Received: 30 November 2018 Revised: 2 February 2019 Accepted: 27 February 2019

DOI: 10.1111/jerd.12471

RESEARCH ARTICLE

Resistance of resin-infiltrated enamel to surface changes

in response to acidic challenge
Enas T. Enan1 | Neven S. Aref1,2 | Shaza M. Hammad3

1
Department of Dental Biomaterials, Faculty
of Dentistry, Mansoura University,
Mansoura, Egypt
2
Department of Basic Oral and Medical
Sciences, Faculty of Dentistry, Qassim
University, Kingdom of Saudia Arabia
3
Department of Orthodontics, Faculty of
Dentistry, Mansoura University, Mansoura,
Egypt
Correspondence
Neven S. Aref, Department of Dental
Biomaterials, Faculty of Dentistry, Mansoura
University, 35516 El Gomhoria St.,
Mansoura, Egypt.
Email: flflaref@gmail.com
Abstract
Objective: To investigate the ability of resin infiltration to protect demineralized enamel against
acidic challenge.
Materials and methods: Forty-five extracted healthy premolars were selected for the study,
each of which was sectioned vertically into 2 halves, giving 90 specimens. Specimens were then
divided into three groups, where specimens of group A were not decalcified (control), while
those of groups B and C were either subjected to decalcification only, or decalcification
followed by Icon resin infiltration, respectively. Each group was further divided into three sub-
groups, according to the type of storage medium (water, Coca-Cola, or Redbull). Evaluation
parameters included color difference and surface roughness. Scanning electron microscope was
used to evaluate enamel surface topography. Statistical analysis was performed by ANOVA
followed by least significant difference test.
Results: Although Coca-Cola caused the highest color change and surface roughness among the
studied specimens, yet, the resin-infiltrated enamel was more resistant to surface changes than
the nonresin infiltrated enamel, even under acid attack.
Conclusion: Resin infiltration has the ability to provide and maintain protection to the demineralized
enamel against acidic attack.

Clinical significance
Resin infiltration may be considered as a promising solution to restore esthetic of demineralized
enamel following orthodontic treatment and to protect it against acidic beverages.

KEYWORDS

acidic beverages, resin infiltration, white spot lesions

1 | I N T RO D UC T I O N masking of demineralized enamel lesions.5–7 This technique utilizes a

Enamel demineralization, or white spot lesion (WSL) is a common
problem related to fixed orthodontic appliances, due to inability of
patients to maintain adequate oral hygiene measures, which subse-
quently results in plaque accumulation.1–3 WSLs appear when the
enamel becomes invaded by pathogenic bacteria which produce
organic acids, with subsequent leaching out of calcium and phosphate
ions, which leaves porosities on the enamel surface and affects its
refractive index.4
Previously, different strategies were tried for correction of WSLs,
such as, restorative treatment, application of calcium-phosphate or
fluoride containing products, microabrasion, and argon-laser irradia-
tion. More recently, “resin infiltration technique” was introduced for
light-curing low-viscosity resin (ICON), composed of triethylene glycol
dimethacrylate (TEGDMA), which actively arrests progression of den-
tal caries by capillary infiltration of the low-viscosity resin to block
pores on the surface of demineralized enamel.8,9
As shown by several researches,10–14 the applied resin was effec-
tive in masking the WSLs, due to the close similarity of its refractive
index to that of enamel. However, a question remaining is whether
resin-treated enamel has the ability to provide long-term protection
against different forms of changes which are commonly encountered
in the oral cavity, such as pH changes?
The long-term stability of restorative materials is usually related
to its resistance to degradation under cyclic changes caused by chemi-
cal and physical factors in the oral cavity.15,16 Thus, for evaluation of

J Esthet Restor Dent. 2019;1–6. wileyonlinelibrary.com/journal/jerd © 2019 Wiley Periodicals, Inc. 1

