obtention of Aloe vera gel protocol described by [18]: Leaves of Aloe vera were cut, washed, and
then sliced an inch on both the upper and lower sides. The leaves were further cut and the pulp was
removed thereafter. The pulp obtained was further crushed in a mechanical crusher. After the crushing
of the pulp it was filtered in order to remove the attached fibres. The obtained sap was stored for
future use.

Additional information: The viscosity of the sesame oil was 54.2 cP. The viscosity of the soybean oil
was 39.5 cP. The moisture content of the Aloe vera gel was 92.23%.

2.2.2. Screening of Factors of Each Phase

The different variables used in this study are shown in Table 1.

Table 1. Different variables.

Phase (Percentage) Material Coded Variable Level of Variable

Soybean oil 1
Oil phase (20%) Sesame oil X1 2
Liquid paraffin 3
Aloe vera gel 1
Aqueous phase (30%) Glycerol X2 2
Propylene glycol 3
Lecithin 1
Emulsyfing phase (8%) Tween X3 2
Lecithin/tween 3

In fact, the amounts of the three components of the emulsion (oil phase (X1 ), aqueous phase
(X2 ), and emulsifying phase (X3 ) (Table 1)) were selected as the factors to systematically optimize
the dependent variables (creaming index, viscosity, and spreadability). All other formulation and
processing variables (Water 31.7%, Acidifiant 0.3%, Beeswax 10%) were kept invariant throughout the
study. The levels of the three factors were selected on the basis of the preliminary studies carried out
before implementing the experimental design. The screening plan proposed by the STATGRAPHICS
Centurion program gave 27 experiments.

2.2.3. Experiment for the Optimization of the Base Cream Formulation

Screening was done to permit us to choose the best mixture with the selected local raw materials
of the oil, aqueous, and emulsifying phases. With them, the following domain with constraints (Table 2)
was used. It was defined according to previous experiments and the literature review.

Table 2. Implicit Domain for optimization plan.

Raw Material Abbreviation Lower Limit (%) Upper Limit (%)

Selected oil phase X1 20 25
Selected aqueous phase X2 28 32
Selected emulsifying
X3 8 10
phase

Based on the above implicit plan proposed by the STATGRAPHICS Centurion program, fifteen
experiments were obtained for optimization. The responses were spreadability, viscosity, and
particle size.
Cosmetics 2018, 5, 7 4 of 14

2.2.4. Preparation of Emulsion Base

The emulsion preparation consisted in the simultaneous mixture of phases. Eight grams of
emulsifier and 10 g of beeswax were dissolved in 20 g of oil phase (Part A) and heated to 75 ◦ C. Water
(31.7 g) and citric acid (0.3 g) were dissolved in 28 g of the aqueous phase (Part B) and heated to 75 ◦ C.
After heating, the aqueous phase was gradually added to the oil phases and stirred with a high shear
mixer for 5 min. Once the emulsion presented a uniform appearance, it was mixed manually [19].

2.2.5. Response Parameters

The response parameters studied included an analysis of the creaming index, viscosity,
spreadability, and particle size.
All analyses were done 24 h after the preparation of different emulsions at room temperature.

Creaming Index
Direct optical observations were employed to determine the instantaneous heights of the emulsion
and the aqueous phase inside the glass vessel. This was donewith the help of a graduated scale. The
creaming index (CI) was estimated using the formula: %CI = CC CT ∗ 100, where CC is the total height
of the cream layer, and CT is the total height of the emulsion layer [20].

Viscosity
Viscosity was determined with the help of a CAP-2000 Brookfield viscometer using the
method [21]. Test samples were taken in clean and dry 250 mL beakers, and the viscosity of a
test sample was determined by the standard operating procedure for the Viscometer using spindle
N◦ 4. This spindle was used to determine the viscosity of the sample at 60 rpm. The reading at 100%
torque was noted. Samples were measured at 25 ± 1 ◦ C. The values were read in centipoise.

Spreadability
The spreadability of the formulation was determined by an apparatus which was set up in the
laboratory. The cream emulsion was placed between two glass slides, a 1000 g mass was placed on
the slides for 5 min to compress the sample to a uniform thickness, and excess cream was scraped off.
A 120 g mass, M, was tied to the upper slide. The time in seconds required to move the slides across a
distance of 10 cm was taken as the measure of spreadability [22]. The following formula was used for
the calculation of Spreadability:
M×L
S=
T
where S is Spreadability, M is the mass tied to the upper slide in g (120 g), L is the length of the slide in
10 cm = 10 × 10−2 m, and T the time taken to separate two slides. Spreadability was recorded in g·m/s.

Particle Size Determination

The particle size of the emulsions was determined using a Malvern particle size analyser
(Mastersizer 2000S, Malvern Instrument Ltd., Malvern, UK). Emulsions were added, in a dropwise
manner, to deionized water in the dispersion cell of the instrument. The optical parameters selected
were as follows: a relative refractive index of 1.449, a particle absorbance of 0, and a continuous
phase refractive index of 1.33. Each sample was analyzed three times and the data are presented as
the average. The average droplet size was characterized by mean diameters related to the volume.
All measurements were carried out at 25 ◦ C. The results of the particle size are expressed as Z-average
size [23].
Cosmetics 2018, 5, 7 5 of 14

2.2.6. Microstructure Observation

The morphology of some selected emulsions was observed using an optical microscope (Axiophot,
Germany) at a 40× magnification. Prior to the microscopic observation, the emulsion samples were
shaken gently. Subsequently, a drop of the emulsion was placed onto a microscope slide and covered
with a cover slip. Photomicrography images of the emulsion were captured using digital image
processing software.

