USE OF FTIR TO EVALUATE THE ABSORPTION AND SOLUBILITY
IN DIET FOOD OF DENTAL COMPOSITE
Rosemarie R. Rezende 1, Hermes S. Costa1, Ezequiel S. Costa Jr.1
1Department
of Materials, Federal Center of Technological Education of Minas Gerais, Belo Horizonte
(MG), Brasil
E-mail: rosemarierezende@yahoo.com.br
Summary. The components present in food can cause alteration in the properties of dental composites. The
objective of this study was to evaluate the absorption and solubility of two nanohybrid composite in alcoholic
and non alcoholic media of the diet. 130 specimens of rectangular shape, with 24mm x 4mm x 0,4mm, prepared
from two light cured dental composite were stored at 37ºC for 48h. Measures were taken of the volume and mass,
and immersed for 7 and 14 days in one of the study medias (water, cachaça, beer, soft drink and wine). After this
period, news measures were taken in 120 specimens to check the inclusion/deletion of elements of the media and
again stored at 37ºC for 48h to obtain its ending mass. Ten specimens immersed for 7 days were analyzed by
FTIR to determine the addition/removal elements of the media. The spectra obtained were compared with the
spectra of the samples before immersion in the media studied. The alcoholic media promoted absorption from
24,4µm/mm³ and the non alcoholic media of 13,4µm/mm³. A greater absorption of water for greater period of
immersion. The reduced mass of the specimens was similar to the alcoholic media (3.5µm/mm³) and non
alcoholic media (3,5µm/mm³). The FTIR showed a change in the intensity of hydroxyl groups after immersion in
beer, soft drink and wine. The immersion of dental composites in the media, that are present in human diet, is
capable of promoting the reaction in the structure of these materials being such changes dependents on media
and time that these materials are exposed to these medias.
Keywords: Composites, Degradation, Diet
1. INTRODUCTION
Several materials have been research and used to replace missing parts of the teeth.
Currently, a composite is used as an aesthetic restorative material. This composite is formed
by inorganic particles and organic matrix that are bonded with bonding agents (WILLEMS,
1995; PEUTZFELD, 1997; MORAES et al., 2003a; MCCABE & WALLS, 2006;
ZIMMERLI et al., 2010). Performing its function, the composite is subjected the presence of
liquids, from food and oral hygienic, which can be absorbed or induces the releases of
elements of the composites (SIDERIDOU et al., 2004; AKOVA et al., 2006; LUIZ, 2007).
The organic matrix type is responsible for absorption, as a good bond with the inorganic
particle prevent that water penetrating between the matrix and particle (MORAES et al.,
2003b; RAWLS & ESQUIVEL-UPSHAW, 2005). The hydroxyl groups’ presents in the
organic matrix increase the absorption of water (ADA, 2003). The solubility and absorption
of the composite cause reduction of resistance to wear and abrasion, color instability and
leakage of inorganic particle (ADA, 2003).
It’s possible to use infrared spectroscopy in Fourier transform (FTIR) to determine the
functional groups of material (PICCOLI et al., 2006). Thus, the objective of this study was to
determine the absorption and solubility of two composites with different organic matrix, using
the ISO4049 recommendations and FTIR.
2. MATERIALS AND METHODS
Were used two commercial composites: Composite A - with the organic matrix
consisting of Urethane Bis-GMA modified, Bis-EMA (ethoxylated bisphenol A
dimethacrylate) and TEGDMA (triethylene-glycol dimethacrylate) and Composite B with
Bis-GMA (bisphenol A dimethacrylate), and TEGDMA in their matrix.
The media used were distilled water (1), cachaça (2), beer (3), soft drink (4) and wine
(5).
65 rectangular specimens of each composite, with dimensions of 24mm x 4mm x
0,4mm, were placed in glass containers and keep dry at 37°C for 48h, had its volume
calculate and were weighed in a digital scale to obtained the initial mass (m1) e subjected to
the media for 7 and 14 days, being measures at the final of these periods to obtain the satured
mass (m2). After this second measures, 60 specimens of each composite were placed again
dried at 37°C for 48h to evaporated the liquids absorbed and the ending mass (m3) were
obtained. The absorption was obtained but the difference between the satured mass (m2) and
the ending mass (m3), while the solubility was given by the difference between initial mass
(m1) and ending mass (m3). 5 specimens of each composite immersed for 7 days were dried
on paper towels and analyzed by FTIR.
Absorption =
Solubility =
(m2 – m3 )
V
(m1 – m3 )
V
in µg/mm3
in µg/mm3
Where:

m1 = weight of specimens before immersion in water;

m2 = weight of specimens after immersion in water;

m3 = weight of specimens after immersion in water and drying;