2 ENAN ET AL.
any restorative material, the conditions of the oral environment should
be simulated, especially with regard to alterations in the pH.16–18
The pH value of dental biofilm may not only affect enamel sur-
face, but also influence the chemical and physical characteristics of
restorative materials.15–20 The influence of pH variation on the sur-
face characteristics of resin infiltrated enamel is not well established.
Therefore the current study aimed to investigate the in vitro ability of
resin infiltration technique to protect demineralized enamel surface
against acidic pH. Surface topography and color of resin infiltrated
enamel were evaluated after exposure to two different acidic bever-
ages. The null hypothesis tested was that resin infiltration would not
have a significant resistance against surface degradation in response
to pH changes.
2 | MATERIALS AND METHODS
2.1 | Specimens' preparation and grouping
A total of 45 healthy upper and lower premolars (obtained from the
out-patients' clinic of Faculty of Dentistry, Mansoura University,
Egypt, which were extracted for orthodontic treatment, ethics com-
mittee approval no. 15080518) were selected for the current study. In
a later stage, each tooth crown was divided into 2 halves, giving a
total number of 90 specimens.
The collected teeth were randomly divided into one control
(A) and two test (B and C) groups (30 specimens each). Specimens of
group A were not decalcified, while those of groups B and C were
either subjected to decalcification only, or decalcification followed by
ICON resin infiltration, respectively.
Then each of the three groups was subdivided, according to the
type of storage medium, into three subgroups (10 specimens each),
where subgroup 1 was immersed in water (baseline), while subgroups
2 and 3 were immersed in Coca Cola and Redbull, respectively.
2.2 | Decalcification
WSLs were artificially created on specimens of group B and C using
an acidic solution as described by Subramaniam et al.21
Teeth were put in decalcification solution (50 mM acetic acid
solution, 3 mM CaCl2_H2O, 3 mM KH2PO4, 6 mM methyl hydroxyl
diphosphonate, pH 4.95, 37 C), and were kept for 160 hours, in order
22
to make decalcified enamel lesions on the exposed enamel. After
enamel decalcification, roots of the decalcified teeth were cut away at
cemento-enamel junction and the crown portion of each tooth was
cut bucco-lingually into two halves, where one half was subjected to
resin infiltration (group C), while the other half was not (group B).
Specimens were embedded into acrylic blocks with the relatively flat
proximal surface facing outside.
2.3 | Application of resin infiltrant
Specimens of group C (n = 30) were cleaned with rubber cup and
pumice. Resin infiltrant (ICON VR, DMG, Hamburg, Germany) was
applied and cured after acid etching of the specimens according to the
manufacturer's instructions.
2.4 | Specimens' immersion
The specimens were immersed in their specified solutions (water,
Coca-Cola, or Redbull) for 5 minutes, 5 times a day for 30 days. Speci-
mens were kept in artificial saliva at during the intervals between
immersion cycles. The drinks were used in the temperature of con-
sumption which is about ±4 C.23
2.5 | Evaluation of color difference
Vita Easyshade spectrophotometer (Vita Zahnfabrik H. Rauter GmbH &
Co. KG, Bad Sackingen, Germany) was used for evaluation of the color
coordinates (L*a*b*) according to manufacturer's instructions.
Measured CIE L*, a*, and b* at each point were compared (to the
control group A1) and color difference (ΔE) was calculated as follows:
h
2
2
2 i
ΔE = ΔL* + Δa* + Δb* ½:
Where L* is the color value (lightness), a* and b* denote chroma-
ticity. ΔE value equal or larger than 3.5 was considered a clinically per-
ceptible color change.24
2.6 | Evaluation of surface roughness
Surface roughness (Ra) values were recorded for all the specimens
using a digital profilometer (Mitutoyo Surf Test SJ 210 Analyzer;
Mitutoyo Corp, Japan). To measure the roughness profile value, the
diamond stylus was moved across the specimen surface at a speed of
0.5 mm/s and a tracing length of 8 mm. This procedure was repeated
five times for each specimen and the average value was considered to
be the mean roughness parameter (Ra) value (μm).
2.7 | Scanning electron microscope
Randomly selected specimens were firstly sputtered with gold for bet-
ter image resolution, and then analyzed using (JEOL JSM-5200, Japan)
machine at a magnification of ×2000.
2.8 | Statistical analysis
Collected data were analyzed by statistical analysis software (SPSS 12.0,
SPSS, Chicago, Illinois). Repeated measure ANOVA and least significant
difference (LSD) test were carried out for color difference and Ra.
3 | RE SU LT S
3.1 | Color difference
Mean color difference values (ΔE) and standard deviations for all
groups are shown in Table 1. The results showed that group B2
(decalcified and immersed in Coca-Cola) had the highest mean ΔE
value (18.47) while group C1 (ICON baseline) showed the lowest
value (2.78). ANOVA test showed significant differences (P = 0.0001)
between ΔE values of the studied groups. LSD test between groups,
showed significant differences between Coca-Cola subgroups (A2, B2,
C2) in all the three studied groups. For the Redbull subgroups, no
ENAN ET AL. 3

