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The effect of adding citric acid on making antibacterial film-formed soap for hospital
AIP Conference Proceedings 2255, 040037 (2020); https://doi.org/10.1063/5.0015253
© 2019 Author(s).
Optimization of Solubilizers Combinations on the
Transparent Liquid Soap with the Addition of Peppermint
(Mentha piperita L.) and Lavender (Lavandula L.) Oil
Susinggih Wijana1, a), Tika Puspita1, b) and Nur Lailatul Rahmah1, c)
1
Department of Agro-industrial Technology, Faculty of Agricultural Technology, Universitas Brawijaya
Jl. Veteran, Malang 65145, Indonesia
a)
Corresponding author: susinggihwijana@gmail.com
b)
tikatikb@gmail.com
c)
nur_laila@ub.ac.id
Abstract. Transparent soap usually produced using a synthetic substance. Therefore, the formula optimization of
transparent soap must be conducted with natural substances. The essential oils can be used as alternative natural substances
and a transparent agent such as peppermint and lavender oil. Furthermore, peppermint and lavender oil have an antibacterial
activity which is beneficial for skin health. Therefore, this study aimed to determine the optimum formula mainly the
solubilizer of essential oil to produce transparent soap using natural substances with antibacterial activity, especially S.
aureus growth. The solubilizers used included ethanol, glycerin, and liquid sugar. The studied responses included
transparency, viscosity, pH, and total fatty acids. A Simplex Lattice Design (SLD) method which consisted of 13 formulas
was carried out to determine the optimum soap characteristics namely organoleptic, free alkali, specific gravity, foam
power, and antibacterial activity. The results showed that the optimum solubilizer formula was 20% liquid sugar, 18%
ethanol, and 18% glycerin. The average of transparency, viscosity, pH, and total fatty acids responses were 98,3%, 553,33
cP, 10,04 and 19,85%, respectively. The characteristics of soap were free alkali 0,12±0.015%, specific gravity 1,161 g/ml,
foam power 1,05±0,050 cm, and growth inhibition zone of S. aureus 10,17± 2,753 mm.
INTRODUCTION
Soap products that are increasingly prevalent in the market are liquid consistency soaps because they are more
practical, easy to store, hygienic, and not easily damaged [1]. Liquid soap is produced by the reaction of saponification
between oil and fat with Potassium Hydroxide (KOH) [2]. One of the innovations in soap products based on their
appearance is transparent soap. Transparent soap has an attractive appearance, so the price is relatively higher than
other soaps [3] and even reach two times then translucent soap.
The level of transparency of soap can be obtained from a mixture of several transparent agents such as glycerin,
ethanol, and sugar. According to Mabrouk [4], transparent agents can maintain the transparency of soap by acting as
a solvent that can inhibit the crystallization of soap. Research on transparent soap making has been carried out by
Hambali [5] using transparent agent combinations, namely 13% glycerin, 15% ethanol, and 17% sucrose. Similar
research has also been carried out by Prapanta [6] with the addition of essential oils from Citrus nobilis Lour. var.
Microcarpa. The combination of transparent agents used is 11% glycerin, 15% ethanol, and 17% sugar.
The right proportion of transparent agent combinations can produce good characteristics of transparent soap, so
optimization of the soap formula needs to be done. There are many optimization models can be used, but the famous
one is the response surface method. Sameera and Raju [7] proposed a Simplex Lattice Design optimization with
relatively simple procedures, and analysis can be done with certain models. Therefore, the Simplex Lattice Design
was carried out to optimize the proportion of transparent agents to produce a transparent liquid soap.
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The use of soap as a cleaning product has been developed into antibacterial soap. Antibacterial soap can minimize
skin infections caused by bacteria. According to Orchard and Vuuren [8], the normal flora of the skin is
Staphylococcus aureus (S. aureus) which can cause infections and allergies to the skin, such as impetigo. Impetigo is
a skin infection caused by bacteria and is most often found in children. More than 62% of S. aureus is found in cases
of impetigo through scraping the nasal mucosa [9]. Therefore, the use of antibacterial soap needs to be done to prevent
the onset of the disease.
