CHARACTERIZATION NANOPARTICLES

ETHANOL EXTRACT OF BETEL NUT (Areca

catechu L) IN VARIOUS CONCENTRATION OF
CHITOSAN
Magfirah1, Ayu andira 2, Muthmainah Tuldjanah 3, Rezky Yanuarti4, Indah Kurnia Utami5,Joni Tandi6
1,2,4,5,6
STIFA Pelita Mas Palu, Pharmacy S1, Palu, Sulawesi Tengah, 94125
2
STIFA Pelita Mas Palu, Pharmacy S1, Palu, Sulawesi Tengah, 94125
Email: magfiralukman@gmail.com1; yundira22 @gmail.com2, muthmainah tuldjanah@email.com3

ABSTRACT
Introduction: Betel nut (Areca catechu L.) contains tannins that are effective as anthelmintics. Nanoparticles
aim to overcome the solubility of active substances that are difficult to dissolve, improve poor bioavailability,
and modify drug delivery systems so that drugs can go directly to specific areas. Purpose: This study aims to
make nanoparticles of betel nut ethanol extract using various concentrations of chitosan, to determine
differences in the characterization of nanoparticles using various concentrations of chitosan. Methodology:
This type of research is experimental laboratory research with quantitative and qualitative approaches. The
nanoparticles were made by ionic gelation method using variations of chitosan and NaTPP with 3 variations
of the formula between chitosan and NaTPP solutions, namely the ratio of 8:1, 10:1, and 12:1. The formed
nanoparticles were then characterized including organoleptic, pH, nanoparticle size, polydispersity index,
Scanning electron microscopy (SEM), and dissolution. Findings The smallest size of nanoparticles of betel
nut ethanol extract was obtained with the formula of chitosan and NaTPP 8:1 (144.4nm), polydispersity index
0.427, and pH value of 6.47. SEM was in the form of irregularly shaped lumps, and dissolution was 66.99%.
Originality/ Value/ Implication: Ethanol extract from areca nut can be made into nanoparticles using
various concentrations of chitosan.

Keywords: ethanol extract of betel nut, characterization, nanoparticles

ABSTRAK

Biji pinang (Areca catechu L.) mengandung tanin yang efektif sebagai antelmentik. Nanopartikel
bertujuan untuk mengatasi kelarutan zat aktif yang sukar larut, memperbaiki bioavailabilitas yang
buruk, memodifikasi sistem penghantaran obat sehingga obat dapat langsung menuju daerah
sfesifik. Penelitian ini bertujuan untuk Membuat nanopartikel ekstrak etanol biji pinang dengan
menggunakan berbagai variasi konsentrasi kitosan, mengetahui perbedaan karakterisasi
nanopartikel menggunakan berbagai konsentrasi kitosan. Jenis penelitian ini merupakan penelitian
eksperimental laboratorium dengan pendekatan kuantitatif dan kualitatif. Nanopartikel dibuat
dengan metode gelasi ionik menggunakan variasi kitosan dan NaTPP dengan 3 variasi formula
antara larutan kitosan dan NaTPP yaitu rasio 8:1 10:1 dan 12:1. Nanopartikel yang terbentuk
kemudian dikarakterisasi meliputi organoleptik, pH, ukuran nanopartikel, distribusi partikel,
Scanning electron microscopy (SEM) dan disolusi. Hasil penelitian menunjukkan bentuk serbuk
berwarnacoklat dan beraroma khas pinang dengan nilai pH 6,47. Ukuran terkecil nanopartikel
ekstrak etanol biji pinang diperoleh dengan formula kitosan dan NaTPP 8:1 (144,4nm),distribusi
partikel 0.427. SEM berupa bongkahan yang berbentuk tidak beraturan, dan disolusi 66,99%.
Ekstrak etanol dari biji pinang (Areca catechu L.) dapat dibuat menjadi nanopartikel dengan
menggunakan berbagai variasi konsentrasi kitosan.