2.2.7. Statistical Analysis

Four experiments were carried out at each experimental design point and the mean values
are stated as observed responses. Experimental runs were randomized to minimize the effects of
unexpected variability in the observed responses. Comparison of means was performed by one-way
analysis of variance (ANOVA) followed by Duncan’s test. Statistical analyses (p < 0.05) were performed
using Statgraphics centurion software (Version XVI.I, Statgraphics Technologies Inc. The Plains,
VA, USA).

3. Results and Discussion

3.1. Screening of Base Cream Materials

The results of the analysis of different formulation bases aimed at choosing the best oil, aqueous,
and emulsifying phases are shown in Table 3. The properties considered during the analysis were the
creaming index, the spreadability, and the viscosity. The experimental results obtained were between
0 and 28.33%, 9.0 and 31.02 g·cm/s, and 290 and 480 cP (centipoise) for the creaming index, the
spreadability, and the viscosity, respectively. It is important to analyze each response individually to
obtain good properties for the emulsion base.

Table 3. Screening design for different ingredient phases of the base cream formulation.

Oil Aqueous Creaming Spreadability Viscosity

Runs Emulsifying
Phase Phase Index (%) (g·cm/s) (cP)
1 1 3 1 0.0 ± 0.0 31.02 ± 1.12 360 ± 10
2 2 3 1 0.0 ± 0.0 20.99 ± 1.01 340 ± 7
3 1 1 1 8.33 ± 0.12 20.46 ± 1.09 320 ± 5
4 1 2 1 0.0 ± 0.0 22.39 ± 1.15 328 ± 8
5 2 1 1 16.66 ± 0.14 17.87 ± 1.15 415 ± 12
6 2 2 1 28.33 ± 0.10 15.07 ± 0.51 425 ± 11
7 3 1 1 25.00 ± 0.11 22.60 ± 1.14 229 ± 8
8 3 2 1 16.67 ± 0.14 21.57 ± 1.17 275 ± 6
9 3 3 1 10.00 ± 0.05 21.99 ± 0.25 290 ± 4
10 1 1 2 20.00 ± 0.13 9.043 ± 0.05 370 ± 6
11 1 2 2 1.66 ± 0.05 20.62 ± 1.01 367 ± 5
12 1 3 2 1.66 ± 0.06 22.18 ± 1.10 315 ± 11
13 2 1 2 15.67 ± 0.17 12.31 ± 0.053 480 ± 14
14 2 2 2 8.33 ± 0.02 14.90 ± 0.95 410 ± 11
15 2 3 2 1.66 ± 0.05 19.27 ± 1.10 419 ± 9
16 3 1 2 20.00 ± 0.17 20.44 ± 1.10 420 ± 7
17 3 2 2 1.66 ± 0.03 22.60 ± 1.11 412 ± 10
18 3 3 2 0.0 ± 0.0 19.64 ± 1.12 390 ± 9
19 1 1 3 8.33 ± 0.11 18.37 ± 1.10 415 ± 11
20 1 2 3 0.83 ± 0.01 18.96 ± 1.09 419 ± 12
21 1 3 3 0.0 ± 0.10 15.70 ± 0.05 417 ± 10
22 2 1 3 15.00 ± 0.11 13.75 ± 0.05 412 ± 8
23 2 2 3 15.00 ± 0.10 21.00 ± 1.03 421 ± 10
24 2 3 3 3.33 ± 0.09 22.19 ± 1.07 450 ± 14
25 3 1 3 13.33 ± 0.14 22.39 ± 1.12 409 ± 6
26 3 2 3 1.60 ± 0.02 19.64 ± 1.08 419 ± 8
27 3 3 3 8.33 ± 0.09 17.70 ± 1.05 290 ± 2
 Cosmetics 2018, 5, 7 6 of 14

24 2 3 3 3.33 ± 0.09 22.19 ± 1.07 450 ± 14

25 3 1 3 13.33 ± 0.14 22.39 ± 1.12 409 ± 6
26
Cosmetics 2018, 5,37 2 3 1.60 ± 0.02 19.64 ± 1.08 419 ±6 of
8 14
27 3 3 3 8.33 ± 0.09 17.70 ± 1.05 290 ± 2

3.1.1. Effect of Different Phases on Creaming Index

3.1.1. Effect of Different Phases on Creaming Index
The creaming index was found to be in the range of 0 to 28.33% depending on the material used
The creaming index was found to be in the range of 0 to 28.33% depending on the material used
at each phase (Table 3). The Pareto chart indicates that each material phase possesses a significant
at each phase (Table 3). The Pareto chart indicates that each material phase possesses a significant
influence on the creaming index. The influence of the different factors on the creaming index are
influence on the creaming index. The influence of the different factors on the creaming index are
shown in Figure 1.
shown in Figure 1.

Aloe vera
Glycerol 3
Propylene glycol

Soy
lecithin/Tween
Soy lecithin 2
Tween

Soybean
1 Liquid paraffin
sesame oil

-8 -6 -4 -2 0 2 4 6 8

Figure 1. Effect of ingredient phases on the creaming index.

Figure 1. Effect of ingredient phases on the creaming index.

