Development and Stability of Intimate Soap Formula
Development and Stability of Intimate Soap Formula
Original Article
Abstract
The use of synthetic surfactants reflects the high demand in the hygiene and cleaning sector for products with
low-cost and good-effectiveness. These ingredients are the main components of intimate soap formulations.
Sapindus saponaria L. is a plant rich in saponins, with the potential to be used as a natural surfactant due to its
amphiphilic character and its foam-forming properties. Therefore, this study aimed to develop intimate soap
formulations using S. saponaria extract as a natural surfactant and analyze its stability and surfactant characteristics.
Preliminary and accelerated stability parameters, rheological characteristics, surface tension, foaming power,
foam stability and emulsification potential were evaluated. The formulations were stable at a pH suitable for the
intimate region (4.0 to 4.5), the presence of S. saponaria extract provided greater reduction of surface tension,
better foaming and foam stability and greater emulsification power, desirable characteristics for an intimate liquid
soap. These results demonstrate that the incorporation of S. saponaria extract into liquid soap formulations is an
excellent option as a natural surfactant to reduce the use of synthetic anionic surfactants such as SLES.
Keywords: saponins, surfactant, cosmetics, lauryl-free.
Resumo
O uso de tensoativos sintéticos reflete a alta demanda do setor de higiene e limpeza por produtos de baixo
custo e boa eficácia. Estes ingredientes, são os principais componentes das formulações de sabonete íntimo.
A Sapindus saponaria L. é uma planta rica em saponinas, com potencial para ser utilizada como tensoativo natural
devido a seu caráter anfifílico e suas propriedades espumógenas. Diante disso, este trabalho teve por objetivo
o desenvolvimento de formulações de sabonete íntimo utilizando o extrato de S. saponaria como tensoativo
natural e analisar sua estabilidade e características tensoativas. Foram avaliados parâmetros de estabilidade
preliminar e acelerada, características reológicas, tensão superficial, poder e estabilidade de espuma e potencial
de emulsionamento. As formulações se mostraram estáveis em pH adequado para a região íntima (4,0 a 4,5),
a presença do extrato de S. saponaria proporcionou maior redução da tensão superficial, melhor poder e estabilidade
de espuma e maior poder emulsificação, características estas desejáveis para um sabonete líquido íntimo. Esses
resultados demonstram que a incorporação do extrato de S. saponaria em formulações de sabonete líquido é uma
excelente opção como tensoativo natural para reduzir o uso de tensoativos aniônicos sintéticos como o LESNa.
Palavras-chave: saponinas, tensoativo, cosméticos, livre de lauril.
1. Introduction
The personal hygiene, perfumery, and cosmetics to be adjusted between 3.8 and 4.5, in order to contribute
sector has been growing exponentially over the years to the maintenance of vaginal flora and protection against
(Almukainzi et al., 2022; Rocca et al., 2022) and soaps diseases such as candidiasis and bacterial vaginosis
are among the most used items (Alquadeib et al., 2018). (Bezerra et al., 2016). They are presented in solid or liquid
They have the function of removing dirt from the body forms, although the ease of pH adjustment is an advantage
helping to maintain skin health (Rai et al., 2021). of liquid soaps.
Soaps are used in various parts of the human body, Surfactants are the main ingredients of liquid soaps,
however, to be used in the intimate region, the pH needs organic substances of amphipathic character that
*e-mail: [email protected]
Received: July 25, 2023 – Accepted: October 6, 2023
This is an Open Access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use,
distribution, and reproduction in any medium, provided the original work is properly cited.
A Cocamidopropyl betaine 25 25 15
B Propylene glycol 2 2 2
C S. saponaria Extract 0 10 10
The preparation was adapted from the methodology of The number of drops formed in a constant flow of 3 mL
Esprendor et al. (2019) where phases A, B, and C were was correlated with the surface tension through the
heated separately. Phase B was poured over phase A and Equation 1 below:
homogenized, then the volume was completed with
= γ sample H ₂ O drop number × γ H ₂ O / sample drop number (1)
phase C. After cooling, the pH was corrected with phase D.
