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Journal of the Mechanical Behavior of Biomedical Materials 97 (2019) 7–12

Contents lists available at ScienceDirect

Journal of the Mechanical Behavior of


Biomedical Materials
journal homepage: www.elsevier.com/locate/jmbbm

Effects of dentifrices on mechanical resistance of dentin and restorative T


materials after erosion and abrasion
Diego Felipe Mardegan Gonçalvesa, André Luiz Fraga Brisoa, Nubia Inocencya Pavesi Pinib,
Mariana Dias Modaa, Renata Parpinelli de Oliveiraa, Paulo Henrique dos Santosc,
Ticiane Cestari Fagundesa,∗
a
Department of Restorative Dentistry, São Paulo State University (Unesp), School of Dentistry, Araçatuba. R. José Bonifácio 1193, CEP, 16015-050, Araçatuba/SP, Brazil
b
Department of Restorative Dentistry and Prosthodontics, Ingá University Center - UNINGÁ, 317 PR Road, Maringá/PR, Brazil
c
Department of Dental Materials and Prosthodontics, São Paulo State University (Unesp), School of Dentistry, Araçatuba. R. José Bonifácio 1193, CEP, 16015-050,
Araçatuba/SP, Brazil

ARTICLE INFO ABSTRACT

Keywords: The aim of this study was to evaluate the mechanical resistance of dentin and restorative materials submitted to
Abrasion. erosion. composite resin. resin- erosive/abrasive challenges with different dentifrices. The dentin was restored using a resin-modified glass-
modified glass-ionomer ionomer (RMGIC) or a composite resin (RC). One hemiface of the sample was protected, and the other was
subdivided according to the applied dentifrice (n = 10): without fluoride (SF), sodium fluoride (NaF) and
stannous fluoride (SnF). The specimens were submitted to erosive/abrasive cycles, the varnish was removed, and
the Martens hardness (HMV) and elastic modulus (Eit) were evaluated. The data were analyzed by repeated two-
way ANOVA measurements and Tukey tests (alpha = 0.05). When analyzing the HMV on the test side, there was
no influence of the dentifrices in the dentin; however, the orders of NaF < SnF = SF in RC and SnF > NaF =
SF in RMGIC were observed. Comparing the treated surfaces, there were no differences in the dentin, and only
the SF since CR presented an HMV superior to that of RMGIC. Comparing control and test sides, both dentins
obtained a decreased HMV after the erosive/abrasive challenge; for the restorative materials, superior values
were found only for SnF in the RMGIC. The Eit values were influenced more by the dentifrices on the test side for
the dentin adjacent to the RMGIC, with the lowest values shown for the SF, and for both materials, the highest
values were shown for the SnF group. No differences were found when comparing each dentin treated with the
same dentifrice; however, the RMGIC presented a superior Eit than the CR when brushed with both dentifrices
with a fluoride. Comparing the control and test sides, the same results were obtained for the HMV. The denti-
frices showed little influence on the dentin substrate, whereas the dentifrice with SnF enhanced the mechanical
properties of the restorative materials, which was more evident in the RMGIC.

1. Introduction reducing its resistance and making it more susceptible to mechanical


stresses, such as attrition or abrasion (West and Joiner, 2014). Dentin is
Erosive dental wear is a multifactorial condition that results in a tissue that is less mineralized with a higher organic content (type I
chemical dissolution of mineralized tissues, loss of enamel and dentin collagen and non-collagenous compounds), lower hardness, and elastic
thickness, and structural changes in the remaining tissues (Lussi and properties than dental enamel (Lussi et al., 2011). In addition, dentin
Carvalho, 2014). Dental erosion occurs from acids of extrinsic (ex- presents peritubular and intertubular dentins, which after challenge
cessive consumption of acidic substances, citrus juices, and soft drinks) acids form a disorganized surface layer (Amaechi and Higham, 2005).
or intrinsic (gastroesophageal disorders) origin (Huysmans et al., The high prevalence of erosive dental wear has resulted in increased
2011). research to improve the treatment and prevention of disease (Lussi and
In dental enamel, wear occurs from demineralization and pro- Carvalho, 2014). Etiologic factors should be removed or controlled to
gressive softening caused by acid on the surface of the dental tissue, reduce the effects of acid on the dental tissue (Amaechi and Higham,