In this figure, it can be observed that the effects of the sesame oil, soy lecithin, glycerol, Aloe vera
In this figure, it can be observed that the effects of the sesame oil, soy lecithin, glycerol, Aloe vera
gel, and soy lecithin/tween combination contribute to reducing the creaming index to a much lower
gel, and soy lecithin/tween combination contribute to reducing the creaming index to a much lower
value than those of the soybean oil, tween, liquid paraffin, and propylene glycol. Therefore, sesame oil,
value than those of the soybean oil, tween, liquid paraffin, and propylene glycol. Therefore, sesame
Aloe vera gel, and the combination of soy lecithin/tween considerably decrease the creaming index,
oil, Aloe vera gel, and the combination of soy lecithin/tween considerably decrease the creaming index,
that is, the degree of destabilization of the emulsion. This can be due to the fact that soy lecithin has
that is, the degree of destabilization of the emulsion. This can be due to the fact that soy lecithin has
two tails, which are C16–C18 in length, and one of the tails has two cis unsaturations [24], which
two tails, which are C16–C18 in length, and one of the tails has two cis unsaturations [24], which
stabilizes better the emulsion oil in water [25]. In fact, soy lecithin has a low tendency to desorb, which
stabilizes better the emulsion oil in water [25]. In fact, soy lecithin has a low tendency to desorb,
fortifies the interfacial film, and the large headgroup of Tween provides steric repulsions between
which fortifies the interfacial film, and the large headgroup of Tween provides steric repulsions
the oil droplets and prevents their coalescence [26]. On the other hand, soy lecithin alone decreases
between the oil droplets and prevents their coalescence [26]. On the other hand, soy lecithin alone
the creaming index, but the combination of lecithin and tween decreases the creaming index more.
decreases the creaming index, but the combination of lecithin and tween decreases the creaming
Soy lecithin and tween blends show a synergistic effect, i.e., their combination is an effective emulsifier,
index more. Soy lecithin and tween blends show a synergistic effect, i.e., their combination is an
but neither soy lecithin or tween is effective on its own. So, it will be necessary to combine both of
effective emulsifier, but neither soy lecithin or tween is effective on its own. So, it will be necessary
them for good cream stability.
to combine both of them for good cream stability.
3.1.2. Effect of Different Phases on Spreadability
3.1.2. Effect of Different Phases on Spreadability
Spreadability is the ability of a cream to spread on the skin. It plays an important role in the
Spreadability is the ability of a cream to spread on the skin. It plays an important role in the
administration of a standard dose of a medicated formulation to the skin and the efficacy of a topical
administration of a standard dose of a medicated formulation to the skin and the efficacy of a topical
therapy. If spreadability decreases, the topical cream is good because applying it to the skin is easy [27].
therapy. If spreadability decreases, the topical cream is good because applying it to the skin is easy
The spreadability values were found to be in the range of 9.0 to 31.02 g·cm/s, depending on the
[27]. The spreadability values were found to be in the range of 9.0 to 31.02 g·cm/s, depending on the
material of each phase (Table 3). The influence of the different factors on spreadability is shown in
material of each phase (Table 3). The influence of the different factors on spreadability is shown in
Figure 2.
Figure 2.
It can be observed that synergism could be obtained by using a combination of sesame oil, soy
lecithin, and Aloe vera gel. This effect can be explained by the fatty acid present in the sesame oil and
soy lecithin. In fact, sesame oil has 96% of total fatty acids [27] and lecithin has 5.68% free fatty acids.
The spreadability of creams decreases with increasing content of unsaturated fatty acids [28].
 Glycerol
Aloe Vera 3
Cosmetics 2018, 5, 7 Propylen glycol7 of 14
Cosmetics 2018, 5, 7 7 of 14

soy lecithin/tween
Soy lecithin 2
Glycerol
Tween
Aloe Vera 3
paraffine Propylen glycol
1 Soybean oil
sesame oil soy lecithin/tween
Soy lecithin 2
Tween
-10 -5 0 5 10 15 20

paraffine
Figure 2. Effect of ingredient phases on spreadability.
1 Soybean oil
sesame oil
It can be observed that synergism could be obtained by using a combination of sesame oil, soy
lecithin, and Aloe vera gel. This effect can be explained by the fatty acid present in the sesame oil and
-10 -5 0 5 10 15 20
soy lecithin. In fact, sesame oil has 96% of total fatty acids [27] and lecithin has 5.68% free fatty acids.
The spreadability of creams decreases
Figure 2. Effectwith increasing
of ingredient content
phases of unsaturated fatty acids [28].
on spreadability.
Figure 2. Effect of ingredient phases on spreadability.

3.1.3. Effect of Different Phases on Viscosity

3.1.3. It
Effect of Different
can be observedPhases on Viscosity
that synergism could be obtained by using a combination of sesame oil, soy
Viscosity
lecithin, was vera
and Aloe found toThis
gel. range fromcan
effect 290be
toexplained
480 cP depending on the
by the fatty material
acid presentofin
each
thephase
sesame(Table 3).
oil and
Viscosity was found to range from 290 to 480 cP depending on the material of each phase (Table 3).
The
soy Pareto
[Link] indicates
In fact, sesamethat
oileach phase
has 96% ofpossesses
total fattyaacids
significant influence
[27] and lecithinon viscosity.
has Thefatty
5.68% free influence
acids.
The Pareto chart indicates that each phase possesses a significant influence on viscosity. The influence
of
Thethespreadability
different factors on viscosity
of creams is shown
decreases in Figure [Link] of unsaturated fatty acids [28].
with increasing
of the different factors on viscosity is shown in Figure 3.

