Design and Development of Peel-off Mask Gel Formulation of

Citronella Oil for Acne Vulgaris

Dyah Rahmasari

, Dian Ermawati, Raditya Weka Nugraheni, Dwi Ramadhaningtyas Putri, and Indah

Nur Pratiwi

Department of Pharmacy, Faculty of Health Science, University of Muhammadiyah Malang, Jalan Bendungan Sutami

188A, Malang 65145, East Java, Indonesia

Keyword: Citronella Oil, Peel-Off Mask Gel, Stabilit, Antibacterial Activity

Abstract: Cymbopogon nardus is a traditional plant that has chemical content of citronella oil with potential antibacterial

activity. Antibacterial peel-off mask is very easy to applicate on face. This research aim is to develop and

characterize the antibacterial peel-off mask gel containing citronella oil. This study used an experimental

method. The peel-off mask was formulated using 8%, 10%, and 12% of polyvinyl alcohol (PVA) as a gelling

agent. Evaluation of peel-off mask including physical characteristics (organoleptic, homogeneity, viscosity,

spreadability, film drying time), chemical characteristic (pH value), stability and antibacterial activity. The

organoleptic properties showed that the citronella oil peel-off gel mask was white, aromatic and had a soft

texture. The variation in PVA affects the pH value, viscosity and film drying time of the peel-off mask,

significantly. Stability test showed that all peel-off mask was no significant changes physically in the freeze-

thaw method, but there was some color change and phase separation in the real-time method. The peel-off

mask containing citronella oil using 8% PVA has the highest inhibition against Propionibacterium acnes

almost the same with the positive control (clindamycin gel). Variation concentration of PVA in the formula

was affected on the physical and chemical characteristics and antibacterial activity of the citronella oil peel-

off mask gel, significantly. The preparation using 8% PVA gives the best formula with optimal results.

1 INTRODUCTION

Acne vulgaris is one of the most common skin

diseases worldwide where it diagnosed in 80% of all

teenagers (Griffiths, C., Barker, J., Bleiker, T.,

Chalmers, R., Creamer, 2016). About 83% to 85% of

adolescent girls and 95% to 100% of adolescent boys

are afflicted (Shalita, Del Rosso and Webster, 2011).

Several major factors influence acne pathogenesis,

including Propionibacterium acnes, which secretes

various biologically active molecules and plays a role

in the initiation of the local inflammatory response

(Zouboulis, Katsambas and Kligman, 2013).

Most people with acne will first try to self-treat

and some of them using antibacterial masks as

treatment (Draelos, 2016) and choosing use natural

products. One of the natural herbs is citronella

(Cymbopogon nardus). Citronella oils contain

citronellal, citronellol, and geraniol as several major

components. It has shown antibacterial and antifungal

activities in vitro, as active as penicillin against

certain Gram-positive bacteria (Ehab, no date). Due

to these data, the citronella oil (C. nardus) has

potential as an anti-acne agent for facial skin

treatment.

Peel-off mask is applied as a liquid film that thinly

spread with fingers on the face and peels-off as a thin

plasticized film (Suhery and Anggraini, 2016) after

complete drying without leaving any residues (Rosa

et al., 2013). It can be repairing refreshing and

tightening facial skin (Husni and Dewi, 2019),

provides deep pore cleansing and skin debris removal

(Suhery and Anggraini, 2016). Peel-off can also

provide slight moisturizing action and enhances the

occlusive effect (Rosa et al., 2013), improving blood

circulation, stimulating the activity of skin cells,

removing dead skin cells, softening the skin and

providing nutrients on the skin (Husni and Dewi,

2019)(Kulkarni, Gupta and Bhawsar, 2019). Mostly,

the peel-off mask is based on polyvinyl alcohol

(PVA) or polyvinyl acetate (PVAc), which causes

tensor and occlusion effects (Nilforoushzadeh et al.,

2018).

Rahmasari, D., Ermawati, D., Nugraheni, R., Putri, D. and Pratiwi, I.

Design and Development of Peel-off Mask Gel Formulation of Citronella Oil for Acne Vulgaris.

DOI: 10.5220/0009126101570163

In Proceedings of the 2nd Health Science International Conference (HSIC 2019), pages 157-163

ISBN: 978-989-758-462-6

157

The objective of this study was to develop and

formulate citronella oil peel-off mask by using

various concentration of PVA and evaluate by several

test methods, which possesses antibacterial activity as

an alternative of facial skin care product.