Many antibacterial soap products on the market use synthetic antibacterial active ingredients such as triclosan and
chloroxylenol [10]. The use of chemical soap continuously can cause antibiotic resistance [11]. Therefore, natural
antibacterial alternatives to soap need to be applied, one of which is by adding antimicrobial essential oils such as
peppermint oil and lavender oil.
The main component of peppermint oil is menthol (29 - 48%) [12]. According to Horváth and Koščová [13],
peppermint oil can inhibit the growth of S. aureus with a minimum concentration of 0.25%. Peppermint oil can cause
a very pungent aroma despite use in minimum concentrations. Therefore, peppermint oil needs to be combined with
other essential oils, such as lavender oil. The main components of lavender oil, linalool (53.5%), can have antibacterial
effects [14] and can be used as aromatherapy substances [15]. According to Djenane [16], lavender oil can inhibit the
growth of S. aureus with a minimum concentration of 0.025%. Therefore, the optimization study of a combination of
transparent liquid soap solvents with the addition of peppermint oil and lavender oil is expected to increase the added
value of soap products and be of interest to many consumers.
EXPERIMENTAL DETAILS
Experimental Design
Component level of solubilizer namely liquid sugar (A), ethanol (B), and glycerin (C) were determined prior to
optimization 56% of liquid soap as depicted in Table 1. A simplex lattice design was used to optimize the solubilizers
of liquid soap as depicted in Table 2, with the mathematical model within equation 1.
TABLE 1. Component Level of Solubilizers
Component Material Upper limit Lower limit Average Deviation
A Liquid sugar 20.00 22.00 20.67 0.7698
B Ethanol 18.00 20.00 18.67 0.7698
C Glycerin 16.00 18.00 16.67 0.7698
Total 56.00
Y = 1( A) 2( B ) 3(C ) 12( A)( B ) 13( A)(C ) 23( B )(C ) 123( A)( B )(C ) 12( A B ) 13( A C ) 23( B C )
(1)
Where 20 ≤ (A) ≤ 22 (%); 18 ≤ (B) ≤ 20 (%); 16 ≤ (C) ≤ 18 (%) and (A) + (B) + (C) = 56%.
Research Parameters
The level of transparency was evaluated using UV-Vis spectrophotometer at a wavelength of 650 nm within 25
°C. Distilled water was used as a blank solution. The best formula is chosen based on the percent transmittance which
is close to 100% with a minimum value of 90% [18]. Another parameter namely viscosity and pH was determined
using viscometer LV and pH meter.
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TABLE 2. Experimental design
Component Response
NO A B C Liquid Ethanol Glycerin Transpar Viscosity pH Fatty
sugar ence Acid
1 1 0 0 22.00 18.00 16.00 β1 β1 β1 β1
2 0 1/3 2/3 20.00 20.00 16.00 β23 β23 β23 β23
3 0 1 0 20.00 20.00 18.00 β2 β2 β2 β2
4 2/3 1/3 0 21.33 18.00 16.00 β12 β12 β12 β12
5 1/3 0 2/3 21.33 18.67 16.67 β13 β13 β13 β13
6 0 0 1 20.67 18.00 16.00 β3 β3 β3 β3
7 2/3 1/3 2/3 20.67 19.33 16.67 β13 β13 β13 β13
8 0 2/3 1/3 20.67 18.67 17.33 β23 β23 β23 β23
9 1/3 1/3 1/3 20.00 19.33 16.67 β123 β123 β123 β123
10 1/3 2/3 0 20.00 18,67 17.33 β12 β12 β12 β12
11 1 0 0 22.00 18.00 16.00 β1 β1 β1 β1
12 0 1 0 20.00 20.00 16.0 β2 β2 β2 β2
13 0 0 1 20.00 18.00 18.00 β3 β3 β3 β3
Fatty acid (F) was determined based on the Indonesian National Standards. 10 g of soap sample (W) was diluted
with 50 ml of distilled water and 25 ml of HCl, then added with methyl orange indicator. The solution then precipitated
in the separating funnel. The solvent is shaken and washed with 10 ml of distilled water each washing until it does not
react acidically (tested with blue litmus paper). The solvent was filtered with N2SO4 anhydrous and put into a fat flask
that had known its weight along with boiling stone (W1). The solvent is distilled and the fat flask is dried at 105 °C
until a fixed weight (W2) was obtained. The total value of fatty acids is calculated based on the formula presented in
equation 2.