Corresponding author. Department of Restorative Dentistry, São Paulo State University (Unesp), School of Dentistry, Araçatuba. R. José Bonifácio 1193, CEP,
16015-050, Araçatuba-SP, Brazil.
E-mail addresses: ticiane.fagundes@unesp.br, ticiane_f@hotmail.com (T.C. Fagundes).

https://doi.org/10.1016/j.jmbbm.2019.05.006
Received 30 January 2019; Received in revised form 30 April 2019; Accepted 3 May 2019
Available online 04 May 2019
1751-6161/ © 2019 Published by Elsevier Ltd.
D.F.M. Gonçalves, et al. Journal of the Mechanical Behavior of Biomedical Materials 97 (2019) 7–12

2005). Some protective therapies using dentifrices, rinsing solutions,


and varnishes have been proposed to increase tissue resistance to acid

Trybol AG, Neuhausen AM Rheinfall,


dissolution (Young et al., 2006; Ganss et al., 2009).

Colgate-Palmolive, São Bernardo do


Conventional formulations with sodium fluoride in their composi-

GC Corporation, Tókio, Japan.


tion form precipitates on the organic layer of demineralized dentin;
however, this layer is unstable and does not provide protection after
new challenges (Huysmans et al., 2014). In this context, dentifrices

P&G, Cincinnati, USA.


St. Paul, MN, USA.
with stannous ions associated with fluoride have presented a better

Campo, SP, Brazil.


anti-erosion effect (Young et al., 2006; Hooper et al., 2007; Faller et al.,

Manufacturer
2011). The deposition of stannous ions in the eroded tissue form a

3M ESPE
protective barrier that remains in position for up to 4 h, preventing

Swiss.
contact with the acids. Furthermore, such composition can reduce the
susceptibility of dental tissues to mineral loss by 80% (Hooper et al.,
2007).

Phosphate, Sodium Lauryl Sulfate, Sodium Lauryl Sulfate, Carrageenan, Sodium Saccharin, Xanthan Gum, Blue 1
Water, Sorbitol, Hydrated Silica, Glycerin, Steareth-20, Titanium Dioxide (Cl 77891), Aroma, Sodium Phosphate,

Glycerin, Hydrated Silica, Sodium Hexametaphosphate, Propylene Glycol, PEG 6, Water, Zinc Lactate, Trisodium
In this context, abrasive components are added to the dentifrices to

Water, Triclosan, Sorbitol, Silica, Sodium Lauryl Sulfate, PMV/ MA Copolymer, Sodium Hydroxide, Saccharin
improve their cleaning and polishing potential, and the concentration is

Powder: fluor-amino-silicate glass. Liquid: aqueous solution of polycarboxylic acid, TEGDMA and HEMA
varied according to the therapeutic purpose. These values have been set

Carrageenan, Sodium Chloride, Citric Acid, Sodium Benzoate, Potassium Thiocyanate, Glucose Oxidase,
Bis-GMA, UDMA, Bis-EMA, TEGDMA, PEGDMA, Zirconia and agglomerates of silica, camphorquinone
by the American Dental Association (ADA) according to the relative
dentin abrasivity (RDA) or relative enamel abrasivity (REA). In erosive
dental wear, there is no consensus regarding the influence of the
abrasiveness of the dentifrices in terms of a protective effect on the
erosion/abrasion (Hughes et al., 2008; Aykut-Yetkiner et al., 2014).
After a loss of tissue thickness in the cervical region, composite
resins and glass ionomer cement should be used to replace the lost
tissue and prevent the occurrence of larger lesions (Colon and Lussi,
2014). It has been observed that composite resin shows less loss of
surface material after an erosive challenge, and RMGIC demonstrates a
reduced acid degradation and protected dental surfaces adjacent to the
erosion (Alghilan et al., 2015). However, few studies have evaluated
the effect of different dentifrices in the prevention of the erosion/
abrasion of composite resin and glass ionomer cement restorations,
mainly analyzing superficial mechanical properties, such as Martens
hardness and modulus of elasticity, since the majority of studies have
evaluated the profilometry (Ganss et al., 2011; Schlueter et al., 2011;

