Journal of Dental Sciences (2019) 14, 87e92

Available online at www.sciencedirect.com

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journal homepage: www.e-jds.com

Original Article

Surface degradation of composite resins

under staining and brushing challenges
Tânia Mara da Silva a*, Débora Cristina Barbosa Dantas b,
Tainá Teixeira Franco b, Lucas Teixeira Franco b,
Maria Filomena Rocha Lima Huhtala b

a
Dentistry College, INAPÓS- Instituto Nacional de Ensino Superior “Padre Gervásio”, Pouso Alegre,
MG, Brazil
b
Department of Restorative Dentistry, Institute of Science and Technology, Sao Paulo State University
(Unesp), São José dos Campos, SP, Brazil

Received 26 July 2018; Final revision received 6 October 2018

Available online 7 December 2018

KEYWORDS Abstract Background/purpose: The primeval evaluation of the properties of composite

Color; resins with different compositions that impact clinical behavior is very important in guiding
Composite resins; use in clinical settings. The aim of this study was to evaluate color stability (DE) and Knoop
Hardness; microhardness (KHN) of composite resins containing different compositions.
Toothpastes Materials and methods: Forty-five disks were made composite resins: Filtek Z350 XT/3MESPE
and Beautifill II/SHOFU and divided into 3 subgroups: Control - immersed in artificial saliva;
OB e brushing with Oral B 3D White; CT - brushing with Colgate Total 12. The OB and CT groups
had the disks brushed daily with 120 cycles after immersion in coffee solution (10 min) for a
period of 30 days. DE and KHN was obtained at baseline and after the treatments. Data were
analyzed ANOVA and Tukey tests (p < 0.05).
Results: ANOVA revealed significant differences for DE and KHN. DE: the highest mean was
observed in Beautifil II composite resin group, which differed significantly from Z350 group.
For the Beautifil II, the treatments were significantly different from each other. For the
Z350, the control group showed significant differences in relation to OB e CT groups. KHN:
the highest mean was observed in Z350 group, which differed significantly from Beautifil II
group. For Z350, the control group showed significant differences in relation to OB e CT groups.
For Beautifil II, the treatments did not differ significantly among themselves.
Conclusion: The composite resin containing fluoride in the composition showed higher color
alteration (DE) and lower Knoop microhardness (KHN), thus demonstrating that composition
is an important factor in the clinical performance of esthetic restorative materials.
ª 2019 Association for Dental Sciences of the Republic of China. Publishing services by Elsevier
B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.
org/licenses/by-nc-nd/4.0/).

* Corresponding author. Avenida Engenheiro Francisco José Longo, 777, Jardim São Dimas, São José dos Campos, SP 12245-000, Brazil.
E-mail address: [email protected] (T. Mara da Silva).

https://doi.org/10.1016/j.jds.2018.11.005
1991-7902/ª 2019 Association for Dental Sciences of the Republic of China. Publishing services by Elsevier B.V. This is an open access article under
the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
88 T. Mara da Silva et al