Kata Kunci : Ekstrak etanol biji pinang, Karakterisasi, Nanopartikel

1. INTRODUCTION Kalimantan and Maluku. Rural
Nanotechnology can make drug communities use betel nut to treat
active ingredients into particles with a inflammation, diarrhea, intestinal worms,
nanometer size, which is less than 1 flatulence due to indigestion, and coughing
micrometer. Nanotechnology does not only up phlegm. Previous research has said that
produce nanometer-sized particles but has a this plant contains tannins, alkaloids,
broader meaning, including how to flavonoids, and saponins(Ferdiansyah et al.,
produce, knowing the use of new properties 2016).
that arise from nanomaterials that have Based on the above background,
been made. (Ayumi et al., 2018). researchers are interested in making
One of the factors that affect the nanoparticles of ethanol extract from areca
effectiveness of drugs is particle size nut using the ionic gelation method by
because particle size is very influential in characterizing the nanoparticles including
the process of solubility, absorption, and organoleptic testing, pH, particle size using
distribution of drugs. (Prasetyorini et al., PSA (Particle Size Analyzer), and particle
2011). morphology using SEM (Scanning Electron
Chitosan nanoparticles can be Microscopy), as well as conducting
absorbed by human organs that can dissolution test.
penetrate nano-sized membranes such as 2. RESEARCH METHODS
the kidneys, liver, and lungs. Particles with 2.1 Instrument
a narrow distribution will result in more Glassware (Pyreex®), dissolution
efficient drug delivery. test equipment, freezer (Panasonic), watch
Chitosan is a natural polysaccharide glass, magnetic stirrer (MR Hei-Tec), pH
[(1→4) glucosamine (2-amino-2-deoxy-d- Meter (Livobond), PSA (Particle Size
glucose)] that has been widely applied in Analyzer), Vacuum Evaporator, a set of the
the pharmaceutical, food, and health centrifuge (centrifuge PLC series), SEM
industries. Chitosan nanoparticles have the (Scanning Electron Microscope),
advantage that they can be used as a matrix Spectrophotometry, Analytical Balance,
for various plant extracts and drugs(Sugita, container, water bat (members).
2019). 2.2 Materials
Herbal nanoparticle technology is Acetic acid glacial, aqua dest, areca
still being developed in Indonesia. Areca nut (Areca catechu L.), ethanol Pa, 96%
catechu L. known as areca nut is a plant ethanol, chitosan, and Na.TPP (Sodium
from the Arecaceae family. Areca nut Tripolyphosphate).
plants can be found in Sumatra, Java,
2.3 Preparation betel nut extract
Areca nut Simplicia powder as much
as 200 grams is put into a vessel or
container and then soaked with 96%
ethanol for 3 times 24 hours, protected from
sunlight while stirring frequently. After
that, it was filtered and the filtrate obtained
was collected and concentrated using a
vacuum evaporator and evaporated using a
water bath to obtain a thick ethanol extract
of areca nut.
2.4 Preparation Chitosan Solution
Chitosan 0.08 grams was weighed
using a watch glass, then the weighed
chitosan was dissolved with 100 ml of 1%
glacial acetic acid solution and stirred using
a magnetic stirrer for 30 minutes until the
chitosan dissolved.
Preparation of Sodium Tripolyphosphate
(NaTPP) Solution
A total of 0.04 grams NaTPP is
dissolved in a beaker then add 400 ml of
distilled water. After that, it was stirred
using a magnetic stirrer until dissolved for
30 minutes.
Preparation of Areca Seed Extract
Nanoparticles
Nanoparticles were made using
ethanol extract of areca nut 1 gram of thick
extract dissolved in 35 ml of ethanol pa and
15 ml of distilled water in a 1000 ml beaker
then add 100 ml of the chitosan solution
that had been made in 1% acetic acid
solution. Then gradually 40 ml of NaTPP
was added to the mixture by stirring using a
magnetic stirrer at a speed of 3000 rpm for
2 hours (Kurniasari and Atun, 2016).
The mixed materials were then
separated using a centrifuge at 3500 rpm for
15 minutes. The areca nut nanoparticle
suspension was put in the freezer for 2 days
at -40C, then continued in the refrigerator at
30C until it became dry powder.
(Kurniasari and Atun, 2017).
2.5 Nanoparticle Characterization
2.5.1 Organoleptic Test
The test was carried out by directly
observing the shape, smell, and color of the
prepared nanoparticles.
2.5.2 Measurement of nanoparticles and
particle distribution.
The size of the nanoparticles and the
distribution of the particles were obtained
from measurements using a PSA tool. A
total of 10 ml samples of areca nut
nanoparticles for each formula were
replicated 3 times. The sample is put into a
cuvette. Next, the PSA tool is
operated(Prihantini et al., 2020).
2.5.3 pH test
The pH test was carried out using a
pH meter. The areca nut nanoparticle
sample is inserted into the container, then
the electrode is dipped into the container
filled with the sample, the number is
allowed to move until it reaches a constant
position. The number indicated by the pH
meter is the pH value of the nanoparticle
preparation(Magfirah and Utami, 2020).
2.5 Nanoparticle Morphological Analysis
Morphological analysis of
appearance of chitosan nanoparticles from
betel nut ethanol extract using SEM. The
sample is attached to the set holder with
double adhesive, then coated with gold
metal under vacuum. After that, the sample
is inserted into a place in the SEM, then the
image is observed and magnified 5000
times(Magfirah and Utami, 2020).
Dissolution Test
A total of 0.5 grams of areca nut
ethanol extract nanoparticles
dissolved in 900 ml of distilled water using
a dissolution device at a temperature of
370C with a stirring speed of 100 rpm for
30 minutes. A total of 5 ml samples were
taken at 5, 10, 15, 20, 25, and 30 minutes.
Each time the sample was taken, the
volume of the taken medium was replaced
with a new medium solution with the same
the volume and temperature. Each sample was
filtered and analyzed using UV-VIS
spectrophotometry at a wavelength of
760nm(Pakki Ermina, 2016).
3. DATA ANALYSIS
The results of the areca nut ethanol
extract nanoparticles were analyzed visually
based on organoleptic observations. The pH
measurement was carried out using a pH
meter. Particle size and distribution were
observed using a PSA tool, and
were confirmation of nanoparticle morphology
visualization was carried out using SEM.
Data on organoleptic results, pH, particle
size and distribution, and Scanning Electron
Microscope (SEM) were compared with the
requirements of several library sources. The
data from the observation of particle
morphology were analyzed descriptively.

