Formulation of Herbal Toothpaste Combination of Anna
Apple Peel and Kaffir Lime
Peel with Variation of
Sodium Lauryl Sulfate Concentration
Andi Nila
Sastrawatia,1*, Jumaina,2, Arisantya,3
a Poltekkes
Kemenkes Makassar, South Sulawesi, Indonesia
1[email protected], 2[email protected],
3[email protected]��
ABSTRACT
Toothpaste is a
preparation whose use aims to clean the mucous membranes of the mouth. Anna's
apple is a fruit that contains malic acid which has the
ability to whiten teeth. Kaffir lime contains essential oils that have
effects as antibacterial, antifungal and refreshing.
This study aims to formulate herbal toothpaste preparations a combination of
Anna Apple Skin extract (Malus domestica) and Purut Orange Peel extract (Citrus
hystrix) and determine the physical quality of the preparation made. This type
of research is experimental research using maceration methods with physical
quality stability testing, namely organoleptic observations, homogeneity, pH,
foam height, viscosity, and dispersion. In this study, two herbal toothpaste
formulations were made with variations in the concentration of Sodium Lauryl
Sulfate as a foaming agent in toothpaste. From the results of the study, it was
obtained that the combination of the two extracts can be formulated into herbal
toothpaste preparations and based on the results of physical quality tests,
both formulations with variations in the concentration of Sodium Lauryl Sulfate
1.5% and 2.5% meet the requirements of the established standards.
Keywords:
anna apple peel, kaffir lime peel, sodium lauryl
sulfate, toothpaste.
Correspondent: Andi Nila Sastrawatia
Email: [email protected] ���
INTRODUCTION
Oral
and dental health is highly maintained because it can affect a person's
standard of living, especially regarding self-confidence (Fellows
et al., 2022). Besides that, the mouth is a place for food and drink to enter as well
as a place for various kinds of diseases. The percentage of oral health
problems in Indonesia is 14% in abscesses and swollen gums cases. Meanwhile, the most effective rate, namely 45.3%, had
cavities or damaged teeth (Riskesdas, 2018).
Tooth discolouration is also a problem that can affect a person's
self-confidence (Zou et al., 2020). Today, one's appearance is essential, especially in
maintaining dental esthetics. Everyone wants to do various ways to increase
self-confidence through body care. With the increasing development of
dentistry, the need for dental aesthetics is also growing (Anggraeni & Aryanto, 2019).
Oral and dental health needs to be maintained by carrying out
maintenance, namely brushing teeth using toothpaste (Carter et al., 2022). The side effects caused by the use of carbamide
peroxide and hydrogen peroxide make researchers continue to try to find alternatives
using natural ingredients that can restore white teeth with few side effects
and affordable prices (Anggraeni & Aryanto, 2019).
Various kinds of plants can be found in Indonesia because the area is
tropical, so it has natural ingredients for various health problems. Apart from
being preferred because of their high nutritional value, apples are also used
as a teeth-whitening agent because of their acidity. As much as 90% malic acid
is the main content of apples. Anna apple is a type of apple with a slightly
yellowish-red colour, thin skin, and more water content than other types of
apples. According to research (Sa'adah & Estiasih, 2015), Anna apples have more acid content than other types
of apples. Organic acids can whiten teeth.
Another natural ingredient that can be used to keep your teeth and mouth
clean is kaffir lime. Generally, kaffir lime adds flavor to dishes where the taste
comes from essential oils. Essential oils function as antimicrobials (Yunilawati et al., 2021). Based on research conducted (Etika, 2019) that
the ability of essential oils in kaffir lime peels is antimicrobial,
antifungal, and tonic. Streptococcus mutants are a bacterium whose growth can
be inhibited by the content of citronellal compounds in essential oils. These
bacteria can form plaque, the leading cause of dental caries (Yuliani et al., 2011).
According to research (Anggraeni & Aryanto, 2019), Anna apples can be a natural teeth-whitening agent.
According to Annisa's research in 2019, kaffir lime peel extract effectively
reduces plaque buildup at a concentration of 5%. This
is due to the antibacterial and antiseptic properties of kaffir lime peels.