Introduction conventional composites.16 On the other hand, new ques-

tions arise on the profile of these materials in relation to
The increasing in the esthetic demanding associated with the daily habits of feeding and hygiene compared with
the improvements in the properties and power of bonding other nanohybrid composites. Thus, this study aimed to
to the tooth substrate result in the supremacy of composite evaluate the color alteration (DE) and Knoop surface
resin over other restorative materials.1 Composite resins microhardness (KHN) of nanoparticle-reinforced composite
aim to mimic the natural features of the tooth, such as the resins containing different compositions, after staining
color, translucency, and texture similar to the teeth. induced by coffee solution and abrasion challenge through
The composition of the composite resin evolves signifi- simulated toothbrushing. The null hypothesis was that no
cantly over the years. Alterations in the matrix composi- significance differences occur in color and superficial
tion, e.g. type and size of filler particles, exemplifies the microhardness between the studied composite resins
constant evolution of this restorative material.2 Recently, a regardless of the surface treatment to which they were
nanohybrid resin composite with surface pre-reactive glass submitted.
(S-PRG) ionomer cement promises to release and uptake
fluoride in the oral environment.3,4 Materials and methods
Since the discovery of a therapeutic agent in preventing
carious lesion, fluoride is largely used in Dentistry with Specimen preparation
different vehicles (gel, varnish, dentifrice, and mouthrinse)
and incorporated into water and food (salt, milk, juice, Forty-five cylindrical specimens were fabricated (shade
soda, and fluoride supplements). The fluoride ability to A2), using a metallic matrix with 2 mm in height and 3 mm
increase the resistance against demineralization, decrease in diameter, of each composite resin brand: Filtek Z350 XT
the microbial activity, and consequently also decrease the (Nanoparticle; 3M/ESPE, St. Paul, MN, USA) and Beautifil II
occurrence of secondary carious lesions is very known in (Nanohybrid; Shofu Inc., Kyoto, Japan). A polyester matrix
current Dentistry. Therefore, composite resins containing was placed over the composite resin and pressed with a
fluoride, aiming to obtain the advantages promoted by this glass slide to provide a flat surface. The composite resin
ion in tooth/restoration interface, would be considered as was inserted in increments of 2-mm and cured on the top
restorative material of great clinical applicability, due to surface using LED curing unit (Elipar Freelight 2, 3M/ESPE,
the capability of fluoride to influence caries risk of tooth St. Paul, MN, USA) at 1200 mW/cm2 power density, acti-
structure adjacent to the restoration. Previous studies vated for 40 s. After curing, the specimens were stored
show similar results regarding mechanical properties of individually in deionized water for 24 h. Then, the speci-
fluoride and conventional composite resin.5 mens were polished using a sequence of 1200, 2400 and
However, the drawbacks of composite resin restoration 4000 grit aluminum oxide abrasive disks (Extec, Enfield, CT,
are surface degradation, technique, fracture, and color USA) in a polishing device (DP-10, Panambra, São Paulo,
alteration.5 These are the main reasons for composite resin Brazil). After polishing, all specimens were stored in
replacement,1 probably because the continuous exposure deionized water at 37
C for 24 h.
to saliva and beverages/food stains within oral conditions. The specimens of each composite resin (n Z 45) were
Previous studies report that direct esthetic restorative randomly divided into 3 subgroups (n Z 15), according to
materials present in vitro and in vivo color instability with the type of toothpaste used: Control Group - The samples
staining.6e8 were immersed in artificial saliva, at 37
C, throughout the
At long term, the surface alterations of composite resin period of study; Colgate Total 12 - The samples were sub-
may occur according to intrinsic and extrinsic factors which mitted daily to brushing cycles with Colgate Total 12
restorations are routinely exposed6: insufficient polymeri- toothpaste (Colgate-Palmolive Industrial Ltda, São Ber-
zation, water sorption, and staining from diet and hygiene nardo do Campos, SP, Brazil), after immersion in coffee
habits of the patient.8,9 Some studies correlate the size and solution for 10 min, under agitation, for 30 days; Oral B 3D
distribution of filler particles and the matrix composition of Group - The samples were submitted daily to brushing cy-
composite resin as factors to interfere in color alteration. cles with Oral B 3D toothpaste (Procter & Gamble Brazil,
The discoloration of composite resin might be related to Louveira, SP, Brazil) after immersion in coffee solution for
the degree of the water sorption and the hydrophilic 10 min, under agitation, for 30 days.
property of the resin matrix.10,11
Additionally to the effect on composites color, the Color measurement (DE)
composition of the food and beverage may degrade the
surface of the restorative materials and affect the organic Prior to surface treatments, baseline color of each spec-
phase of the resin matrix, promoting the disintegration of imen was assessed under standardized ambient conditions
the disperse phase and altering the surface hardness of according to the CIE L*a*b* system, using a spectropho-
composite resin.12e14 Furthermore, the hygiene habits, e.g. tometer (CM2600d, Konica Minolta, Osaka, Japan) and an
toothbrushing, also influence on the material’s longevity. integrating sphere. The device was adjusted to use the D65
Abrasion may result in alterations in the material surface standard light source with 100% UV included or 100% UV
affecting in the contour, coloration and favoring the plaque excluded and specular reflection included (SCI). The
retention due to the surface roughness.15 observer angle was set at 2
and the device was adjusted to
The literature affirm that the mechanical properties of a small reading area. The color of each specimen was
the current fluoride composites are similar to those of the measured three times and averaged. The results of the
Properties of composites under staining and brushing 89