2 METHODS

Instruments

pH meter, Brookfield viscometer, autoclave, petri

dish, incubator, climatic chamber, refrigerator.

Ingredients

Citronella (Cymbopogon nardus L.) oil, Polyvinyl

Alcohol (PVA), Polyethylene glycol 400, Propylene

glycol, Butylated Hydroxyl Toluene (BHT), Methyl

Paraben, Ethyl Paraben, Disodium EDTA, Glycerin,

Sweet orange oil, polysorbate 80 (Tween 80), and

aquadest. Propionibacterium acne was used for

antibacterial activity test and clindamycin gel was

used as the positive control.

Peel-off mask gel preparation of citronella oil

The formulation of a peel-off mask gel of citronella

oil was made according to the formula presented in

Table 1. PVA was dispersed in 80% of the distilled

water (85 - 90) in a water bath (mixture 1). PEG

400 was dissolved in the water (mixture 2). Methyl

paraben and disodium EDTA was dispersed into the

propylene glycol and glycerin then stirred until

homogenous and added with Tween 80 and the

remaining amount of water (20%) (mixture 3). Propyl

paraben and BHT were dispersed into the citronella

oil (mixture 4). Then added mixture 3 into mixture 2

homogenously and added again into mixture 1.

Lastly, added some fragrance into mixture 1 and

poured with mixture 4 homogenously until peel-off

masks are formed.

Physicochemical evaluation of citronella oil peel-

off mask gel

The physicochemical evaluation involved was

organoleptic, homogeneity test, determination of pH

value, viscosity, gel spreadability, and film drying

time. Organoleptic was observed as its odor, color,

and consistency visually. The homogeneity test was

observed by applying the gel on transparent glass. pH

value was measured by using pH meter and viscosity

was determined by using Viscometer. Gel

spreadability was measured by applying gel on

transparent glass plates then loading by some loads.

Film drying time was observed by applying the

amount of gel on hands and wait until it formed a dry

and elastic layer.

Stability evaluation

The stability evaluation was held using two methods,

real-time and accelerated stability method. The real-

time stability method evaluation was observed by

storing the peel-off mask gel under the following

storage conditions: 30±2°C (room temperature) and

40±2°C (climatic chamber). Each sample was

analyzed for one month (28 days) according to the

following parameters: organoleptic characteristic and

pH value. The accelerated stability method evaluation

was performed to see the stability of formulations at

low (4ºC ± 2ºC) and high temperature (40ºC ± 2ºC)

for 24 hours respectively. It was counted as one cycle

and was analyzed for 6 cycles according to the several

parameters: organoleptic characteristic, phase

separation and pH value.

Table 1: Formulation of Citronella oil peel-off mask gel.

Ingredients

F1 F2 F3

Citronella Oil 0.5 % 0.5 % 0.5 %

PVA 8 % 10 % 12 %

PEG 400

2 % 2 % 2 %

BHT

0.7 % 0.7 % 0.7 %

Propylene glycol 2 % 2 % 2 %

Glycerin

2 % 2 % 2 %

Methyl paraben

0.1 % 0.1 % 0.1 %

Ethyl paraben 0.3 % 0.3 % 0.3 %

Tween 80 1 % 1 % 1 %

Disodium EDTA

0.02 % 0.02 % 0.02 %

Sweet orange oil 0.1 % 0.1 % 0.1 %

Aquadest until 100% until 100% until 100%

HSIC 2019 - The Health Science International Conference

158

Antibacterial activity test on citronella oil peel-off

mask gel

The disc diffusion method was used to determine the

zone of inhibition against Propionibacterium acnes.

Antibacterial activity of citronella oil peel-off mask

gel was tested by a modified well in agar method

(Ilavenil, S, B. Kaleeswaran, B. and Ravikumar,

2010). Paper discs (6mm in diameter) were placed on

MHA (Mueller Hinton Agar) media surface that been

inoculated with bacterial suspension (Budiman et al.,

2017). Bacteria that were suspended with 0.9% NaCl

equalized using nephelometer (BD Pheonix) with a

standard of 0.5 Mc Farland (estimated 1.5 x 10

bacterial cells / mL) (Azrifitria; Aziz, 2010). Then

poured the citronella oil peel-off mask gel into each

well about 50μm using micropipette. Each gel was

assayed in triplicate. The antibiotic (Clindamycin gel)

was used as a positive control, while the negative

control contained peel-off mask gel without citronella

oil. Petri dishes were incubated at 37 for 24 hours

(Ilavenil, S, B. Kaleeswaran, B. and Ravikumar,

2010).