4. Results and Discussion

4.1 Results
Table 1. The results of the organoleptic test for the preparation of areca nut ethanol
extract nanoparticles
Organoleptic Observations
Formula
Day 0 7th day Day 14 Day 21
Brown powder, Brown powder, Brown powder, Brown powder,
distinctive aroma distinctive aroma distinctive aroma distinctive aroma
F1
of areca nut of areca nut of areca nut of areca nut
extract. extract. extract. extract.
Brown powder, Brown powder, Brown powder, Brown powder,
distinctive aroma distinctive aroma distinctive aroma distinctive aroma
F2
of areca nut of areca nut of areca nut of areca nut
extract. extract. extract. extract.
 Brown powder, Brown powder, Brown powder, Brown powder,
distinctive aroma distinctive aroma distinctive aroma distinctive aroma
F3
of areca nut of areca nut of areca nut of areca nut
extract. extract. extract. extract.

Table.2 pH test results for betel nut ethanol extract nanoparticles

the pH of areca nut nanoparticles
Formula
Day 0 7th day 14th day Day 21 Average
F1 6.46 6.46 6.47 6.47 6.47
F2 6.56 6.53 6.51 6.53 6.53
F3 6.65 6.67 6.69 6.68 6.67

Table. 3 Particle size test results for betel nut ethanol extract nanoparticles
Nanoparticle Size
Formula
Average ± SD
F1 146.1 nm 146.4 nm 140.7 nm 144.4 nm ±3.208
F2 157.7 nm 173.5 nm 157.4 nm 162.9 nm ± 9,210
F3 383.9 nm 451.9 nm 397.3 nm 411 nm ± 36,020