Based
on this description, researchers developed a Formulation of Herbal Toothpaste
Preparation Combination of Anna Apple Skin Extract (Malus domestica) and
Purut Orange Peel (Citrus hystrix) with Variations in Lauryl Sulfate
Sodium Concentration of 1.5% and 2.5%. Sodium lauryl sulfate in the formula
acts as a surfactant with the ability to reduce surface tension and reduce food
waste on the teeth. This study aims to formulate an Herbal Toothpaste
Preparation Combination of Anna Apple Skin Extract (Malus domestica) and
Purut Lime Fruit Peel (Citrus hystrix) with Variations in Sodium Lauryl
Sulfate Concentration with physical quality stability testing, namely
organoleptis observation, homogeneity, pH, foam height, viscosity
and dispersion.
The
purpose of the study was to formulate herbal toothpaste preparations from a
combination of Anna Apple Skin Extract (Malus domestica) and Purut
Orange Peel (Citrus hystrix) and to determine the physical quality of
the toothpaste preparations made.
The
benefit of research is to add insight into science in the pharmaceutical field,
especially in the manufacture of toothpaste preparations with the use of
natural ingredients and this research as reference material for further
research.
METHODS
This research is experimental with the aim of formulating
Herbal Toothpaste Preparations Combination of Anna Apple Skin Extract (Malus
domestica) and Purut Orange Peel (Citrus hystrix) with Variations in
Sodium Lauryl Sulfate Concentration with physical quality stability testing,
namely organoleptis observation, homogeneity, pH, foam height, viscosity and
dispersion. The population in the study is all types
of plants that can be formulated in the dosage form of toothpaste. The
equipment used is a maceration tool, knife, stirring rod, sieve, petri dish,
gauze, glass funnel, glass beaker, erlenmeyer, mortar and stamfer, horn spoon,
measuring cup, analytical balance, sudip, orek, drip pipette, pH meter, Rotary
Evaporator, Waterbath, Incubator, refrigerator, and viscometer. The
ingredients used are Anna Apple peel, Kaffir Orange peel, Tocopherol, Glycerol,
Calcium Carbonate, Methyl Paraben, Sodium Lauryl Sulfate, Sorbitol, Ethanol,
Oleum Menthae Piperitae, dyes and Aqua Destillata. The
following is the design formula for this study:
Table 1. Herbal Toothpaste
Formula Design Combination of Anna Apple Peel (Malus Domestica) and
Kaffir lime (Citrus Hystrix) Peel
|
Material |
Composition
% |
Reference |
|
|
Toothpaste
Formulas |
|||
|
Formula
1 |
Formula
2 |
||
|
Anna Apple fruit skin extract |
5 |
5 |
(Annisa, 2019) |
|
Kaffir lime peel extract |
5 |
5 |
(Annisa, 2019) |
|
Calcium carbonate |
30 |
30 |
(Arisanty, 2016) |
|
Glycerin |
5 |
5 |
≤ 30 (HPE Fifth Edition, 2006) |
|
Sorbitol |
20 |
20 |
20-60 (HPE Fifth Edition, 2006) |
|
Sodium Lauryl Sulfate |
1.5 |
2,5 |
0.5-2.5 (HPE Fifth Edition, 2006) |
|
Methyl Paraben |
0.1 |
0.1 |
0.015-0.2 (HPE Fifth Edition, 2006) |
|
Tocopherol |
0.05 |
0.05 |
(Nur Sa'adah, 2016) |
|
Oleum Mentha Pip. |
0.5 |
0.5 |
(Zulfa, 2012) |
|
Dye |
qs |
qs |
|
|
Aqua Destillata |
Ad 100 |
Ad 100 |
|
The process of making toothpaste is made
of two formulas. The first step is to crush Calcium Carbonate, sieved, and then
weigh it. Then the extracts of Anna apple peel and Kaffir lime peel, Sodium
Lauryl Sulfate, Glycerin, Sorbitol, Methyl Paraben, Tocopherol, and Oleum
Menthae Pip were weighed. Moreover, measured Aqua Destillata. Next, heat
Aquadest in a glass beaker on a hot plate. After it was hot, Methyl Paraben was
added and stirred until it dissolved (mass 1). Add Sodium Lauryl Sulfate into
the mortar and grind until smooth, then add Calcium Carbonate while grinding
until uniform (mass 2). Next,
the extract of Anna apple peel and kaffir lime peel was dissolved with some
glycerin (mass 3). Put the rest of the glycerin into the mortar, grind it, and
add part of the mass 2 bit by bit while grinding it until it is homogeneous and
forms an emulsion. Then add the remaining mass two while grinding until
homogeneous (mass 4). Sorbitol is added and then crushed until homogeneous.