Where 𝛄= surface tension and H2O = water.
2.5. Quality control and stability of formulations
The organoleptic characteristics and some physico- 2.5.5. Determination of Foaming Power and Foam Stability
chemical parameters of the developed formulations were The foaming power and foam stability were determined
evaluated after 24 h of preparation. The same parameters by the stirring method (Chen et al., 2010; Gomes et al., 2022),
were evaluated in the preliminary stability tests (alternating where 20 mL of solutions at 0.5% and 1.0% (v/v) concentrations
temperature cycles of 45 ± 2 ºC and 5 ± 2 ºC every 24 h for of formulations F1, F2, F3, and S. saponaria extract were
a period of 14 days) and accelerated stability, where new manually stirred for 15 s and, after 30 s of rest, the volume
formulations were prepared and subjected to different (mL) of the formed foam was measured. After 5 min of rest,
storage temperatures (5, 25, and 45 ± 2 ºC) and exposure the foam stability (R5) was determined by the Equation 2:
to light radiation for a period of 90 days. All tests were
= R5 ( foam volume after 5 min / foam volume after 30 s ) × 100 (2)
performed in triplicate.
Where R5 = ratio of foam volume in 5 min to foam volume
2.5.1. Organoleptic characteristics in 30 s
The formulations had their organoleptic characteristics
visually evaluated by verifying homogeneity, color, and odor 2.5.6. Determination of the Emulsification
or changes such as the presence of precipitates, lumps, and The percentage of emulsification was measured using
dispersed particles (Brasil, 2004; Almukainzi et al., 2022). the methodology of Basu et al. (2015) where 2 mL of liquid
paraffin and 2 mL of formulations F1, F2, F3, and of the
2.5.2. Physico-chemical parameters S. saponaria extract were subjected to agitation in a Vortex
The parameters were evaluated according to (Cosmetics mixer (Norte Científica, model NA 3600) for a period of
Europe, 2004; Brasil, 2004): 2 min and then allowed to rest for 24 h. The percentage of
Centrifugation (Quimis®) was performed at 1000 g paraffin emulsification was determined using the Equation 3:
for 30 min to check for signs of instability and need for % emulsification =
(3)
formulation adjustments. emulsified area height / total solution height
The pH (Del Lab®) and conductivity (Tecnopon®)
were evaluated by direct insertion of the electrode into
the formulations. 2.6. Analysis of the results
The relative density was performed by the pycnometer The results of the stability tests were subjected to
method, through the ratio of the sample mass to the analysis of variance (ANOVA) and the significant difference
water mass at a given temperature, and then calculated between the mean values were verified by Tukey’s multiple
the mass density ( ρ ). comparisons test with 95% significance (p<0.05). Results
The refractive index (Polax WYA-2S) was evaluated with were expressed as mean ± standard deviation using the
the equipment previously calibrated with distilled water. Origin Pro software version 8.5.1 (OriginLab©).
The industry’s interest in natural ingredients reflects The mass density result of the formulations (Table 4)
consumer demand for less aggressive and more sustainable was between 1.0369 and 1.0562 g/mL. Although there
products, and the replacement of synthetic raw materials are no established values for density, authors such as
with natural ingredients offers better biocompatibility Hawa et al. (2022) and Pires et al. (2021) found values
and less risk of allergens, as well as socio-environmental between 1.0077 and 1.066 g/mL with plant extracts.
benefits with impact reduction (Rocca et al., 2022). According to Rusdianto et al. (2021), values between
Table 2 shows the results for the organoleptic 1.01 and 1.10 g/mL are acceptable for liquid soaps. This is
characteristics and physico-chemical parameters obtained an important parameter since it interferes with consumer
during the preliminary stability test of formulations experience with the product and the weight and volume
F1, F2, and F3, which remained stable at the end of the of the final packaging (Brasil, 2004).