V = specimens volume in mm3
The FTIR was performed on equipment IRPrestige-21 model, Shimadzu, with a
resolution of 4cm-1, using a wavelength in the range 4000 to 400cm-1. The material was
placed on the ATR crystal.
The medias were changed every 24 hours.
3. RESULTS AND DISCUSSION
The table 1 shows the average of the absorption and solubility with the medias
(alcoholic and non alcoholic) used and the FTIR spectra for the Composite A are shows in the
figure 1A and for the composite Composite B in the figure 1B, including the range between
3.750 to 750cm-1. It is possible to relate the chemical groups presents in the composite using
correlation tables and wave numbers, however, this identification is not without error
(COSTA, 2005). The various peaks presents in the spectra were associated to the presence of
compounds identified in table 2 according to literature (SKOOG et al., 2002; ORÉFICE et al.,
2003; MORAES, 2004; COSTA, 2005; ROCHA, 2006; BEUN et al., 2007).
According to the ADA (2003) the composites must have absorption less than
40µg/mm3 and solubility less than 7,5µg/mm3 after immersion for seven days in water. The
results presented on immersion in water, shows that absorption and solubility are consistent
with the ADA(2003), in seven days, but the solubility of Composite B showed an inspected
increase in 14 days, therefore, Archegas (2005) observed that solubility was higher in the first
24 hours.
Table 1 - Average results of absorption and solubility in µg/mm3
Tests
Absorption
µg/mm³
Composite
Time
Water
Soft drink
Cachaça
Wine
Beer
Composite A
7
7,33
7,7
49,12
26,94
18,77
14
7,59
3,82
21,57
7,29
7,31
7
24,41
27,49
51,68
17,62
25,11
14
28,06
0
24,51
16,79
22,59
7
-2,48
-3,2
11,21
0,57
-7.32
14
3,79
0,17
0
0
0
7
2,8
13,55
18,57
0
7,26
14
16,82
-3,21
7,12
-10,11
16,04
Composite B
Composite A
Solubility
µg/mm³
Composite B
10
9
8 7654 32
1
A
wine
Intensity (u.a.)
soft drink
beer
cachaça
water
without
immersion
3500
3000
2500
2000
1500
1000
8 7654 32
1
-1
Wavelenght(cm )
10
9
B
wine
Intensity (u.a.)
soft drink
beer
cachaça
water
without
immersion
3500
3000
2500
2000
1500
1000
-1
Wavelenght(cm )
Figure 1 - FTIR spectra of Composite A and Composite B before and after immersion in the medias
.
Table 2 – Identification of chemical groups of composite
Absorption in (cm-1)
Chemical groups
1
2
3
4,5,6
7
8
9
10
940
1234
1294
1454, 1509, 1608
1635
1716
2922
3335
C-C and CH2
Si-O
C-O
C=C of the aromatic rings
C=C of aliphatic chain
C=O
C-H
O-H
Comparing alcoholic media and non alcoholic, it is observed that alcoholic media
shows higher absorption that non alcoholic media, which is suggest by Ferracane et al. (1998),
that the water may be less aggressive. The solubility was greater in alcoholic media for the
composite Composite A, which is in accordance with Pfeifer et al., (2009), but for the
composite Composite B the solubility in the soft drink was higher than in wine and beer. With
variance analysis, it’s observed that for absorptions the media (p=0,005) and time (p= 0,015)
were significant (p<0,05) and not the composite (p=0,194). For the solubility, no factor is
significant (composite p=0,051, time p=0,764 and media p=0,282). The interactions between
the factors aren’t significant for absorption and solubility.
The solubility occurs mainly by the release of unreached components and degradation
products of the composite (FERRACANE, 2006). Different results are probably related to the
composition and polymerization of the composite used, because the composites exhibit
differences in the composition of the organic matrix and inorganic filler similar (BERGER et
al., 2009; ÖRTENGREN et al., 2001). The commercially available resins, including those
used in this study, are combinations of Bis-GMA, TEGDMA, UDMA and Bis-EMA. Based
on the characteristics of each one of the monomers, it is expected that the composite
Composite A having less absorption, because Bis-EMA has a structure similar to Bis-GMA,
but less two hydroxyl groups (PEUTZFELD, 1997; ÖRTENGREN et al., 2001; ADA, 2003),
which was confirmed by this test. The presence of Bis-GMA and TEGDMA in the
composition of the composite Composite B may be responsible for the increased absorption
according Sideridou et al. (2004). Besides the composition of the matrix, the amount of each
monomer and the effectiveness of silanization, must be consider (ASAOKA & HIRANO,
2003; NOORT, 2004; RAWLS & ESQUIVEL-UPSHAW, 2005; FERRACANE, 2006).
Can be seen, in the spectra shown in Figure 1, chemical modifications of the samples
after immersion in the media tested. When water or chemical solvents, such as ethanol,
penetrate the polymer, can cause swelling and start the chemical degradation creating
oligomers and monomers, which gradually change the microstructure of the polymer, forming
pores which release the components (GÖPFERICH, 2005; FERRACANE, 2006; PFEIFER et
al., 2009). In their work, using Raman spectroscopy, Luiz (2007) observed no reaction
between the resin and the components of the beverage, but in this study using the FTIR, it was
possible to observe the emergence of peaks between the bands 3700 to 3000cm-1, especially
after immersion in beer, soft drink and wine. The only media that this change was not caused
is the water. This difference suggests the presence of hydroxyl groups absorbed the media or
resulting from changes in the polymer chain.
CONCLUSIONS
The water absorption of the composite tested were the according the Standards
required by ADA, but the composite Composite B has solubility above the standards in 14
days. Immersion of dental composite in that medias present in human food can cause
alterations in the structure of these materials, such modifications dependents on the media and
time that the composite are exposed to such medias.
ACKNOWLEDGMENTS
The authors gratefully acknowledge CAPES, CNPq, FAPEMIG and CEFET/MG.
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