3.1.3. Effect of Different Phases on Viscosity

Glycerol
Viscosity was found toVera
Aloe range from 290 to
3 480 cP depending on the material of each phase (Table 3).
Propylen glycol
The Pareto chart indicates that each phase possesses a significant influence on viscosity. The influence
of the different factors on viscosity is shown in Figure 3. Lecithin/Tween
Lecithin 2
Tween

Glycerol Liquid paraffin

Soybean oil Aloe Vera 13
sesame oil Propylen glycol

Lecithin/Tween
-50 -40 -30 -20 -10
Lecithin 2 0 10 20 30 40 50 60
Tween

Figure 3. Effect
Figure 3. Effect of
of ingredient
ingredient phases
phases on
on viscosity.
viscosity.
Liquid paraffin
Soybean oil 1
Viscosityisisaameasure
Viscosity measure of of the
the resistance
resistance of of aa fluid
fluid to to flow.
[Link]
Themore
sesame oil moreviscous
viscous aa liquid,
liquid, the
the greater
greater
is the
is the quantity
quantity of of energy
energy required
required to to produce
produce aa desired
desired statestate of
of flow.
flow. Thereby,
Thereby, liquid
liquid paraffin
paraffin and
and
-50 -40 -30 -20 -10 0 10 20 30 40 50 60
propylene glycol have viscosities that are not interesting
propylene glycol have viscosities that are not interesting for our desired [Link] our desired product.
Onthe
On theother
other hand,
hand, soysoy lecithin localizes
lecithin theon the surface of the emulsion particles, reduces
Figure localizes oningredient
3. Effect of surface of the
phases onemulsion
[Link], reduces interfacial
interfacial
free energy,free energy,
provides provides abarrier
a mechanical mechanical barrier to[29],
to coalescence coalescence
and reduces [29],viscosity.
and reducesHowever,viscosity.
the
However,
addition the
of tween
Viscosity addition
is aresults
measure of
in oftween
a better results in
end product,
the resistance a better
perhaps
of a fluid end product,
due The
to flow. perhaps
to synergistic
more viscous due
effects to synergistic
[30]. The
a liquid, cream
the greater
effects
is the quantity of energy required to produce a desired state of flow. Thereby, liquid paraffintype
retained [30].
the The cream
desirable retained
effects of the desirable
lecithin but effects
the of
lecithin lecithin
did but
not the
alter lecithin
the type did
of not alter
emulsion the
in any
and
of emulsion
significant
propyleneor in any significant
detrimental
glycol way.
have viscositiesor detrimental way.
that are not interesting for our desired product.
Viscosity
Viscosity
On the other decreases
decreases with
soyAloe
hand,with Aloe vera localizes
vera
lecithin gel. This
gel. This on is mainly
is mainly due to
due
the surface to the
ofthe presence
thepresence
emulsionof ofparticles,
polysaccharides
polysaccharides
reduces
composed
composed of
of a
a mixture
mixture of
of acetylated
acetylated glucommannans
glucommannans that
that lose
lose their
their
interfacial free energy, provides a mechanical barrier to coalescence [29], and reduces viscosity. properties
properties after
after extraction,
extraction,
apparently
apparently
However, due due addition
the to enzymatic
to enzymatic degradation
degradation
of tween [31].
results [31].
in a It Itbetter
is important
is important to associate
to
end product, associate
perhaps it with
it with another
dueanother gel to
gel
to synergistic to
maintain
maintain its viscosity.
its viscosity.
effects [30]. The cream retained the desirable effects of lecithin but the lecithin did not alter the type
The screening
of emulsion in anyof factors allowed
significant [Link] oil for the oily phase, Aloe vera gel for the
us to choose
or detrimental
aqueous phase, and
Viscosity the combination
decreases with Aloe of soygel.
vera lecithin/tween for due
This is mainly the emulsifier. We willofadd
to the presence natural gum
polysaccharides
from local plants to stabilize the Aloe vera gel.
composed of a mixture of acetylated glucommannans that lose their properties after extraction,
apparently due to enzymatic degradation [31]. It is important to associate it with another gel to
maintain its viscosity.
Cosmetics 2018, 5, 7 8 of 14

3.2. Correlation between Responses

Correlation studies of different responses are given in Table 4.

Table 4. Correlation of different responses.

Responses Coefficient Correlation Goal

Height Viscosity 0.71 Moderately strong
Spreadability Viscosity 0.95 Strong
Spreadability Height 0.66 Average

From the table above, a strong inverse correlation was observed between spreadability and
viscosity. It is in accordance with works which showed that when the viscosity of a formulation
increases, the spreadability decreases and vice versa [32].

3.3. Optimization of Base Cream Formulation

The results for the optimization of the formulation matrix are shown on the table below (Table 5),
we used oil phase (X1 : sesame oil), aqueous phase (X2 : Aloe vera gel), and emulsifying phase (X3 : soy
lecithin/tween). The responses observed in the course of these analyses are spreadability, viscosity,
and particle size. The experimental results obtained are between 28.95 and 154.45 g·cm/s, 83 and
840 cP (centipoise), and 8.71 and 208.93 for spreadability, viscosity, and particle size, respectively.
The maximum value for spreadability (154.45 g·cm/s) was found for Experiment 2. The maximum
value for viscosity (840 cP) was seen for Experiment 15, and the maximum value for particle size
(208.93) was obtained in Experiment 13. Consequently, it was indispensable to realize an optimization
in order to obtain the desired properties of the base cream.