TABLE 1 Color difference (ΔE) between control subgroup and other subgroups

Groups Mean SD F-value P-value LSD

B
A. Control A2: Coca-Cola 11.13 0.86 249.5 0.0001 0.98
A3: Redbull 3.2DE 0.82
B. Decalcified B1: baseline 3.9D 0.47
B2: Coca-Cola 18.47A 1.04
C
B3: Redbull 6.9 0.79
C. ICON C1: baseline 2.78E 0.37
C2: Coca-Cola 6.3C 0.86
C3: Redbull 3.4DE 0.65

Means with the same superscript letter are not significantly different at P ≤ 0.05.

significant difference was observed between the control group
(A3) and the ICON group (C3), while Group B3 (Decalcified) was sig-
nificantly different. Comparisons within groups showed significant
differences between Coca-Cola and Redbull, and also between
Coca-Cola and baseline.
3.2 | Surface roughness
Mean surface roughness (Ra) values (μm) and standard deviations for
all groups are shown in Table 2. The results indicated that group B2
(decalcified and immersed in Coca-Cola) had the highest mean
Ra value (1.46 μm) while group C1 (ICON baseline) showed the
lowest value (0.43 μm). ANOVA test showed significant differences
(P < 0.0001) between surface roughness values of the studied
groups. LSD test within groups, showed significant differences
between Coca-Cola (A2, B2, C2) and baseline A1, B1, C1) and also
between Coca-Cola and Redbull (A3, B3, C3) in the three groups.
3.3 | SEM
Scanning electron micrographs of selected groups are shown in
Figure 1. In Figure 1A, the characteristic fish scales appearance of
healthy enamel can be obviously seen on the surface of control speci-
men. In Figure 1B,C, decalcified specimens showed a sponge-like struc-
ture and enamel erosion, which was more extensive with Coca-Cola
(Figure 1B). SE micrographs of resin-infiltrated specimens (Figure 1D,E)
showed less surface irregularities, indicating more resistance to the ero-
sive attack by acidic beverages.
4 | DI SCU SSION
Resin infiltration has become a promising treatment option for incipi-
ent white lesions (WSLs) of enamel.9,10,25–29 However, concerns still
exist regarding its ability to resist degradation by different factors in
the oral cavity.30–32
Thus, the present study was conducted to estimate the ability
of ICON resin to provide and maintain surface protection for
demineralized enamel in presence of two different beverages of acidic
pH (Coca-Cola and Redbull). These beverages were selected because
they have a pH level that is below the critical limit for enamel demin-
eralization (5.5).33 Surface roughness and color change were specifi-
cally chosen for evaluation, due to their particular importance for
orthodontic patients, as these patients expect a long-lasting beautiful
smile at the end of the procedure. So, any discoloration or roughness
would not be acceptable for them.
In the current study, specimens with ICON resin infiltration
showed lower color change and surface roughness, than the non resin
infiltrated specimens, even on exposure to acidic beverages. It was
found that Coca-Cola caused higher discoloration and surface rough-
ness than Redbull, even in ICON-treated specimens. The discoloration
caused by Coca-Cola was clinically-detectable (ΔE ≥ 3.5) in all speci-
mens, while for Redbull the color change was below the clinically per-
ceptible threshold. These results can be explained in reference to the
more acidic nature of Coca-Cola (pH = 2.37), as compared to that of
Redbull (pH = 3.43). It may also be attributed to the fact that Coca-
Cola is darker than Redbull beverage.34 Ourcolor results came in
agreement with those of Bak et al.25 and Yetkiner et al.35 who proved
the ability of resin infiltrant to resist thermal and discoloration