3 RESULTS AND DISCUSSION

Physicochemical evaluation of citronella oil peel-

off mask gel

Organoleptic test was carried out to see the physical

appearance of the preparation by observing the color,

smell, consistency, and homogeneity of the

preparation. The all peel-off masks gel are white. It

had a distinctive smell of citronella oil and a hint of

orange scent. These gels had a semi-solid

consistency, soft and smooth, easy to apply, light to

spread, thin and get thicker with the addition of PVA.

Homogeneity of the preparation was shown by the

absence of coarse particles (Ditjen POM, 1985), has

a flat color and showed no phase separation (between

citronella oil and peel-off mask gel base) in the

preparation after its application to a transparent glass.

The pH value should be in the broad range of skin

pH (from 4.0 to 7.0) to avoid any irritation to the skin

(Ali and Yosipovitch, 2013) and should be lower than

5.0 for better skin condition (Lambers et al., 2006).

The result of pH value measurement was done in

triplicate and average values calculated (Table 2).

PVA is a water-soluble synthetic polymer that has a

pH value of 5.0 – 8.0 (Rowe, Sheskey and Cook,

2009). The variation of PVA concentration in the

citronella oil peel-off mask gel will affect the pH

value of resulting preparation. The greater

concentration of PVA, the higher the pH value of the

preparation obtained. The pH of peel-off mask gel

preparations was within the normal pH range of the

skin.

A viscosity test was carried out to determine the

thickness of a preparation and was measured using

Brookfield viscometer. As shown in Table 2, the

greater the concentration of PVA as a film-forming or

gelling agent, the higher viscosity of the preparation

was obtained. Viscosity in the peel-off mask gel is

influenced by an increase in gelling agent

concentration (Yuliani, 2010). PVA has substantial

flexibility, tensile strength and hardness (Gaaz et al.,

2015). This will cause a greater binding and retention

of the fluid by the gelling agent, therefore, the

viscosity of the preparation increases.

A gel spreadability test was performed to examine

the ability of citronella oil peel-off mask gel to spread

when applied on the skin. The rate of spreading

depends on the rate and time of shear produced upon

smearing and also depends on the viscosity of the

formulation (Garg et al., 2002). In the topical

preparation, spread is inversely proportional to its

viscosity. Based on the results of testing the

spreadability of peel-off mask gel, it was concluded

that the increasing of PVA concentration affected the

gel spreadability. The lower the viscosity, the higher

the dispersal power (Chandira, R. M. Pradeep;

Pasupathi, A.; Bhowmik, D. Chiranjib, Jayakar and

K., K. Tripathi; Kumar, 2010). A good peel-off mask

gel has a dispersion of 5 – 7cm (Rahmawanty, Dina;

Yulianti, Nita; Fitriana, 2015) (Table 2).

Film Drying Time was carried out to find out how

long the peel-off mask gel preparation will dry on the

surface of the skin and form a layer of film. Ideally,

the peel-off mask gel should dry between 15 – 30 min

(Vieira et al., 2009). As shown in Table 2, the drying

test of the film showed that F3 dried faster than F1

and F2, this might be caused by the high

concentration of PVA in the formula.

Table 2: Results of the physicochemical evaluation.

Parameter F1 F2 F3

pH 4,80 ± 0,23 5,28 ± 0,58 6,11 ± 0,32

Viscosity (cps) 500 ± 0 1467 ± 115,47 3800 ± 1609,35

Spreadability (cm) 7,18 ± 0,32 6,67 ± 0,51 6,22 ± 1,15

Film Drying Time (min) 23,38 ± 0,08 21,18 ± 0,25 16,66 ± 0,30

Design and Development of Peel-off Mask Gel Formulation of Citronella Oil for Acne Vulgaris

159

Stability evaluation

Freeze-thaw stability evaluation was evaluated in 6

cycles (12 days) to verify signs of instability in the

formulations under extreme conditions. The results

are shown in Table 3 and Figure 1. It was verified that

the optimized formulations stored at extreme

temperature (4ºC ± 2ºC to 40ºC ± 2ºC for 6 cycles)

did not show signs of instability, both in organoleptic

parameters or in pH value.