color measurements were quantified in terms of three co- Statistica for Windows (version 9.1, StatSoft Inc., Tulsa, OK,
ordinate values (L*, a*, b*) as established by the Commis- USA) and Statistix 9 (version 9.1, Tallahassee, FL, USA).
sion Internationale de l’Eclariage (CIE), which locates the Statistical analysis was submitted to two-way analysis of
color of an object in a three-dimensional color space. From variance (ANOVA; composite resin and surface treatments)
the color measurement at baseline and those after the and Tukey tests, with a significance level set at 5% (p < 0.05).
surface treatment, the values of the changes of L* (DL), a*
(Da), and b* (Db) were calculated. The total change in color
Results
or the variation in perception of color of each specimen was
calculated, designated by the abbreviation DE*ab. This
parameter was calculated according to the following for- Color measurement (DE)
mula: DE*ab Z (DL2 þ Da2 þ Db2)1/2.
According to ANOVA, the treatment (F Z 72.98;
Knoop microhardness analysis (KHN) p Z 0.0001), composite resin (F Z 49.98; p Z 0.0001), and
the interaction (F Z 2.92; p Z 0.0016) were statistically
significant. Table 2 displays the mean values of the color
The microhardness measurement was performed with a
change (DE) for the composite resin factor for each treat-
microhardness tester (FM-700, Future-Tech, Tokyo, Japan),
ment. It is observed that the greatest mean values were
Knoop tip, under 50 g load for 15 s. Three indentations were
presented by Beautifil resin group, which differed signifi-
performed 100, 200 and 300 mm apart from each other, on
cantly from the Filtek group. For the Beautifil group, the
the surface of the specimens. The means were determined
treatments differed significantly from each other. For the
as Knoop Hardness Number (KHN).
Filtek group, the control group presented significant dif-
ferences in relation to the treatment groups (Colgate and
Surface treatments: staining in coffee solution and
Oral B). Regarding surface treatments, all groups (Control,
brushing simulation Colgate, and Oral B) exhibited significant differences be-
tween the studied composite resins (Filtek and Beautifil II).
In each daily cycle, the samples were first immersed in 2 ml
of coffee solution, at 37
C for 10 min, under constant
Knoop microhardness (KHN)
agitation. The coffee solution was prepared with 1 tsp. of
soluble coffee (Nescafé Original, Nestlé, Araras, São Paulo,
Brazil) dissolved in 50 ml of boiling water. Subsequently, ANOVA showed statistically significant differences for treat-
the specimens were subjected to brushing abrasion in an ment (F Z 21.76; p Z 0.0001), composite resin (F Z 38.96;
automatic toothbrushing (TB) machine (ODEME Biotech- p Z 0.0001), and interaction (F Z 6.96; p Z 0.0016). Table 3
nology, Joaçaba, SC, Brazil), which imparted reciprocating presents the mean values of the Knoop microhardness (KHN)
motion to 6 soft bristle toothbrush heads (Sanifill Ultra- for the factor composite resin in each treatment. The com-
profissional, Hypermarcas, São Paulo, SP, Brazil). This posite resin Filtek exhibited the greatest mean value, sta-
apparatus provides linear brushing movements across the tistically different from that of the resin Beautifil. In relation
specimens at a speed of 120 cycles per min at 37
C, with a to surface treatments, the control group and the Oral B
double pass of the brush head over the surface, simulating 3 group statistically differ between the studied composite
brushings of 40 cycles per day, which corresponds to 3 daily resins, while the group Colgate did not statistically differ. It
brushings in oral cavity for one month.17 The abrasive slurry could be observed that the composite resin containing fluo-
consisted of toothpaste and artificial saliva, in a ratio of ride Beautifil II and the composite resin fluoride-free Filtek
1:3, by weight. The toothpastes used in this study are reduced the microhardness values after the treatment with
specified in Table 1. After brushing, the specimens were the dentifrices compared with the control groups. However,
kept in deionized water at 37
C. At the end of this proto- in spite of this reduction, the microhardness values pre-
col, the specimens were rinsed with deionized water and sented by the Filtek composite resin were higher than those
microhardness and color measurement were performed. of the Beautifil II composite resin.