Stannous fluoride (1100 ppm F as SnF2)


Alghilan et al., 2015).
Amyloglucosidase, Lactoperoxidase .
Sodium Fluoride (1450 ppm as NaF)

Therefore, the objective of the present study was to investigate the


protective capacity of dentifrices on the mechanical resistance of dentin
and restorative materials after erosion and abrasion. Three null hy-
Sodium, Titanium Dioxide

potheses were proposed: (1) there is no difference among the dentifrices


applied for dentin and restorative materials after erosion and abrasion
cycles, (2) there are no differences among the analyzed surfaces when a
Composition

single type of dentifrice is evaluated after the erosion and abrasion


cycles, and (3) there is no difference between both sides (control and
test) for the dentin and restorative materials.

2. Materials and methods


RMGIC
Code

NaF

SnF
CR

SF

2.1. Study design


Stannous Fluoride Toothpaste
Resin-modified glass-ionomer

Sodium Fluoride Toothpaste

A total of 120 dentin bovine blocks; two restorative materials,


Fluoride-free Toothpaste

namely, a composite resin (CR) and resin-modified glass ionomer ce-


ment (RMGIC); three dentifrices, namely, without a fluoride group with
Composite Resin

low abrasivity (SF), sodium fluoride with medium abrasivity (NaF), and
stannous fluoride with high abrasivity (SnF); and control and test sides
were employed in this in vitro study. Erosive/abrasive cycles were ap-
cement
Type

plied. The Martens hardness (HMV) and elastic modulus (Eit) were used
to evaluate the mechanical properties of dentin and the restorative
material surfaces. The materials used are described in Table 1.
Colgate Total 12 (RDA-70/80)
Materials used in this study.

Curaprox Enzycal Zero (RDA-

Crest Pro-Health (RDA-155)


Filtek Z350 XT (color A2B)

2.2. Specimen preparation


Fuji II LC (color A3)

Bovine teeth were obtained and stored in a 0.1% thymol solution for
30 days (#00453–2017 ethical protocol). Dentin blocks (4 × 4 mm2)
were obtained from the cervical dentin using diamond discs (Isomet
Material

30)
Table 1

1000, Buehler, Illinois, USA). The samples were polished with sand-
paper (#600, #1200, #2000) under constant irrigation. The specimens

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D.F.M. Gonçalves, et al. Journal of the Mechanical Behavior of Biomedical Materials 97 (2019) 7–12

Fig. 1. Experimental design. (a) The specimens obtained


(4 × 4 mm2) were submitted to initial microhardness
analyses for selection (b). Both specimens were included
in an acrylic base with a 1-mm distance between them
(c). A cavity was prepared on the walls of the specimens,
with a total distance of 2 mm between them (d). The re-
storation was applied, (e) the restorations were polished
(f) and the hemiface of each specimen/restoration set was
covered with an acid-resistant varnish (g). The samples
were submitted to erosive/abrasive challenges (h).
Finally, the acid-resistant varnish was removed (i) and
the samples were subjected to the Martens hardness and
modulus of elasticity (j).