Table 5. Experimental design.

Responses
Variables Level
Viscosity Spreadability Particle Size
N◦ X1 X2 X3 Observed. Adjusted. Observed. Adjusted. Observed. Adjusted.
1 24 28 8 734 785.4 28.9 34.5 34.6 21.8
2 20 32 8 293 276.0 154.4 140.3 22.9 25.1
3 22 28 10 640 611.6 54.5 57.7 8.7 3.7
4 20 30 10 100 382.8 34.9 24.9 34.6 25.0
5 22.75 28.75 8.5 760 747.8 46.3 34.2 104.7 106.3
6 20.75 30.75 8.5 218 221.4 57 65.7 138.0 140.7
7 21.75 28.75 9.5 220 240.2 54.5 45.6 138.0 142.0
8 20.75 29.75 9.5 83 54.1 38.9 39.9 158.4 158.7
9 22 30 8 320 332.7 46.3 48.2 60.2 64.5
10 23 28 9 386.7 406.3 35.4 36.8 69.1 77.0
11 20 31 9 240.3 264.4 45 51.9 69.1 77.4
12 21 29 10 426 473.6 40.2 49.5 79.4 98.3
13 21.5 29.5 9 284 253.1 42.3 42.62 208.9 186.3
14 20 32 8 266.7 785.4 132.3 34.5 30.2 21.8
15 24 28 8 840 276.0 35.6 140.3 11.4 25.1

Table 6 presents the significance of different effects of base cream models and the indicators for
the validation of the models for the different responses, respectively. Lack of fit was also given in order
to check the quality of the fitted models.
Cosmetics 2018, 5, 7 9 of 14
Cosmetics 2018, 5, 7 9 of 14

Table 6. Significance of different effects of base cream models and indicators of validations.
Table 6. SignificanceViscosity
of different effects of base cream models and indicators ofParticle
Spreadability validations.
Size
Parameters
Coefficient Probability Coefficient Probability Coefficient Probability
Viscosity Spreadability Particle Size
X1
Parameters 785.4 34.5 21.8
Coefficient Probability Coefficient Probability Coefficient Probability
X2 276.0 140.4 25.1
X13
X 785.4
13,733.3 34.5
155.1 21.8
−626.1
X2 276.0 140.4 25.1
X1 X× X2 −792.2
13,733.3
0.01 −156.9
155.1
0.007 164.5
−626.1
0.01
3
X ×
X1 × X2
1 X3 −26,590.8
−792.2 0.0009
0.01 −148.2
−156.9 0.2
0.007 1201.7
164.5 0.0009
0.01
X12 ×
X ×X X33 −26,590.8
−26,487.5 0.0009
0.0009 −148.2
−491.1 0.002
0.2 1302.3
1201.7 0.0008
0.0009
X × X
X1 × X2 × X3
2 3 − 26,487.5
32,404.4 0.0009
0.002 − 491.1
576.5 0.002
0.06 1302.3
2048.3 0.0008
0.002
X1 × X2 × X3 32,404.4 0.002 576.5 0.06 2048.3 0.002
X 1 × X2(X1 − X2)
X1 × X2 (X1 − X2 )
3013.8
3013.8
0.004
0.004
−287.2
−287.2
0.003
0.003
X11 ×
X ×XX33(X
(X11 −−XX33)) 14,610.4
14,610.4 0.002
0.002 −86.3
−86.3 0.002
0.002
X22 ×
X (X22 −−XX33))
× X33(X 16,964.6
16,964.6 0.001
0.001 −310.2
−310.2 0.0010
0.0010
R 2 98.25 95.44 96.92
R 2 98.25 95.44 96.92
R22 adj 95.09 92.02 91.39
R adj 95.09 92.02 91.39
Lack of fit 0.24 0.68 0.23
Lack of fit 0.24 0.68 0.23

3.3.1. Influence of Formulation on Viscosity

3.3.1. Influence of Formulation on Viscosity
The following equation shows the cubic model obtained after the analysis of viscosity.
The following equation shows the cubic model obtained after the analysis of viscosity.
Viscosity = 785.4X
Viscosity 1 + 276.0X
= 785.4X 2 + 13,733.3X
1 + 276.0X 3 −3 792.2X
2 + 13,733.3X − 792.2X 1 × X22 −
1 ×X 26,590.8X11××
− 26,590.8X − 26,487.5X
X3X–326,487.5X 2 2
×
× XX33+32,404.4X
+32,404.4X 1 ×
1× × 2X×
X2 X 3 +X3 + 3013.8X
3013.8X ×1 X
1 × X21(X − 2X(X − X2 ) +14,610.4X
2) 1+14,610.4X 1 × X3(X11−×
X3X
) 3+(X1 − X3 ) 2
16,964.6X
+ 16,964.6X
X3(X X3)2 − X3 )
2 2X−3 (X

The coefficient of determination (R2) obtained was 98.25% for viscosity. The p-value for lack of
The coefficient of determination (R2 ) obtained was 98.25% for viscosity. The p-value for lack of fit
fit was 0.05, which suggests that the model fits the experimental data. Concerning the contribution of
was 0.05, which suggests that the model fits the experimental data. Concerning the contribution of
different factors to viscosity in Figure 4 below, it is observed that the single emulsifying X3 (10.12) and
different factors to viscosity in Figure 4 below, it is observed that the single emulsifying X3 (10.12) and
interaction between the three mixtures X1 × X2 × X3 (23.88) have a positive effect on spreadability, and
interaction between the three mixtures X1 × X2 × X3 (23.88) have a positive effect on spreadability,
interaction between X1 × X3 (19.60%) and X2 × X3 (19.52) show the contrary.
and interaction between X1 × X3 (19.60%) and X2 × X3 (19.52) show the contrary.