Then add tocopherol little by little and grind until homogeneous. Entered Oleum
Menthae Pip. and crushed to form a paste. Added coloring and then crushed
again. Then the paste is put into the container for further testing of the
physical quality of the preparation.
Accelerated
stability testing (Cycling Test) using the Freeze-Thaw method aims to determine the
physical stability of the preparation.
This test is based on
the effect of changing the temperature of the cycling test at a temperature of 4oC, followed by a
temperature of 40oC which is carried out in 6 cycles. One cycle lasts 24 hours (Suryani & Hernaman,
2017).
Evaluation of
toothpaste preparations, namely:
Organoleptic
Test
An organoleptic test
is a test that looks at visual preparation. The preparations were observed for
their shape, color, and aroma (Azkiya et al., 2017). According to SNI No. 12-3524-1995, the
conditions for a good toothpaste preparation are soft and homogeneous, with no
air bubbles, lumps, and separate parts.
Homogeneity Test
The
preparation is taken and smeared on a petri
dish, then observed. Good preparation standards based on SNI No. 12-3524-1995
that is homogeneous, with no air bubbles, lumps, and separate parts.
pH
test
The tool in the form of a pH meter electrode is dipped in formulas one
and two until an equivalent value appears on the pH screen (Lestari et al., 2020). Toothpaste is safe if it is within the range of 4.5 �
10.5, according to SNI 12-3524-1995.
Foam
Height Test
Most toothpaste
requires much foam to lift the remaining dirt on the teeth. This test method
takes 1 gram of the preparation, puts it in a 50 ml measuring cup, and then
dissolves it with 10 ml of Aqua Distillate. Shake five times and pay attention
to the height of the foam (Daud et al., 2016). The
maximum foam height requirement for toothpaste preparations is 15 mm (Achsia, 2020).
Viscosity
Test
Viscosity measurement
using a Brookfield viscometer on the spindle and the appropriate speed.
Tests were carried out before and after the
cycling test (Pratasik et al., 2019). Based on SNI 16-4399-1996, the viscosity
standard for semisolid toothpaste preparations ranges from 2000 � 50000 cP.
Spreadability
Test
Weigh 0.5 g of
the preparation and store it on a 20x20 cm glass, then overlap it again using a
glass and place a weight of 125 g on it. Then the diameter of the spreading
power was measured after 1 minute (Nurjannah et al., 2018). Toothpaste
requirements are in the range of 3 � 5 cm spreadability (Wahidin et al., 2021).
RESULTS AND DISCUSSION
Organoleptic Test
Table 2. Organoleptic
test results for herbal toothpaste
preparations combined with Anna Apple Peel (Malus domestica) and Kaffir
lime (Citrus hystrix) Peel before and after storage using
accelerated stability method with three replications
|
Formulas |
Organoleptic |
|||||
|
Before Accelerated Storage |
After Expedited Storage |
|||||
|
Form |
Color |
Smell |
Form |
Color |
Smell |
|
|
F1 |
Semisolid |
Green |
Mint |
Semisolid |
Green |
Mint |
|
F2 |
Semisolid |
Green |
Mint |
Semisolid |
Green |
Mint |
Homogeneity Test
Table 3. Results of
homogeneity testing of herbal
toothpaste preparations combined with extracts of Anna apple peel (Malus
domestica) and kaffir lime peel
(Citrus hystrix) before and after storage using the accelerated
stability method with three replications
|
Formulas |
Before Accelerated Storage |
After Expedited Storage |
Condition |
Results |
|
F1 |
Homogeneous |
Homogeneous |
There are no coarse details |
Qualify |
|
F2 |
Homogeneous |
Homogeneous |
Qualify |
pH test
Table
4. Test results for the pH of herbal toothpaste preparations combined with Anna Apple Peel (Malus
domestica) and Kaffir lime Peel (Citrus hystrix) extract
before and after storage using the accelerated stability method with three
replications
|
Formulas |
Before Accelerated Storage |
After Expedited Storage |