were then polished using a felt disc and 1-μm diamond paste (Arotec, adhesive interface: dentin underlying the restorative materials, RMGIC,
Cotia, SP, Brazil). These procedures allowed dentin blocks with a and CR on the control and test sides (Guedes et al., 2016). A flowchart
thickness of 1 mm to be obtained, which were controlled using a digital of the study is shown in Fig. 1.
caliper. The specimens were then exposed to Knoop microhardness
(Shimadzu Corporation, Kyoto, Japan) with a static load 50 g for 15 s 2.5. Statistical analyses
until standardization (Souza et al., 2015).
Two specimens were embedded in acrylic resin using a metal matrix Data were analyzed for normality using a Shapiro-Wilk test.
with a 1-mm distance. Wear was carried out between the blocks using a Repeated two-way ANOVA measurements and a Tukey's post-test were
diamond tip (#1090, KG Sorensen, Barueri, SP, Brazil) coupled in a used. The level of significance was 5%. The data were analyzed using
high-rotation, simulating cavity walls adhered to the restorative ma- SigmaPlot 12.0 software (Systat Software, San Jose, CA, USA).
terials. Thirty samples were restored using CR and photocured for 20 s
(Kavo, Joinville, SC, Brazil). Thirty other samples were restored using
3. Results
RMGIC, photocured for 40 s, protected with petroleum jelly, and kept
under humid conditions at 37 °C for 7 days. After storage, the samples
The HMV analyses (Table 2) showed differences only for dentin
were polished as previously described for excess removal. A hemiface of
adjacent to the RMGIC on the control side (p < 0.05); however, there
each specimen was protected using an acid-resistant varnish (Colorama,
were no differences between the dentifrices applied to the adjacent
São Paulo, SP, Brazil) to create the control and test sides.
dentin to the restorative materials on the test side. Lower values for the
NaF as compared to the SF and SnF were found in the CR (p < 0.05);
2.3. Erosion/abrasion cycling however, the SnF showed higher values than the NaF and SF
(p < 0.05). Comparing the treated surfaces, there were no differences
The specimens of each type of material tested were divided into between the dentins (p > 0.05), and only SF CR presented a superior
three groups according to the dentifrices (n = 10): SF, NaF, and SnF. HMV than the RMGIC (p < 0.05). The HMV of the dentin on both the
The sample size was determined from a previous pilot study using the control and test sides decreased after the challenge; for the restorative
minimum difference between the means and the mean of the standard materials, superior values were found only for the SnF in the RMGIC
deviations, with a test power of at least 80% and a significance level of (p < 0.05).
5%. During the experiment period, specimens were subjected to a 5-day Regarding the Eit data (Table 3), a statistical difference was de-
erosive/abrasive cycling regimen. Erosive cycles were performed four monstrated only for DRMGIC in the NaF group for the control side
times daily, and abrasive challenges were applied after the first and last (p > 0.05). On the test side, the Eit values were influenced by denti-
cycles. frices in the dentin adjacent to the RMGIC, with the lowest values
The samples were eroded by immersion in 250 ml of citric acid shown for SF (p < 0.05). The SnF group presented the highest values
(pH = 3.2) for 2 min under an orbital shaking table (Tecnal TE – 420, for both materials (p < 0.05). No differences were found when com-
Piracicaba, SP, Brazil) (Cruz et al., 2015). The dentifrices were diluted paring the dentin treated with the same dentifrice; however, the RMGIC
in distilled water (1:3), and 2 ml of this solution was pipetted on the presented a superior Eit than the CR when brushed with both denti-
samples after the first and last cycles. The abrasive challenge was ap- frices with fluoride (p < 0.05). Comparing the control and test sides,
plied with an electric brush (Oral-B Plak Control Ultra; Braun, Frank- the same results as those obtained for HMV were found.
furt, Germany) with a weight of 200 g for 15 s, and immersed in the
slurry for 2 min (Pini et al., 2016). After the daily challenges, the 4. Discussion
samples were stored in artificial saliva at 37 °C for 1 h until the next
cycle (Pini et al., 2016). At the end of experiment period, the acid- HMV analyses were conducted to measure the mechanical proper-
resistant layer was removed and the samples were stored under 100% ties and the simultaneous plastic and elastic deformations of the dentin
humidity until analysis. and restorative materials through indentations applied under low loads
(Schlueter et al., 2011; Alghilan et al., 2015; Suzuki et al., 2015). These
2.4. Surface analyses analyses allow an evaluation of not only the mechanical behavior of
dentin and the restorative materials, but also the changes in resistance
The response variables (HMV and Eit) were measured using a dy- values of different areas, in other words, if one “reference area” remains
namic ultra microhardness tester (DUH-211S; Shimadzu, Kyoto, Japan) unchanged. In the present study, the sound untreated dentin or re-
under a load of 50 mN for 5 s (Mahoney et al., 2003). Three indenta- storative material served as the “intra-specimen” reference area used to
tions were applied using a Vickers indenter in each region of the analyze the change in resistance of the treated areas after erosion/