X2*X3(X2-X3) 12.50
X1*X3(X1-X3) 10.77
X1*X2(X1-X2) 2.21
X1*X2*X3 23.88
X2*X3 -19.52
X1*X3 -19.60
X1*X2 -0.58
X3 10.12
X2 0.20
X1 0.58

-30 -20 -10 0 10 20 30

Figure 4. Contribution
Figure 4. Contribution of
of factors
factors to
to viscosity.
viscosity.

This means
This means that
that the
the binary
binary effects
effects of
of the
the oil
oil phase
phase and
and emulsifying
emulsifying phase,
phase, the
the oil
oil phase
phase and
and
aqueous phase, and the aqueous phase and emulsifying phase tend to reduce viscosity
aqueous phase, and the aqueous phase and emulsifying phase tend to reduce viscosity comparatively comparatively
toeach
to eachphase
phasetaken
takenindividually.
individually. This
This cancan be due
be due to fact
to the the that
fact the
thatoil
the oil phase
phase here ishere is sesame
sesame oil,
oil, which
which
has has
in its in its composition
composition a high of
a high content content of fatty
fatty acids thatacids
reducethat reduce viscosity.
viscosity. It was that
It was observed observed that
vegetable
vegetable oils usually have higher viscosity [33], and emulsions made from them
oils usually have higher viscosity [33], and emulsions made from them require a higher energy input require a higher
energy input with the result in an emulsion being is that it is less stable to the migration of water in
and out of the internal aqueous phase.
Cosmetics 2018, 5, 7 10 of 14

Cosmetics 2018, 5, 7 10 of 14
with the result in an emulsion being is that it is less stable to the migration of water in and out of the
internal aqueous phase.
Concerning viscosity, the range obtained, 320 to 734 cP, is slightly comparable to the values
Concerning viscosity, the range obtained, 320 to 734 cP, is slightly comparable to the values
obtained by [34], ranging from 129 to 361 cP. During their formulation, Gelucire 44/14, propylene
obtained by [34], ranging from 129 to 361 cP. During their formulation, Gelucire 44/14, propylene
glycol, and white petrolatum were used as the emulsifying, aqueous, and oil phase, respectively.
glycol, and white petrolatum were used as the emulsifying, aqueous, and oil phase, respectively. Also,
Also, the slight difference in value can be due to the ratio (0.05:10:60) used for the formulation. From
the slight difference in value can be due to the ratio (0.05:10:60) used for the formulation. From this,
this, our formulation base cream from local raw materials could be used as a matrix in the cosmetic
our formulation base cream from local raw materials could be used as a matrix in the cosmetic and
and pharmaceutics industries. This is because viscosity governs many properties of a formulation,
pharmaceutics industries. This is because viscosity governs many properties of a formulation, such as
such as spreadability and pourability of the product from the container [35].
spreadability and pourability of the product from the container [35].
3.3.2. Influence of Formulation on Spreadability
3.3.2. Influence of Formulation on Spreadability
The following equation shows the special cubic model obtained after the analysis of
The following equation shows the special cubic model obtained after the analysis of spreadability.
spreadability.
Spreadability = 34.5X
Spreadability + 140.3X
= 134.5X 2 + 155.0X
1 + 140.3X 3 − 156.9X
2 + 155.0X 1 × 1X×2 X
3 − 156.9X −2 −148.1X
148.1X1 ×
1 ×XX33− 491.0X22 ×× X3
− 491.0X
+X576.5X ×
3 + 576.5X X × X
1 1 ×2X2 × X 33

The coefficient
The coefficientof ofdetermination
determination(R (R22)) obtained
obtained was
was 92.02%
92.02% for
for spreadability.
spreadability. TheThe p-value
p-value forfor lack
lack
of fit was 0.68, which suggests that the model fits the experimental data. Concerning
of fit was 0.68, which suggests that the model fits the experimental data. Concerning the contribution the contribution
of different
of differentfactors
factors to
to spreadability
spreadability in
in Figure
Figure 55 below,
below,ititwas
wasobserved
observedthat
thatthethesingle
singleaqueous
aqueousphase phase
XX22 (8.24),
(8.24), the
theemulsifying
emulsifyingphase
phaseXX3 3(9.10),
(9.10),andandinteraction
interactionbetween
betweenthethethree
threemixtures
mixtures X1X× 1 ×XX2××X
2
X33
(33.84) have a positive effect on spreadability, and interaction between X × X (9.21),
(33.84) have a positive effect on spreadability, and interaction between X1 × X2 (9.21), X1 × X3 (8.74%),
1 2 X 1 × X 3 (8.74%),
and XX22 ×
and × XX33(28.82)
(28.82)show
showthethecontrary.
contrary.