Condition |
Results |
||
|
F1 |
I |
8,22 |
I |
7,79 |
4.5 - 10.5 |
Qualify |
|
II |
8,18 |
II |
7,67 |
|||
|
III |
8,14 |
III |
7.59 |
|||
|
Average |
8,18 |
7,68 |
||||
|
F2 |
I |
8.40 |
I |
7,84 |
Qualify |
|
|
II |
8.35 |
II |
7,82 |
|||
|
III |
8,31 |
III |
7,78 |
|||
|
Average |
8.35 |
7,81 |
||||
Foam Height Test
Table 5. The results
of high foam testing of herbal
toothpaste preparations combined with extracts of Anna apple peel (Malus
domestica) and kaffir lime peel (Citrus hystrix) before and
after storage using the accelerated stability method with three replications
|
Formulas |
Before Accelerated Storage |
After Expedited Storage |
Condition |
Results |
||
|
F1 |
I |
8mm |
I |
6mm |
15mm |
Qualify |
|
II |
8mm |
II |
7mm |
|||
|
III |
7mm |
III |
7mm |
|||
|
Average |
7.6mm |
6.6mm |
||||
|
F2 |
I |
13mm |
I |
12mm |
Qualify |
|
|
II |
11mm |
II |
9mm |
|||
|
III |
12mm |
III |
10mm |
|||
|
Average |
12mm |
10.3mm |
||||
Viscosity Test
Table 6. The results
of viscosity testing of herbal
toothpaste preparations combined with extracts of Anna apple peel (Malus
domestica) and kaffir lime peel (Citrus hystrix) before and
after storage using the accelerated stability method with three replications
|
Formulas |
Before Accelerated Storage |
After Expedited Storage |
Condition |
Results |
||
|
F1 |
I |
10100 |
I |
9963 |
2000-50000 |
Qualify |
|
II |
11297 |
II |
10708 |
|||
|
III |
12053 |
III |
11838 |
|||
|
Average |
11150 |
10836 |
||||
|
F2 |
I |
11752 |
I |
10730 |
Qualify |
|
|
|
II |
12107 |
II |
11133 |
||
|
III |
12141 |
III |
11931 |
|||
|
Average |
12000 |
11264 |
||||
���
Spreadability Test
Table 7. Test results
for the spreadability of herbal
toothpaste preparations combined with extracts of Anna apple peel (Malus
domestica) and kaffir lime peel
(Citrus hystrix) before and after storage using the accelerated
stability method with three replications
|
No |
Formulas |
Before Accelerated Storage |
After Expedited Storage |
Condition |
Results |
||
|
1. |
F1 |
I |
3.3cm |
I |
3.5cm |
3 - 5 cm |
Qualify |
|
II |
3.1cm |
II |
3.2cm |
||||
|
III |
3.2cm |
III |
3.4cm |
||||
|
Average |
3.2cm |
3.36cm |
|||||
|
2. |
F2 |
I |
3.4cm |
I |
3.6cm |
Qualify |
|
|
II |
3.2cm |
II |
3.2cm |
||||
|
III |
3.2cm |
III |
3.5cm |
||||
|
Average |
3.26cm |
3.43cm |
|||||
In this research, herbal toothpaste was made from natural ingredients
with a combination of Anna apple peel extract (Malus domestica) and
Jeruk Purut peel (Citrus hystrix) by varying Sodium Lauryl Sulfate 1.5%
and 2.5% as a surfactant or detergent with its primary function is to form foam
and has the cleaning power that can clean plaque and food residue easily.
The extraction technique used in this research is maceration. The advantage
of this technique is that the active substance of the extract is not easily
damaged, uses simple equipment, and is easy to work with. The submerged
material releases secondary metabolites due to the breakdown of the cytoplasm
from the breakdown of the cell wall and cell membrane caused by the pressure
difference between inside and outside the cell. 216 g of Anna's apple skin and
215 g of Jeruk Purut peel which had been dried, then soaked in 96% ethanol for
15 days, stirring occasionally and changing the solvent three times.
Furthermore, the resulting filtrate was evaporated using a Rotary Evaporator.
The ingredients used are Anna apple peel extract, Jeruk Purut peel
extract, Tocopherol as an antioxidant, Glycerol as a moisturizer, Calcium
Carbonate as an abrasive, Methyl Paraben as a preservative, Sodium Lauryl
Sulfate as a foaming agent, Sorbitol as a sweetener, Oleum Menthae Piperitae as
fragrances, dyes and Aqua Destillata. The finished toothpaste preparations were
tested for physical quality stability by organoleptic tests, homogeneity, pH,
foam height, viscosity, and spreadability tests.
