Effect of hydroxyapatite nila fish scale addition on 

compressive strength of GIC and RMGIC 

K Harahap1*, A Yudhit1, LT Anindita2 
1
Department of Dental Material and Technology, Faculty of Dentistry, Universitas 
Sumatera Utara, Jl. Alumni No.  Kampus USU Medan, Indonesia
2
Dental Student, Faculty of Dentistry, Universitas Sumatera Utara

*Corresponding author: [email protected] 

Abstract. The aim of this study was to evaluate the effect of hydroxyapatite nila fish scale
(Oreochromis niloticus) addition on compressive strength of glass ionomer cement and glass
ionomer cement modified resin as restorative materials. Fourty specimens were made from
glass ionomer cement and glass ionomer cement modified resin, respectively. Specimens
divided into four test groups there are control group, 2%, 5% and 8% hydroxyapatite addition.
Hydroxyapatite was synthesized from nila fish scale (Oreochromis niloticus) by combination
of heat-alkali treatment and calcination method in temperature 800℃ for 5 hours. Compressive
strength was measured by Universal Testing Machine. Data were analyzed by One Way
ANOVA followed by LSD tests (p<0.05). The results showed that 2% hydroxyapatite addition
into glass ionomer cement has the higher compressive strength (30.39 ± 0.76 MPa) than others.
For glass ionomer cement modified resin added with 2% hydroxyapatite showed the higher
compressive strength (….) than others. There is significant differences between test groups
(p<0.05) based on Anova oneway test. It can be concluded that the addition hydroxyapatite
from nila fish scales can increase the compressive strength of glass ionomer cement and glass
ionomer cement modified resin with 2% is an ideal amount.
Key words: GIC, RMGIC, hydroxyapatite, fish scale, compressive strength

1.  Introduction
Glass ionomer cement is a material which produced from combination of silicate cement and
polycarboxylic acid that introduced by Wilson and Kent in 1972. Glass ionomer cement used to
restore deciduous teeth, caries in class III and V. This material has advantages such as the ability to
release fluoride, translucent, can bind to tooth structure, good biocompatibility and has the same
coefficient of thermal expansion as tooth. 1,2 This material has disadvantages too like low mechanical
strength and tend to be wear. 3 One of the most important mechanical properties of glass ionomer
cement is compressive strength to resist masticatory load. 4
Karena beberapa kelemahan bahan ini, maka semen ionomer kaca dimodifikasi dengan
penambahan resin di dalam komposisinya. Penambahan monomer hidroksietilmetakrilat (HEMA) ke
dalam cairan semen ionomer kaca meningkatkan kekuatan dan ketahanan terhadap keausan. Selain itu,
dapat memperpanjang waktu kerja pada saat memanipulasinya. Proses pengerasan bahan ini
menggunakan aktivasi sinar tampak biru dengan panjang gelombang 450 nm. Akan tetapi, kekuatan
semen ionomer kaca modifikasi resin ini masih dibawah kekuatan resin komposit .
Several methods have been made to improve the mechanical properties of glass ionomer cement
and glass ionomer cement modified resin. Modifying it with resin, adding some fillers such as
hydroxyapatite, nanobioceramics fluoroapatite, nanoparticles forsterite, and others. 3 Hydroxyapatite is
one of the bioceramics that has recently been studied intensively, especially for medical applications.
Hydroxyapatite is widely applied for bone regeneration, bone and dental implants, and orthopedics.
Many used of the application is inseparable from the important properties possessed by hydroxyapatite
including bioresorbable, osteoconductive, biocompatible and non-toxic. 5 Hydroxyapatite can be
obtained from natural ingredients such as animal bones, egg shells and fish scales. Research by
Khaghani M, found that 5%wt microhydroxyapatite and nanohydroxyapatite addition to glass
ionomer cament, synthesized from bovine bone, can increase the compressive strength of glass
ionomer cement.3 Mozartha found the addition of 8 %wt of hydroxyapatite from eggshells to glass
ionomer cement can increase its compressive strength.6
In North Sumatra, Indonesia, the highest freshwater fish production is nila fish (Oreochromis
niloticus) with total production 110.144 tons. 9 Nila fish is a type of Tilapia originating from Nile river
valley of Africa, and was first imported to Indonesia in 1969, 1990 and 1994, each from Taiwan,
Thailand and Philippines. Nila fish belong in the phylum Chordata, class Pisces, sub class Teleostei,
Order Percomorphi, Subordo percoidea, Family Cichlidae, Genus Oreochromis, and Species
Oreochromis Sp.10 Researchers chose nila fish scales as a source of hydroxyapatite because nila fish
production in North Sumatra is the highest for freshwater fish species. With high numbers of nila fish
production, researchers want to take this opportunity to use nila fish scales waste and make it as a
useful material.
Chemical analysis shown that fish scales are considered a waste product that contain a lot of
calcium in the form of carbonates and oxides. 7 There are many organic and inorganic components in
fish scales. Organic components are around 40%-55%, including collagen, scleroprotein, lecithin, fat
and various vitamins, etc. The percentage of organic components is 7%-25%, including hydroxyapatite
and calcium phosphate.8
The aim of this study was to evaluate the compressive strength of restorative glass ionomer cement
and glass ionomer cement modified resin after addition of hydroxyapatite synthesized from nila fish
scales (Oreochromis niloticus).