X1X2X3 33.84

X2X3 -28.82

X1X3 -8.74

X1X2 -9.21

X3 9.10

X2 8.24

X1 2.03

-40 -30 -20 -10 0 10 20 30 40

Figure 5. Contribution
Figure 5. Contribution of
of factors
factors to
to spreadability.
spreadability.

This means
This means that
that the
the binary
binary effects
effects ofof the
the oil
oil phase
phase and
and aqueous
aqueous phase
phase and
and the
the oil
oil phase
phase and
and
emulsifying phase exert an antagonistic effect on spreadability. The antagonistic effect can
emulsifying phase exert an antagonistic effect on spreadability. The antagonistic effect can be due to be due to
the high
the high content
content in
in unsaturated
unsaturated fatty
fatty acid
acid ofof the
the oil
oilphase
phase(sesame
(sesame oil),
oil), which
which tends
tends to
tomoderate
moderate thethe
positive effect of the emulsifying and oil phases on spreadability. However, the strongest
positive effect of the emulsifying and oil phases on spreadability. However, the strongest synergism synergism
couldbe
could beobtained
obtainedby bythe
themixture
mixtureofofoil,
oil,aqueous,
aqueous,and andemulsifying
emulsifyingphases.
phases.

3.3.3. Influence
3.3.3. Influence of
of Formulation
Formulation on
onParticle
ParticleSize
Size
The following
The followingequation
equationshows
showsthe
thecubic
cubicmodel
modelobtained
obtainedafter
afterthe
theanalysis
analysisof
ofparticle
particlesize.
size.
Yps = 21.8 X1 + 25.1X2 − 626.1X3 + 164.4X1 × X2 + 1201.7X1 × X3 + 1302.3X2 × X3 +
Yps = 21.8 X1 + 25.1X2 − 626.1X3 + 164.4X1 × X2 + 1201.7X1 × X3 + 1302.3X2 × X3
2048.3X1 × X2 × X3 −287.2X1 × X2(X1 − X2) − 86.2X1 × X3(X1 − X3) − 310.2X2 × X3(X2 − X3)
+ 2048.3X1 × X2 × X3 −287.2X1 × X2 (X1 − X2 ) − 86.2X1 × X3 (X1 − X3 ) − 310.2X2 × X3 (X2 − X3 )
The coefficient of determination (R2) obtained was 96.92% for particle size. The
p-value for lack of fit was 0.23, which suggests that the model fits the experimental data. Concerning
the contribution of different factors to particle size in Figure 6 below, it was observed that the single
Cosmetics 2018, 5, 7 11 of 14

The coefficient of determination (R2 ) obtained was 96.92% for particle size. The p-value for lack of
Cosmetics
fit 2018,which
was 0.23, 5, 7 suggests that the model fits the experimental data. Concerning the contribution 11 ofof
14

different factors to particle size in Figure 6 below, it was observed that the single emulsifying X3 (10.31)
emulsifying X3 (10.31) has a negative effect on particle size and interaction between X1 × X3 (19.73%),
has a negative effect on particle size and interaction between X1 × X3 (19.73%), X2 × X3 (21.44), and
X2 × X3 (21.44), and interaction between the three mixtures X1 × X2 × X3 (33.72) show the contrary.
interaction between the three mixtures X1 × X2 × X3 (33.72) show the contrary.

X2*X3(X2-X3) 5.11
X1*X3(X1-X3) -1.42
X1*X2(X1-X2) -4.73
X1*X2*X3 33.72
X2*X3 21.44
X1*X3 19.79
X1*X2 2.71
X3 -10.31
X2 0.41
X1 0.36

-20 -10 0 10 20 30 40

[Link]
Figure Contributionof
offactors
factorsto
toparticle
particlesize.
size.

This means
This means that
that all
all of
of the
the binary
binary effects
effects and
and interactions
interactions between
between the the three
three mixtures
mixtures have
have aa
synergisticeffect
synergistic effectononthe
theparticle
particlesize.
[Link]
Thiscancan
bebeduedue to the
to the factfact
thatthat
the the oil phase
oil phase (sesame
(sesame oil) and
oil) and the
the emulsifying phase (soy lecithin/Tween) have in their composition
emulsifying phase (soy lecithin/Tween) have in their composition high molecules, which are activehigh molecules, which are
active molecules that have the ability to facilitate the formation of emulsions,
molecules that have the ability to facilitate the formation of emulsions, improve their stability, and improve their stability,
and produce
produce desirable
desirable properties
properties in them
in them [36].[36]. In fact,
In fact, highhigh molecules
molecules adsorb
adsorb totothe
thesurfaces
surfacesof
offreshly
freshly
formed oil droplets created by the homogenization of oil–water–molecules
formed oil droplets created by the homogenization of oil–water–molecules mixtures, where they mixtures, where they
facilitate further droplet disruption by lowering the interfacial tension and retard
facilitate further droplet disruption by lowering the interfacial tension and retard droplet coalescence droplet coalescence
byforming
by formingprotective
protectivemembranes
membranesaround aroundthe thedroplets
droplets[37].[37].