14-day cycle. The rheology of the formulations showed that the
The preliminary stability parameters (Table 2) showed behavior of the upward and downward flows occurs in a
the adequacy of the formulations, remaining stable non-linear manner and that as the shear rate increases,
throughout the entire period. New samples were prepared a slight decrease in viscosity occurs (Figure 1 and Figure2),
and subjected to accelerated stability (Table 3). demonstrating that the samples behave as pseudoplastic
The formulations stored at a temperature of 25 ºC type non-Newtonian fluids with a tendency to Newtonian,
maintained all their organoleptic characteristics during verified by the minimum hysteresis area.
the 90-day test period. The pH values were stable and Literature reports that pseudoplastic behavior is
within the established range of 4.0 to 4.5. Although there a desirable characteristic in liquid soaps because it is
is no consensus, the literature suggests that the pH of related to the consistency of the formulation (Kumar and
intimate soaps should be in this range, as this prevents an Mali, 2010; Sharma et al., 2011; Alquadeib et al., 2018).
imbalance of the intimate microbiota (Sousa et al., 2019; Also, the incorporation of the extract into the formulations
Gupta et al., 2019). led to a reduction in viscosity from approximately 3.5 Pa∙s
The incorporation of S. saponaria extract as a natural to values less than 0.5 Pa∙s, a behavior that provides less
surfactant favored the acidic pH of the intimate liquid soap resistance to flow and improves characteristics such as
formulations because, due to the extract’s pH of 4.29, the spreadability (Cornwell, 2018).
formulations had a pH of 3.8 to 4.8, being possible to adjust The surface tension has great significance in the
formulations to the desired range if necessary. evaluation of liquid soap formulations since it is related
The electrical conductivity values of the formulations to the detergency process. Figure 3 shows the surface
contributed to the evaluation of stability since the increase tension data of formulations F1, F2, F3, and S. saponaria
or decrease of these values are indicators of coalescence extract, which ranged from 48.22 to 31.72 m/Nm as the
or aggregation of constituents in the formulation concentration of the samples increased.
(Brasil, 2004). All formulations showed good surface tension reduction
The formulations submitted to a temperature of 5 ºC and the addition of the extract in F2 and F3 potentiated this
presented similar results to the formulations at 25 ºC. At effect in all concentrations evaluated. This is an important
a temperature of 45 ºC, all formulations presented one parameter to be analyzed since surfactants, when in
or more changes (color, pH, and electrical conductivity). aqueous solutions, tend to interfere with factors such as
Changes at high temperatures are expected, by the wettability, wetting (Daltin, 2011), cleaning potential and
possibility of evaporation of water from the formulation, particle dispersion (Teixeira Neto et al., 2009).
or by enzymatic oxidation of compounds present in The extract of S. saponaria presented a minimum surface
the extract that are sensitive to temperature (Silva and tension value of 48.22 m/Nm. Formulations and extracts
Cavalcante, 2022). analyzed by Kumar and Mali (2010), Wojton et al. (2021),
When subjected to light radiation, the formulations and Yang et al. (2010), presented corroborating surface
remained stable, that is, they did not present any type tension values and although there are no pre-established
of change, showing that transparent packaging can be values of surface tension, these data indicate that S.
used, which favors the acceptance of the product by the saponaria extract offers the potential to be used for
consumer (Pires et al., 2021; Silva and Cavalcante, 2022). detergent purposes.
Table 2. Organoleptic characteristics and physico-chemical parameters of intimate soap formulations during the preliminary stability test.
Time Formulation Color, Odor and Appearance pH Electric Conductivity (mS/cm) Refractive index
Table 3. Accelerated stability test of intimate soap formulations at different temperatures (5, 25, and 45 ± 2 ºC) and light radiation (UV).