2.  Materials and Methods
3. Hydroxyapatite synthesis
Eighty grams of nila fish scales are washed with soap and rinsed with distilled water until clean. Then
fish scales dried in the sun for three days. The dried fish scales are crushed with blender and sifted
with 200 mesh sieve. Sixty grams of nila fish scales powder were soaked in 250 ml HCl 0.1 M for 2
hours at room temperature and rinsed with distilled water until its free of acid measured by using
litmus paper. Fish scales powder were immersed in 50 ml of 5% NaOH then heated on a hot plate with
70 oC for 5 hours while stirring with magnetic stirrer. The white sediment were washed with distilled
water and dried at 60 oC using a hot plate. The white sediment powder then mixed with 5 mL 50%
NaOH in beaker and heated to 100 oC while stirring with a magnetic stirrer for 1 hour. The obtained
white sediment powder then rinsed with distilled water and then dried at 60 oC using an oven. The
powder is then calcined at 800 oC for 1 hour in the furnace to synthesize hydroxyapatite ceramics.
Hydroxyapatite ceramics are then crushed using mortar and pestle and filtered with a 200 mesh filter
to obtain hydroxyapatite powder. The obtained hydroxyapatite powder is keep in a closed and dry
container.
2.2 Samples preparation 
In each group there were 10 samples and were divided into 4 groups. Group 1 (without addition of
hydroxyapatite), group 2 (addition of 2 %wt of hydroxyapatite), group 3 (addition of 5 %wt of
hydroxyapatite, and group 4 (addition of 8 %wt of hydroxyapatite). Cylinder shaped samples with a
diameter of 4 mm and a height of 6 mm were made from type II glass ionomer cement (GC Gold
Label HS Posterior EXTRA, Fuji, Japan). In group 1, samples were made with a ratio of powdered
glass ionomer cement with hydroxyapatite powder as much as 0.36 g of glass ionomer cement without
the addition of hydroxyapatite. Group 2, samples were made with a ratio of powdered glass ionomer
cement with hydroxyapatite powder as much as 0.35 g glass ionomer cement and 0.01 g
hydroxyapatite. Group 3, samples were made with a ratio of powdered glass ionomer cement with
hydroxyapatite powder as much as 0.34 g glass ionomer cement and 0.02 g hydroxyapatite. Group 4,
samples were made with a ratio of powdered glass ionomer cement with hydroxyapatite powder as
much as 0.33 g of glass ionomer cement and 0.03 g of hydroxyapatite. The powder is mixed with the
liquid of glass ionomer cement 0.14 g on a paper pad for 30 seconds. The homogeneous mixture is
then inserted using a plastis instrument into the mold on the master cast which has been smeared with
silicone oil and covered with a celluloid strip below it. The upper part of the mold covered with glass
slide and given a load of 1 kg to harden 2 minutes 20 seconds. Then the sample is removed from the
mold. Samples were kept in a closed container for 24 hours at room temperature .

2.3 Compressive strength test

After 24 hours, the compressive strength test was carried out on the sample. Each sample to be tested
is placed on a placemat on a Universal Testing Machine (Tensilon, Dynatech, Japan). Then pressed
with a crosshead speed of 0.5 mm / minute and a load of 500 KgF until the sample breaks. The result
of the load value when the sample breaks will be seen on the scale shown on the screen of the
compression test equipment. Compressive strength is calculated using a formula K = 4F/πd2. Where K
is compressive strength (Mpa), F is the load at fracture (KgF), and d is the diameter of the cylindrical
specimen (mm).

2.4 Analysis data

4.  Results
The mean value and standard deviation of group 1 (without addition of hydroxyapatite) is 19.88 ±
1.12, group 2 (with the addition of 2 %wt hydroxyapatite) is 30.39 ± 0.76, group 3 (with the addition
of 5 %wt hydroxyapatite) is 26.89 ± 1.15 and group 4 (with the addition of 8 %wt hydroxyapatite) is
22.79 ± 1.11 can be seen in table 1.

Table 1. Mean value of compressive strength.

Compressive Strength (MPa)

Test Groups Glass ionomer cement Glass ionomer cement
modified resin
Control
2% Hydroxyapatite
5% Hydroxyapatite
8% Hydroxyapatite
5.  Discussion

6.  Conclusion

7.  Acknowledgement

References
[1] A reference
This reference has two entries but the second one is not numbered (it uses the ‘Reference (no
number)’ style.
[2] Another reference
[3] More references