Toothpaste organoleptic observation was done by looking at its texture,
color, and aroma. The observations of the two formulations were the
same, and the results obtained on the texture of the paste were semi-solid,
green in color, and smelled of mint. Thus the varied
concentration of Sodium Lauryl Sulfate had no effect on the organoleptic of the
toothpaste prepared. The test results are in table II.
Homogeneity
testing was done by smearing the preparation
on a petri dish and then visually see the preparation. The observations showed
no coarse grains, air bubbles, and separate parts when the preparation was
smeared on the cup. This means that the ingredients in the preparation are
uniform and evenly mixed and meet the requirements of SNI 12-3524-1995 (Warsy et al., 2016). The test results are shown in Table III.
The pH test is carried out using
a pH meter. The pH test aims to see the degree of acid in the preparation so
that it is comfortable to use and does not irritate the oral mucosa. The pH
test for the two formulations with three replications showed that the
toothpaste was still good because it was still in the 4.5 � 10.5 based on SNI
12-3524-1995. The test results used Two Way ANOVA P = 0.553 (ɑ > 0.05),
meaning there was no significant difference in the pH of the preparation before
and after storage. The changing pH indicates that the preparation during
storage is less stable but still meets the pH range in the pH requirements of
toothpaste preparations. The test results are shown in table IV.
The foam height test shows the
ability of a preparation to produce foam, in which the foaming agent used is
Sodium Lauryl Sulfate. The test was carried out by observing the height of the
foam formed from the toothpaste preparation to measure the strength of the
preparation in removing dirt and the ability to clean the mouth when brushing
teeth. In the formula made, there are variations in the concentration of the
foaming agent used. The test results show that when the concentration of Sodium
Lauryl Sulfate is high, the foam produced also increases. The foam height test
for both formulations with three replications showed that the results met the
requirements. The test results using Two Way ANOVA P = 0.495 (ɑ > 0.05)
proved no significant difference in the foam height before and after storage.
The results of the foam height test are shown in table V.
Viscosity testing was conducted
using a Brookfield viscometer measured with spindle number 4 at 30 rpm.
Viscosity is a quantity of fluid viscosity that measures the size of the
friction in the fluid. If the viscosity is
large, the object is increasingly difficult to move in the fluid. Viscosity is
closely related to toothpaste, so whether the preparation can stick well to the
toothbrush (Adrianto, 2012). After the cycling test, there is a decrease in the
viscosity value. The longer the storage time, the lower the viscosity value.
This is also due to the less stable storage temperature (Widarsih et al., 2017). The test results using Two Way ANOVA P = 0.181
(ɑ > 0.05) proved that there was no significant difference in
the viscosity of the preparation before and after storage. The
results of the viscosity test are shown in table VI.
The spreadability test was
carried out to know the mass of the toothpaste. The characteristics of quality
toothpaste are that it is easily removed from the tube and can maintain its
shape when applied to a toothbrush just before use (Lestari et al., 2020). The test results show that the diameter of F1
is 3.3 cm and F2 is 3.4 cm. This is due to the different concentrations of
foaming agents for the two formulas. The results of the spreadability
measurements showed that after the storage cycling test, the two formulas with
three replications experienced an increase in spreadability. However, the
spreading power diameter is still within the 3 � 5 cm standard range.
Meanwhile, the test results using Two Way ANOVA P = 0.553 (ɑ > 0.05)
proved that there was no significant difference in the spreadability of the
preparations before and after storage. The results of the spreading power test
are shown in table VII.
CONCLUSION
The study concluded that the combination of Anna apple (Malus
domestica) and Jeruk Purut (Citrus hystrix) peel extracts could be formulated
into herbal toothpaste preparations with varying concentrations of Sodium
Lauryl Sulfate 1.5% and 2.5%. Based on the results of the physical quality test
of toothpaste preparations, the two formulations of toothpaste combined with
extracts from the skin of the Anna apple (Malus domestica) and the Peel of the
Jeruk Purut (Citrus hystrix) with varying concentrations of 1.5% and 2.5%
sodium lauryl sulfate meet the requirements. Stability of physical quality
based on literature.
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