Sample T (ºC) Days Organoleptic Characteristics pH Electric Conductivity (mS/cm) Refractive Index
F1 5±2 0 N 4.23 ± 0.00 15.53 ± 0.00 1.3705 ± 0.00
30 N 4.28 ± 0.13 15.85 ± 0.28 1.3711 ± 0.02
60 N 4.30 ± 0.13 15.64 ± 0.09 1.3704 ± 0.02
90 N 4.30 ± 0.35 15.72 ± 0.47 1.3710 ± 0.03
25 ± 2 0 N 4.23 ± 0.00 15.53 ± 0.00 1.3705 ± 0.00
30 N 4.24 ± 0.35 15.99 ± 0.25 1.3745 ± 0.02
60 N 4.26 ± 0.23 15.81 ± 0.41 1.3744 ± 0.04
90 N 4.26 ± 0.13 16.08 ± 0.12 1.3722 ± 0.02
45 ± 2 0 N 4.23 ± 0.00 15.53 ± 0.00 1.3705 ± 0.00
30 M 4.46 ± 0.48 16.26 ± 0.21 1.3744± 0.046
60 M 4.50 ± 0.15 16.67 ± 0.19 1.3752 ± 0.06
90 M 4.57 ± 0.15 16.49 ± 0.08 1.3728 ± 0.01
UV 0 N 4.23 ± 0.00 15.53 ± 0.00 1.3705 ± 0.00
30 N 4.27 ± 0.27 16.00 ± 0.40 1.3732 ± 0.03
60 N 4.32 ± 0.13 16.52 ± 0.36 1.3732± 0.04
90 N 4.29 ± 0.46 16.49 ± 0.12 1.3771 ± 0.04
F2 5±2 0 N 4.25 ± 0.00 13.62 ± 0.00 1.3812 ± 0.00
30 N 4.27 ± 0.35 13.70 ± 0.40 1.3850 ± 0.03
60 N 4.28 ± 0.13 13.67 ± 0.37 1.3848 ± 0.06
90 N 4.27 ± 0.46 13.70 ± 0.22 1.3824 ± 0.02
25 ± 2 0 N 4.25 ± 0.00 13.62 ± 0.00 1.3812 ± 0.00
30 N 4.24 ± 0.23 13.84 ± 0.15 1.3882 ± 0.05
60 N 4.22 ± 0.23 13.88 ± 0.40 1.3878 ± 0.02
90 N 4.23 ± 0.36 13.89 ± 0.21 1.3849 ± 0.04
45 ± 2 0 N 4.25 ± 0.00 13.62 ± 0.00 1.3812 ± 0.00
30 M 4.26 ± 0.16 13.65 ± 0.25 1.3840 ± 0.03
60 M 4.27 ± 0.13 13.95 ± 0.25 1.3834 ± 0.05
90 M 4.27 ± 0.13 14.02 ± 0.10 1.3848 ± 0.03
UV 0 N 4.25 ± 0.00 13.62 ± 0.00 1.3812 ± 0.00
30 N 4.24 ± 0.35 13.58 ± 0.25 1.3873 ± 0.03
60 N 4.25 ± 0.13 13.87 ± 0.23 1.3879 ± 0.03
90 N 4.24 ± 0.35 13.94 ± 0.21 1.3847 ± 0.01
F3 5±2 0 N 4.28 ± 0.00 12.19 ± 0.00 1.3848 ± 0.06
30 N 4.28 ± 0.13 12.67 ± 0.19 1.3865 ± 0.03
60 N 4.30 ± 0.13 12.43 ± 0.42 1.3864 ± 0.04
90 N 4.29 ± 0.13 12.55 ± 0.21 1.3860 ± 0.02
25 ± 2 0 N 4.28 ± 0.00 12.19 ± 0.00 1.3859 ± 0.00
30 N 4.24 ± 0.13 12.36 ± 0.28 1.3890 ± 0.03
60 N 4.25 ± 0.13 12.16 ± 0.21 1.3909 ± 0.02
90 N 4.30 ± 0.48 12.69 ± 0.23 1.3852 ± 0.05
45 ± 2 0 N 4.28 ± 0.00 12.19 ± 0.00 1.3859 ± 0.00
30 M 4.47 ± 0.31 11.04 ± 0.10 1.3822 ± 0.01
60 M 4.50 ± 0.12 10.69 ± 0.33 1.3846 ± 0.04
90 M 4.58 ± 0.21 10.30 ± 0.20 1.3833 ± 0.02
UV 0 N 4.28 ± 0.00 12.19 ± 0.00 1.3859 ± 0.00
30 N 4.28 ± 0.23 12.21 ± 0.12 1.3882 ± 0.04
60 N 4.29 ± 0.13 12.67 ± 0.20 1.3907 ± 0.06
90 N 4.29 ± 0.48 12.84 ± 0.20 1.3928 ± 0.04
Appearance, color and odor: N – normal, M – modified. Results expressed as mean values and relative standard deviation.