W1 W2
F = 100%
W (2)
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influence on the response. The model regression equation for each response namely transparency (Y1), viscosity (Y2),
pH (Y3), and fatty acids (Y4) which is influenced by liquid sugar (X1), ethanol (X2), and glycerin (X3) with a 95%
confidence level can be seen in the following equations:
Y1 = 451 .731 X 1 X 2 (4)
Y2 = 299.487 X 1 + 379.487 X 2 + 561.026 X 3 - 402.692 X 1 X 2 - 451.154 X 1 X 3 - 811.154 X 2 X 3 + 6795 X 1 X 2 X 3 (5)
Y3 = 10.39239 X 1 + 10.3114 X 2 + 10.0406 X 3 0.845192 X 1 X 2 1.22942 X 1 X 3 1.27788 X 2 X 3 - 10.8225 X 1 X 2 X 3 (6)
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A: Liquid sugar (%) A: Liquid sugar (%)
22 22
2 2
300
97.5 98 16 400
18
16 18
500
300
98 98.5 2 2
2 2 20 20 18
20 20 18 B: Ethanol (%) C: Glycerin (%)
B: Ethanol (%) C: Glycerin (%) Viscosity (cP)
Transparency (%)
(a) (b)
A: Liquid sugar (%) A: Liquid sugar (%)
22 22
2 2
21
10.4 10.5
10.5
16 18 16 22 18
10.3
22
23
21
10.4 10.2
10.5 10.1 20
2 2 2 2
20 20 18 20 20 18
B: Ethanol (%) C: Glycerin (%) B: Ethanol (%) C: Glycerin (%)
pH Fatty acid (%)
(c) (d)
FIGURE 1. The contour plot with a special cubic model for each response transparency (a); viscosity (b); pH (c); and fatty acid
(d)
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TABLE 3. Organoleptic test
Component Transparent soap Commercial soap; Dettol
Texture 4.6 4.4
Aroma 4.5 4.8
Color 3.5 4.4
The results obtained were the color, and aroma attributes of Dettol soap were preferred by panelists as a whole
compared to transparent liquid peppermint and lavender oil. The aroma attribute is the lowest attribute of its
assessment in transparent peppermint and lavender oil liquid soap products. This is because the peppermint aroma is
more dominant than lavender. Meanwhile, the texture attributes of peppermint and lavender oil transparent liquid soap
are preferred over Dettol soap. This is because the thickness of Dettol soap is too high. According to Karsheva [25],
the viscosity is the two parameters of concern in liquid soap preparations. Viscosity aims to determine the consistency
of the preparation, which will later affect the application of preparations such as easily poured from the container but
not easily spilt flowing from the hands.
The free alkaline analysis aims to determine the amount of free alkaline present in the soap products produced.
Soap that has been made has free alkaline content of 0.12 ± 0.015%. The free alkali value obtained still meets the SNI
quality standard requirements for liquid bath soap, so transparent liquid peppermint oil and lavender soap are still safe
for use on the skin. According to Widyasanti [26], good soap is a soap that results from a perfect reaction between
fatty acids and alkalis which is expected to have no residue after the reaction. The excess alkali in soap should not
exceed 0.14% because alkali is hard and can cause irritation to the skin.