Statistical analysis Discussion

Data analysis was carried out using the software program This study evaluated the effect of the immersion into
Minitab for Windows (version 16.1, College State, PA, USA), coffee solution associated to simulated toothbrushing on

Table 1 Toothpastes used.

Toothpaste Compositions
Colgate Total 12 (Colgate-Palmolive Ind.Ltda) Sodium fluoride (1100 ppm fluoride), water, hydrated sı́lica,
pentasodium triphosphate, PEG-12, tetrapotassium pyrophosphate,
sodium lauryl sulphate, polyethylene, cocamidopropyl betaine,
sodium saccharin, sodium hydroxide, titanium dioxide.
Oral-B 3D White (Procter&Gamble GmbH) Sodium fluoride (1450 ppm fluoride), water, hydrated sı́lica, sorbitol,
sodium lauryl sulphate, sodium hydroxide, sodium saccharin
90 T. Mara da Silva et al

Table 2 Mean values  standard deviation of DE and the results of Tukey tests (5%).
Composite resin Treatments
Control Colgate Oral B
Filtek Z350 XT 1.73  1.19 Ab 7.00  2.15 Aa 7.27  2.55 Aa
Beautifil II 4.50  2.96 Ba 9.29  2.33 Bb 12.11  1.56 Bc
Different letters show statistically significant differences (p < 0.05): uppercase letters refer to columns; lowercase letters refer to lines.

Table 3 Mean  standard deviation of KHN values and the results of Tukey tests (5%).
Composite resin Treatments
Control Colgate Oral B
Filtek Z350 XT 27.16  10.85 Ab 8.23  6.27 Aa 15.48  9.66 Aa
Beautifil II 11.21  5.17 Ba 6.25  5.08 Aa 4.35  4.69 Ba
Different letters show statistically significant differences (p < 0.05): uppercase letters refer to columns; lowercase letters refer to lines.

changing the color and surface microhardness of used. The rationale behind this color change could be the
nanoparticle-reinforced composite resins. The surface daily immersion into coffee solution, similarly to the
treatments significantly reduced the properties of the studies of Patel et al.22 and Ertas et al.,10 in which the
studied composite resins, showing differences in color coffee solution had the greatest DE values, mostly influ-
and superficial microhardness. Thus, the null hypothesis encing on the resin color.
was rejected. Also, the simulated toothbrushing could have favored
The samples not subjected to the surface treat- some changes in the composite resin surface. The in vitro
ments were immersed into artificial saliva, as a positive simulated toothbrushing is a parameter to evaluate the
control. According to this present study, the artificial saliva restorative material’s ability to maintain the smoothness,
slightly altered the color of the resin Filtek Z350 XT brightness, and to avoid staining.24 The greater the number
(DE Z 1.73  1.19), a result similar to that of previous of toothbrushing cycles and period, the highest is the
studies.1,18 However, when compared to the Beautifil II degradation of the composite resin with higher surface
samples, it was observed that artificial saliva had a signif- roughness and lower brightness.24 Similarly, in this present
icant color change (DE Z 4.50  2.96), since the DE value study, the simulated toothbrushing significantly altered the
equal or below to 3.3 is considered clinically acceptable in color of the evaluated composite resins. The increase of the
Dentistry.19,20 This color change could be related to the roughness due to the gradual removal of the filler particles,
long immersion period to which the samples were during the toothbrushing process, may account for this
immersed. According to Domingos et al.1 the immersion result,24,25 thus favoring the staining of the composite
into artificial saliva significantly influenced the color sta- surface. This effect in color change differs depending on
bility of composite resin after 30 days, but not at the initial the composite resin composition: particle size, resin matrix
period. Also, the artificial saliva components and the water composition, and conversion after polymerization.24 This
sorption by the resin matrix could result in plasticization, would explain the difference observed by this present
softening, and hydrolysis of the material, thus promoting study, in which the nanohybrid resin Beautifil II had the
greater susceptibility to color change.1 highest DE variation than the nanoparticulate resin Filtek
On the other hand, coffee was the substance used to Z350 XT, in agreement with other studies.26
stain the material because of its greater consumption by The abrasiveness of the dentifrices would have affect
the population and potential to stain both the tooth and the the surfaces of the studied composites. The greater the
composites.9 Furthermore, the coffee can significantly dentifrice abrasiveness, the greater is the surface rough-
alter certain resin properties at high temperatures.10,21,22 ness and the material’s weariness.17,27 This present study
Routinely, food and beverage have short contact with employed two dentifrices with different compositions. The
tooth and restorative material surfaces before either the nanoparticulate composite without fluoride did not show
saliva wash-out or toothbrushing. Notwithstanding, as far as statistically significant differences in color alteration after
we are concerned, this is the first study that immersed the the treatment with both toothpastes. However, the nano-
samples for a shorter period to mimic daily habits, that is, hybrid composite with fluoride exhibited a higher DE vari-
each sample was immersed into the coffee solution for ation after the treatment with dentifrice Oral-B than with
10 min per day, followed by simulated toothbrushing, and the dentifrice Colgate Total 12. Probably, the different
kept in distilled water to copy the neutralizing effect of the dentifrice compositions and the different composite resin
saliva, but without the saliva components.23 compositions explain this difference. The different meth-
The results of the color change showed significant dif- odologies regarding the dentifrice slurry, toothbrushing
ferences among the evaluated treatments and between the type, hardness and rigidity of the bristles, and number of
composites. Both composite resins increased the DE values the toothbrushing cycles25 make difficult to compare our
after the surface treatment, regardless of the toothpaste results with those of the literature.
Properties of composites under staining and brushing 91