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D.F.M. Gonçalves, et al. Journal of the Mechanical Behavior of Biomedical Materials 97 (2019) 7–12

Table 2
Mean and standard deviation of HMV (GPa) according to each dentifrice, substrate and restorative material.
Dentifrice Control

DCR DRMGIC CR RMGIC

SF 1.57 ± 0.05 Aa 1.28 ± 0.02 Cb 1.69 ± 0.05 Aa 1.47 ± 0.11 Aa


NaF 1.66 ± 0.07 Aa 1.68 ± 0.14 Aa 1.49 ± 0.06 Aa 1.59 ± 0.16 Aa
SnF 1.58 ± 0.04 Aa 1.48 ± 0.07 Ba 1.79 ± 0.04 Aa 1.78 ± 0.05 Aa

Dentifrice Test
DCR DRMGIC CR RMGIC

SF 0.55 ± 0.02 Aa* 0.58 ± 0.01 Aa* 1.84 ± 0.05 Aa 1.42 ± 0.06 Bb
NaF 0.53 ± 0.02 Aa* 0.74 ± 0.04 Aa* 1.59 ± 0.14 Ba 1.64 ± 0.10 Ba
SnF 0.49 ± 0.04 Aa* 0.62 ± 0.03 Aa* 1.98 ± 0.04 Aa 2.22 ± 0.07 Aa*

SF (Without Fluoride)/ NaF (Sodium Fluoride)/ SnF (Stannous Fluoride)/ DCR (Dentin adjacent Composite Resin)/ DRMGIC (Dentin adjacent Resin-Modified Glass-
Ionomer).
Upper case letters compare toothpastes. Lowercase letters compare surfaces alone between dentin and restorative materials. * Compare differences between control
side and test.