TABLE 2 Mean and SD for surface roughness Ra (μm) of the studied groups

Groups Mean SD F-value P-value LSD

D
A. Control A1: Baseline 1 0.02 134.97 <0.0001 0.097
A2: Coca-Cola 1.34B 0.08
A3: Redbull 1.2C 0.04
B. Decalcified B1: Baseline 1.3BC 0.13
A
B2: Coca-Cola 1.46 0.09
B3: Redbull 1.31B 0.03
C. ICON C1: Baseline 0.43F 0.06
C2: Coca Cola 0.75E 0.1
F
C3: Redbull 0.45 0.08

Means with the same superscript letter are not significantly different at P ≤ 0.05.
4 ENAN ET AL.

FIGURE 1 SE micrographs (×2000 magnification) showing enamel surface of A, Control specimen. B, Decalcified specimen after immersion
in Coca-Cola. C, Decalcified specimen after immersion in Redbull. D, Decalcified and resin-infiltrated specimen after immersion in Coca-Cola.
E, Decalcified and resin-infiltrated specimen after immersion in Redbull

challenges. Regarding surface roughness, our results agreed with pre- to 24% of their orthodontic patients, had existing WSLs at the time of
vious studies36–40 which concluded that resin infiltration of enamel bracket fixation. Thus, preventive strategies; as ICON resin, may be
lesions can provide and maintain smoother surface. However, these needed during and after orthodontics especially if applied to the gingi-
41–43 val region or more preferably around all the brackets, to remineralize
results contrast those of other researches which reported that
surface roughness and color stability of resin-infiltrated enamel any demineralized enamel and to provide better satisfaction with
lesions were less than ideal and could further recede with aging in the orthodontic treatment.
oral environment. This disagreement may be a result of mismatching
in the experimental conditions and evaluation methods.
5 | C O N C LU S I O N A N D RE C O M M E N D A T I O N
The threshold level for plaque retention of the enamel roughness
is 200 nm. Plaque retention cannot be reduced below this value.44
Within the limitations of this study, it can be concluded that the resin
Patients usually regard surfaces to be rough when the Ra value is
infiltrant has the ability to provide and maintain protection to
more than 0.5 μm.45 Thus, according to the present study, it may
demineralized enamel in presence of acidic challenge. However, fur-
be assumed that patients would regard the infiltrated enamel surface
ther studies are needed to evaluate its resistance to the long-term
to be smooth and feel no discomfort, even if exposed to Redbull
effect of different influences encountered in the oral environment.
(Ra = 0.45 μm), while those consuming Coca-cola in large amounts
would feel the roughness and discomfort of resin-infiltrated enamel
(Ra = 0.75 μm). CONFLIC T OF INT E RE ST
WSLs can become noticeable around the orthodontic brackets The authors have no conflict of interest to report.
within 1 month of bracket placement. These lesions are commonly
seen on the buccal surfaces of teeth around the brackets, especially in
the gingival region.46,47 In recent decades, beverages consumption AUTHOR CONT RIB UTI ON S
has also steadily increased among children and adolescents in both The hypothesis was suggested EE. The experimental design was
Western and developing countries.1,10 Tufekci et al.48 found that 11% carried out by EE and NA under supervision of SH. Specimens'
ENAN ET AL.
preparation and all investigations were performed by NA. EE did the
data acquisition and interpretation. EE and NA contributed and per-
formed the statistical evaluation. EE wrote the manuscript and
SH critically revised it for important intellectual content. All authors
read and approved the final manuscript. NA submitted the manu-
script and SH modified the manuscript regarding the reviewers'
recommendations.
ORCID
Neven S. Aref https://orcid.org/0000-0002-5241-2838
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How to cite this article: Enan ET, Aref NS, Hammad SM.
Resistance of resin-infiltrated enamel to surface changes in
response to acidic challenge. J Esthet Restor Dent. 2019;1–6.
https://doi.org/10.1111/jerd.12471