Foam, although not essential and does not contribute to at the same concentration of the formulation solution.
the detergency process, is a relevant factor for the consumer The legislation does not present pre-established values
when choosing a soap, due to the fact it is associated with for this parameter, but the findings are in agreement with
greater cleaning power (Rai et al., 2021). Foam height authors such as Rusdianto et al. (2021) and Meshram et al.
values are in Table 5. (2021), who worked with plant extracts.
The formulation without extract, F1, presented
foam volume values of 96 and 108 mL in 0.5 and 1.0%
solutions. The incorporation of the extract in formulations Table 4. Mass density of intimate soap formulations.
F2 and F3 contributed in enhancing this power. These
values corroborate those found in shampoos (formulation Sample Density (g/mL)
with characteristics similar to liquid soaps) with plant
F1 1.0369 ± 0.01
extracts by Sharma et al. (2011) and Panotin et al. (2022).
The foam potential of the extract in a solution at the F2 1.0478 ± 0.00
same concentrations of the formulations demonstrated
F3 1.0562 ± 0.00
that the foam increase percentage of the formulations is
equivalent to the foam percentage of the extract solution Results expressed as mean values and relative standard deviation.
Figure 2. Shear stress by shear rate curve of formulations F1, F2 and F3.
Table 5. Foaming power and foam stability of F1, F2, F3, and S. saponaria extract in 0.5% and 1.0% solutions, measured after 30 s and
after 5 min.
0.5% after 30 s 0.5% after 5 min R5* (%) 1.0% after 30 s 1.0% after 5 min R5* (%)
F2 304 ± 0.36 280 ±0.34 92.10 332 ± 0.33 299 ± 0.32 90.06
F3 325 ± 0.34 294 ± 0.38 90.46 360 ± 0.31 327 ± 0.34 90.83
Ext 191 ± 1.55 166 ± 1.35 86.91 235 ± 0.82 197 ± 0.99 83.82
*R5 is the ratio of foam volume in 5 min to volume in 30 s. Results expressed as mean values and relative standard deviation.
Table 6. Percentage of paraffin emulsification for formulations F1, that contributes to justify the potential of the extract as
F2, F3, and S. saponaria extract. a surfactant (Wisetkomolmat et al., 2019).
The cleaning potential (Table 6) was calculated by
Sample % Emulsification the percentage of paraffin emulsification, and the values
ranged between 18.47 and 89.90%.
F1 18.47 ± 2.17
F1, which does not have the extract in its composition,
F2 88.75 ± 1.99 presented a value of 18.47%, and the addition of S. saponaria
extract to F2 and F3, enhanced the emulsification, with
F3 89.90 ± 1.58 results close to 90%. S. saponaria extract in a 10% solution
Ext 10% 62.90 ± 3.62 showed 62.20% of emulsification, demonstrating excellent
potential for incorporation into cleaning formulations.
Results expressed as mean values and relative standard deviation. Natural surfactants need to have an emulsifying activity of
50 to 90% (Bezerra et al., 2018), a fact that is directly related
to the surfactant potential of the product (Daltin, 2011).
The values found corroborate the results of authors such as
Saripalla et al. (2022) and Basu et al. (2015) in formulations
and in plant extracts.
Emulsification is an important attribute because it is
related to detergency through the removal of dirt from
the body, such as oiliness (Daltin, 2011) and also brings
the possibility of S. saponaria extract being used as an
emulsifier in cosmetic formulations.
4. Conclusions
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