abrasion cycling. Therefore, sound untreated dentin and restorative demineralization and remineralization around the restorations depend
materials needed to be protected during the erosion/abrasion cycling. on the restorative material used, and this effect was not observed on the
Care was taken to apply and remove the “protective” nail varnish. substrate adjacent to the CR (Zan et al., 2018). Furthermore, a residual
The first null hypothesis was partly rejected because there was an effect from the presence of fluoride may occur in the dentin-adjacent
influence of the dentifrices in dentin adjacent to the RMGIC and re- RMGIC on the control side because the analyses were conducted after
storative materials. For dentin, the effect of the dentifrice with fluoride the challenge cycles. It is thought that the acid penetrated the dentinal
was more evident when the dentin adjacent to the RMGIC was brushed tubules and acted at a distance, changing the hardness on the control
with NaF. This effect was observed in the same manner for the HMV of side because the HMV was evaluated relatively close to the border re-
the control side. The protective effect of sodium fluoride on dental gion of the control and test sides. For the other conditions evaluated, no
erosion is related to the formation of a physical barrier with minerals differences were shown between the dentifrices in the dentin substrates,
similar to CaF2, which can be dissolved through an acidic challenge corroborating with a previous study (Schlueter et al., 2007) that also
before the underlying tissue is affected (Ganss et al., 2001; Diamanti did not find an anti-erosive action for NaF with the formulations ma-
et al., 2016). In this study, the superiority of the NaF group on the nipulated in the laboratory under pH conditions similar to those of the
dentin adjacent to the RMGIC may have occurred owing to a confine- present study (Huysmans et al., 2014). Moreover, the dentin on the test
ment of F ions in the monomeric matrix of the ionomeric material, al- side may have been similar in all groups owing to its loss on the surface
lowing an effect on the surface mechanical properties. Furthermore, the after an erosive/abrasive challenge (Ganss et al., 2011; Schlueter et al.,
RMGIC is able to recharge using F ions that bind poorly in the matrix 2011; Alghilan et al., 2015).
and release slowly, as well as protect the adjacent dental structure Regarding the restorative materials, the SnF group in contact with
submitted to erosive challenges (Freedman and Diefenderfer, 2003; the restorative materials presented the highest mechanical properties,
Mousavinasab and Meyers, 2009; Selimović-Dragaš et al., 2013; being more evident its effect on the RMGIC. It is assumed that stannous
Alghilan et al., 2015). The NaF contains approximately 10%–20% created a protective film on the restorative materials, as demonstrated
abrasive silica particles (medium abrasivity), which may reduce the loss in the dental substrates (Hooper et al., 2010). In addition, another study
of the substrate and increase the mechanical properties, presenting observed that enamel specimens brushed with the dentifrices con-
superior results when compared to the SnF (high abrasivity) (Ganss taining stannous/amine fluorides revealed significant mineral gains and
et al., 2017). However, dentifrice formulations with polyvalent fluoride lesion depth reductions in pre-demineralized enamel (Kielbassa et al.,
sources, such as a stannous association, have been shown to be pro- 2009). It has been speculated that negative zeta-potential abrasive silica
mising for a dental erosion (Lussi and Carvalho, 2015). Dentin particles have bound to the positive stannous and formed a precipitate

Table 3
Mean and standard deviation of Eit (GPa) according to each dentifrice, substrate and restorative material.
Dentifrice Control

DCR DRMGIC CR RMGIC

SF 30.03 ± 1.57 Aa 24.78 ± 2.84 Ba 27.16 ± 2.45 Aa 27.75 ± 2.36 Aa


NaF 31.80 ± 1.29 Aa 32.31 ± 2.15 Aa 25.31 ± 1.17 Aa 32.79 ± 1.38 Aa
SnF 31.32 ± 1.33 Aa 28.10 ± 2.79 ABa 28.45 ± 1.80 Aa 34.41 ± 0.78 Aa

Dentifrice Test
DCR DRMGIC CR RMGIC

SF 15.52 ± 0.72 Aa* 15.72 ± 0.52 Ba* 28.44 ± 0.92 ABa 25.36 ± 1.85 Ca
NaF 15.42 ± 0.54 Aa* 20.50 ± 1.81 Aa* 23.22 ± 0.97 Bb 34.56 ± 2.03 Ba
SnF 15.03 ± 0.80 Aa* 17.44 ± 0.79 ABa* 30.45 ± 0.46 Ab 44.79 ± 0.95 Aa*

SF (Without Fluoride)/ NaF (Sodium Fluoride)/ SnF (Stannous Fluoride)/ DCR (Dentin adjacent Composite Resin)/ DRMGIC (Dentin adjacent Resin-Modified Glass-
Ionomer).
Upper case letters compare toothpastes. Lowercase letters compare surfaces alone between dentin and restorative materials. * Compare differences between control
side and test.

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D.F.M. Gonçalves, et al. Journal of the Mechanical Behavior of Biomedical Materials 97 (2019) 7–12

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Declarations of interest experimental chitosan-containing solutions as anti-erosive agents in enamel. Caries
Res. 50, 337–345. https://doi.org/10.1159/000445758.
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This study was financially supported by the FAPESP—São Paulo Schlueter, N., Hara, A., Shellis, R.P., Ganss, C., 2011. Methods for the measurement and
characterization of erosion in enamel and dentine. Caries Res. 45, 13–23. https://doi.
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