Table 4. Results of particle distribution test for betel nut ethanol extract nanoparticles
particle distribution
Formula
A B C Average
F1 0.405 0.451 0.424 0.427 ± 0.023
F2 0.544 0.736 0.535 0.605 ± 0.114
F3 0.897 1.305 0.977 1.060 ± 0.216
 Figure 1. SEM results for the preparation of betel nut ethanol extract nanoparticles

Table. 5 Dissolution Test Results

Level Correctio Corrected Dissolution
Minute Absorbance Fp
(mg) n Factor Rate Rate
5 0.1921 5 50.59 0 50.59 59.14
10 0.1929 5 50.81 0.2811 51.09 59.72
15 0.1941 5 51.13 0.5634 51.69 60.43
20 0.1677 5 51.83 0.8474 52.68 61.59
25 0.1699 5 51.89 0.8487 52.74 61.65
30 0.1975 5 52.05 1.1370 53.19 62.18
Average soluble content 60.79%

Discussion The formulation of nanoparticles was

Areca nuts are extracted using the made using ethanol extract of areca nut as
maceration method using 96% ethanol as a the active ingredient. The formulation of
solvent. The viscous extract obtained after nanoparticles of areca nut ethanol extract
the solvent separation was carried out using was made with 3 concentrations of chitosan
a rotary evaporator resulting in a viscous variations, namely 0.08%, 0.1%, and
extract of 75 grams with an extract 0.12%. The finished nanoparticle
percentage of 18.75 %. preparations were evaluated for their
Nanoparticles of betel nut ethanol physicochemical quality. Evaluation of the
extract were prepared by the ionic gelation physical and chemical quality of betel nut
method. In the manufacturing process, 5 ethanol extract nanoparticles included
grams of areca nut ethanol extract was used organoleptic tests, pH tests, particle size
so that the number of nanoparticles of betel tests, and morphology tests or SEM. Tests
nut extract was 0.7 grams with a yield value were carried out for 21 days of storage with
of 14%. tests on days 1, 7, 14, and 21
 Characterization using organoleptic
results obtained brown powder,
distinctive aroma of betel nut extract and
the pH test obtained an average result of
6.47. The particle size test using the PSA
tool shows the results with the smallest
nanometer-size being formula 1, which is
144.4 nm with a ratio of 0.08% chitosan
and 0.01% NaTPP. The polydispersity
index value is 0.427. So the composition of
chitosan and NaTPP (8:1) is the optimum
concentration of chitosan and produces
nanometer particle size.
The particle size results show that the
particle size is influenced by the amount of
chitosan and NaTPP used where the particle
size increases with the amount of chitosan
and NaTPP used. (Nurwaini et al., 2019).
Characterization using the SEM tool
aims to see the shape of the surface of the
nanoparticles. SEM analysis was carried
out on formula 1 with a magnification of
2000x and 5000x. The surface morphology
of the nanoparticles was irregularly shaped
with a wavy and uneven surface.
The dissolution test was carried out
using a dissolution device at a temperature
of 370C at a speed of 100 rpm for 30
minutes. The results are shown in Figure
4.4. In the picture, the dissolution results of
the areca nut nanoparticles show a higher
percent dissolution compared to the areca
nut ethanol extract, this is because the
particle size is smaller, so the surface area
will be larger. A larger surface allows
greater interaction with solvent leading to
a increased solubility(Karma, 2020).
CONCLUSION
Ethanol extract from betel nut (Areca
catechu L.) can be made into nanoparticles
using various concentrations of chitosan.
The optimal concentration of chitosan and
NaTPP to form nanoparticles is in formula
1 with a size of 144.4 nm and a particle
distribution value of 0.427. There are
differences in the characterization of
nanoparticles using various concentrations
of chitosan. The difference is that in the pH
test the average value for formula 1 is 6.47,
formula 2 is 6.53, and formula 3 is 6.67.
For the particle size, the results for formula
1 are 144.4 nm, formula 2 is 162.9 nm and
formula 3 is 411 nm and the results for the
distribution of nanoparticles are obtained in
formula 1, which is 0.427, formula 2 is
0.605, and formula 3 is 1.060.
SUGGESTION
Based on the research that has been
done, it is suggested to conduct further
research so that the nanoparticles of the
ethanol extract of areca nut are tested for %
transmittance.
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