The surface hardness is the mechanical property related Despite of the fluoride presence, the composite resin
to the material’s resistance to wear. Generally, the hard- Beautifill II showed unsatisfactory color and hardness
ness alterations of the composite resin occurred within the outcomes after daily food and hygiene habits compared
first seven days after the exposure to chemical solutions.28 with the composite resin Filtek 350 XT without fluoride.
In this study, the microhardness was evaluated just after Within the limitation of this study, the fluoride release and
the polymerization and after the surface treatments. In this uptake was not evaluated. Further studies are necessary
present study, both composites statistically decreased the to verify this property of fluoride release and uptake
microhardness after the immersion into artificial saliva claimed by the manufacturer, as well as the effects of this
without simulated toothbrushing. The chemical degrada- restorative material with fluoride in patients with high
tion on the composite surfaces related to the resin matrix caries prevalence.
would explain the differences in the microhardness Based on the results of this study, it can be concluded
values.29 Still, the hydrolytic instability of the organic ma- that the fluoride-containing composite resin presented
trix, considered the most fragile point of the composites, higher color changes and microhardness reduction than the
could have accounted for the changes due to the high non-fluoride composite resin; after daily treatments with
sensitivity of the material to water absorption.23 immersion in coffee solution associated with brushing cy-
We found differences in the microhardness between the cles. Thus, demonstrating that composition is an important
two composites after immersion into artificial saliva, related factor in the clinical performance of esthetic restorative
to the composition and content of the particles. Despite of materials.
the similar matrix compositions, the size and amount of the
filler particles are different. The resin Filtek Z350 XT has
Conflicts of interest
nanoparticles of approximately 0.6 mm and smaller filler
content (78.5%) than the resin Beautifil II (nanohybrid par-
None.
ticles of 0.8 mm and 83% of filler content). Probably, the
smaller filler content of the resin Filtek Z350 XT favored the
significant wear of the surface hardness after the immersion Acknowledgements
in artificial saliva for 30 consecutive days. However, the KHN
values of the resin Filtek Z350 XT were higher than those of The authors would like to thank CNPq/PIBIC/UNESP for the
the tested composite resin containing fluoride. financial support and Prof. Dr. Ivan Balducci for his assis-
After the surface treatments, the resin Beautifil II tance in statistical analysis.
exhibited KHN values smaller than that of resin Filtek Z350
XT, at all time periods. Beautifil II is composed by S-PRG
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