3.3.4. Optimization
3.3.4. Optimizationof
ofBase
BaseCream
CreamFormulation
Formulation
Inorder
In ordertotohave
haveaastable
stableand andoptimal
optimalformulation,
formulation,ititisisnecessary
necessaryto tounderstand
understandthe theproportion
proportion
and nature of each component. In addition, each formulation must be specifically
and nature of each component. In addition, each formulation must be specifically designed according designed according
to the
to the desired
desired purpose of of its
its use
useandandsite
siteofofapplication.
[Link]
Fromthethe
above
aboveobservations,
observations,there must
there not
must
be a high amount of oil phase (sesame oil) in the formulation
not be a high amount of oil phase (sesame oil) in the formulation to to facilitate viscosity; instead, there
instead, there
shouldbe
should beaahigh
highamount
amountof ofemulsifying
emulsifyingphase
phase(soy(soylecithin/tween)
lecithin/tween) to to maintain
maintain the
the emulsion.
emulsion. Thus,
Thus,
aamulti-response
multi-responseanalysis
analysiswas was done
done to to obtain
obtain thethe optimal
optimal combination
combination to betoused
be used to formulate
to formulate the
the final
final product, with X :X :X at a ratio
product, with X1 :X2 :X3 at a ratio of 24:28:10.
1 2 3 of 24:28:10.

3.3.5.
3.3.5. Microstructure
MicrostructureObservation
Observation
Figure
Figure 77shows
showsthethemicrostructures
microstructuresof ofthe
theunhomogenised
unhomogenised emulsion:
emulsion: sesame oil, Aloe
sesame oil, Aloe vera
vera gel,
gel,
and
andsoy lecithin/tween; and sesame oil, Aloe vera gel/gum,
soylecithin/tween; soy lecithin/Tween,
gel/gum, soy lecithin/Tween,and
andbase
basecream.
cream.
WeWeobserved
observedthat
thatwhen
whenthe theaqueous phaseisisAloe
aqueousphase Aloevera
veragel
gelalone,
alone,the
theemulsion
emulsionisisnot
notstabilized
stabilized
due
duetotothe
thefact
factthat
thatthis
thisgel
gel loses
loses its
its properties
propertiesafter
afterextraction.
extraction. A
A further
further reduction
reductionwas
wasobserved
observedwith
with
the
theaddition
additionof ofnatural
naturalgum.
gum.
Cosmetics 2018, 5, 7 12 of 14
Cosmetics 2018, 5, 7 12 of 14

(a) (b)

(c) (d)
Figure 7. Microscopic images of (a) Unhomogenised emulsion; (b) Mixture of sesame oil, Aloe vera
Figure 7. Microscopic images of (a) Unhomogenised emulsion; (b) Mixture of sesame oil, Aloe vera gel,
gel, and soy lecithin/tween; (c) Mixture of sesame oil, Aloe vera gel/gum, and soy lecithin/Tween; and
and(d)
soy lecithin/tween;
base cream. (c) Mixture of sesame oil, Aloe vera gel/gum, and soy lecithin/Tween; and
(d) base cream.
4. Conclusions
4. Conclusions
This work aimed at studying the effect of local raw materials on a formulation of a topical cream
emulsion.
This workAfter screening,
aimed it was found
at studying that sesame
the effect of localoil,raw
Aloe materials
vera gel, and
onsoy lecithin were of
a formulation theabest
topical
ingredients
cream [Link] After
the cream emulsion.
screening, A multi-response
it was optimization
found that sesame wasvera
oil, Aloe done to and
gel, obtain a combined
soy lecithin were
the optimal proportion,
best ingredients forwhich gave emulsion.
the cream us 24% of A sesame oil, 28% ofoptimization
multi-response Aloe vera gel,wasanddone
10% to
of obtain
soy a
lecithin/Tween. However, studies still need to be done to determine the stability of the formulation
combined optimal proportion, which gave us 24% of sesame oil, 28% of Aloe vera gel, and 10% of soy
in the long term and whether or not to use antimicrobial substances for the conservation of the
lecithin/Tween. However, studies still need to be done to determine the stability of the formulation
formulation. This base cream can be used for further work as a matrix for the incorporation of the
in the long term and whether or not to use antimicrobial substances for the conservation of the
active principle in the cosmetic and pharmaceutical industries.
formulation. This base cream can be used for further work as a matrix for the incorporation of the
active principle in theWe
Acknowledgments: cosmetic
thank theand pharmaceutical
laboratories industries.
of University of Ngaoundere will provide the research facilities.

Author Contributions: Gertrude Eleonore DJIOBIE TCHIENOU, Roli Karole TSATSOP TSAGUE, Therese
Acknowledgments: We thank the laboratories of University of Ngaoundere will provide the research facilities.
Florence MBAM PEGA, Vera BAMA, Albert BAMSECK, all make different formulations, and all analyses after
Author Contributions:
the preparation Gertrude
of different EleonoreGertrude
emulsions. DJIOBIEEleonore
TCHIENOU,
DJIOBIERoli Karole TSATSOP
TCHIENOU, TSAGUE,
Roli Karole Therese
TSATSOP
Florence MBAM
TSAGUE, PEGA,
Selestin Vera BAMA,
Dongmo Albert
SOKENG, andBAMSECK, all make
Martin Benoît different formulations,
NGASSOUM and
all interpret the all analyses
results, after the
write and
preparation
correctedof
thedifferent
article. emulsions. Gertrude Eleonore DJIOBIE TCHIENOU, Roli Karole TSATSOP TSAGUE,
Selestin Dongmo SOKENG, and Martin Benoît NGASSOUM all interpret the results, write and corrected the article.
Conflicts of Interest: The authors declare no conflict of interest.
Conflicts of Interest: The authors declare no conflict of interest.

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