Nevertheless, the storage at real-time method (28

days) with exposure in room temperature (30ºC ±

2ºC) and in climatic chamber (40ºC ± 2ºC) led to a

sign of instability in phase separation. The citronella

oil peel-off mask gel showed a visual phase

separation in 3

weeks on storage in room

temperature and in 2

weeks on storage in the

climatic chamber (Table 4). The sedimentation

phenomenon on phase separation led to a distribution

gradient where larger particles were concentrated at

the bottom of the glass bottle (Beringhs et al., 2013).

Table 3: Result of the freeze-thaw stability evaluation.

Parameter

F1 F2 F3

Time (Cycle)

1 2 3 4 5 6 1 2 3 4 5 6 1 2 3 4 5 6

Color

N N N N N N N N N N N N N N N N N N

Odor

N N N N N N N N N N N N N N N N N N

Consistency

N N N N N N N N N N N N N N N N N N

Phase

Separation

NS NS NS NS NS NS NS NS NS NS NS NS NS NS NS NS NS NS

N Normal, NS No Separation

Figure 1: Variation of pH value on freeze-thaw stability method evaluation

4.80

5.28

6.11

5.12

4.78

5.16

4.30

4.40

4.50

4.60

4.70

4.80

4.90

5.00

5.10

5.20

5.30

5.40

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

I II III

pH Value

Formula

Before

After

HSIC 2019 - The Health Science International Conference

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Table 4: Result of the real-time stability evaluation

Parameter

F1 F2 F3

Time (Week) Time (Week) Time (Week)

1 2 3 4 1 2 3 4 1 2 3 4

30±2°C 30±2°C 30±2°C

Color N N N N N N N N N N N N

Odor N N N N N N N N N N N N

Consistency N N N N N N N N N N N N

Phase

Separation

NS NS S S NS NS S S NS NS S S

40±2°C 40±2°C 40±2°C

Color N N N N N N N N N N N N

Odor N N N N N N N N N N N N

Consistency N N N N N N N N N N N N

Phase

Separation

NS S S S NS S S S NS S S S

N Normal, NS No Separation, S Separation

Figure 2: Variation of pH value on real time (30±2°C) stability method evaluation

Figure 3: Variation of pH value on real time (40±2°C) stability method evaluation.

4.80

5.28

6.11

5.12

4.72

5.13

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

4.20

4.40

4.60

4.80

5.00

5.20

5.40

I II III

pH Value

Formula

Before

After

4.80

5.28

6.11

4.82

4.98

4.91

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

4.60

4.65

4.70

4.75

4.80

4.85

4.90

4.95

5.00

5.05

I II III

pH Value

Formula

Before

After

Design and Development of Peel-off Mask Gel Formulation of Citronella Oil for Acne Vulgaris

161

Figure 4: Results of antibacterial activity test Citronella oil peel-off mask gel

Antibacterial activity test of citronella oil peel-off

mask gel

The result of the antibacterial activity test of

citronella oil peel-off mask gel can be seen in Figure

4. The results of the antibacterial activity test showed

that the citronella oil peel-off mask gel can inhibit the

growth of bacteria Propionibacterium acnes. Most of

the antibacterial activity from natural plants identified

as phenolic and terpenoids. The compounds include

citronellal, citronellol, and geraniol, which grouped

as terpenoids (Bota, Welmince; Martosupono,

Martanto ;Rondonuwu, 2015).

Terpenoids were considered as fast-acting

compounds, since they inactivated organism in a

short period, with mechanism of action should be

related by the dysfunction or rupture of the cell

membrane of bacteria (Guimarães et al., 2019). The

inhibition zone in the peel-off mask gel is influenced

by an increase in gelling agent concentration. The test

results demonstrate that the greater concentration of

PVA as a gelling agent, the lower was the inhibition

zone of the preparation. This can occur because of the

greater trapping active compound by the gelling

agent, therefore, the antibacterial activity of the

preparation decreases.

4 CONCLUSIONS

The citronella oil peel-off mask gel with PVA has the

best physical properties in Formulation 1 caused the

formulation showed the greatest pH value, viscosity,

spreadability and film drying time on human skin.

Nevertheless, it was showed instability in 30±2°C and

40±2°C storage. The Formulation 1 of citronella oil

peel-off mask gel has antibacterial activity against

Propionibacterium acnes (MIC 10,00mm ± 0,7550)

almost the same with the positive control (MIC 10,33

± 0,9074). The result demonstrated that variation

concentration on PVA was affected on

physicochemical characteristics and antibacterial

activity of citronella oil peel-off mask gel,

significantly.

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