Specific gravity analysis aims to determine the weight ratio of liquid soap in the air at 25 °C to the weight of water
with the same volume and temperature. Soap that has been made has a specific weight of 1.161 g/mL. The value of
the specific gravity of the soap obtained did not meet the SNI standard for liquid bath soap i.e. 1.01-1.10 g/mL.
Increasing the value of the specific gravity of peppermint and lavender oil transparent liquid soap can be caused by
the high specific gravity of the solvent used, namely liquid sugar and glycerin, although it is dissolved with ethanol,
it is suspected that the substance mixed tends to have a high weight. According to Predianto [27], testing of specific
gravity is important because it can determine whether a solid can be mixed or not with other substances so that it will
be easier in the formulation of soap.
Foam power analysis is carried out by measuring foam height. The soap foam power test produced was done by
comparing the Dettol brand of commercial soap as a control. Transparent peppermint liquid soap and optimal lavender
oil have a foam height of 1.05 ± 0.050 cm. Commercial soap of the Dettol brand has a high foam value of 2.53 ± 0.076
cm. The test results showed that the power of peppermint and lavender oil transparent liquid soap was lower than the
Dettol brand of commercial soap. The low amount of soap foam produced when compared with the high Dettol brand
soap foam is caused by the absence of additional surfactant on the soap preparation. The composition of Dettol soap
is a surfactant, namely Sodium Lauryl Sulfate (SLS), which functions as a foam enhancer. According to Sari and
Ferdinan [28], SLS is a surfactant that is often used in making soap and in large doses can irritate the skin. Therefore,
soap making in this study did not use SLS.
Antibacterial activity characterized by the presence of a clear zone occurs around the paper disk in a petri dish
containing a suspension of the S. aureus bacteria. The test sample was divided into transparent liquid peppermint and
lavender oil (A), commercial Dettol (B) brand soap as a positive control, and transparent liquid soap without
peppermint oil and lavender (C) as negative controls. The test results showed that the samples tested could inhibit the
S. aureus bacteria. The inhibition zone of sample A was obtained at 10.17 ± 2.753 mm. The sample B inhibition zone
was obtained at 8.17 ± 1.755 mm. The inhibition zone of sample C was obtained at 3.00 ± 0.866 mm. The test results
show that transparent peppermint and lavender oil liquid soap has the greatest antibacterial activity compared to
similar commercial soaps that use chloroxylenol as an antibacterial agent.
Transparent peppermint oil and lavender liquid soap can inhibit bacterial growth due to both uses as an
antibacterial. According to Alankar [29] research, the antiplasmid activity of peppermint oil and its main constituent,
menthol, can remove plasmids in bacteria. According to Zengin and Baysal [30], linalool, a component of lavender
oil, is monoterpene alcohol which has a hydroxyl (-OH) group. The hydroxyl group is responsible as an antimicrobial
which results in interactions with intracellular components such as irregular and wrinkled cell structure, as well as
leakage of cell contents and lysis in S. aureus.
The test results also showed that transparent liquid soap without active substances also had antibacterial activity.
This activity is thought to arise from constituent components such as coconut oil. According to Thormar [31],
monolaurin, a monoglyceride compound contained in coconut oil, can damage bacterial cell walls and membranes,
resulting in cell leakage which ultimately leads to cell death.
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SUMMARY
Solvent combinations consisting of 20% liquid sugar, 18% ethanol, and 18% glycerin produced an optimal
transparent liquid soap in the appearance. However, the specific gravity has a slightly higher than Indonesian National
Standards by .061 g/mL. The transparent liquid soap formula with the addition of peppermint and lavender oil has a
greater antibacterial activity compared to the commercial soap that uses chloroxylenol as an antibacterial agent. This
study proved that the natural substance of peppermint and lavender oil have the antibacterial ability with potential
application to health benefit.
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