Clin Oral Invest
DOI 10.1007/s00784-016-1850-z
ORIGINAL ARTICLE
Color stability of nanohybrid resin-based composites,
ormocers and compomers
Carmen Llena 1 & Sarai Fernández 1 & Leopoldo Forner 1
Received: 2 February 2016 / Accepted: 5 May 2016
# Springer-Verlag Berlin Heidelberg 2016
Abstract
Objective The aim of this study is to evaluate the color stabil-
ity of two nanohybrid resin-based composites, two organic
modified ceramic resin composites (ormocers) and a
compomer, following their immersion during 4 weeks in four
usual drinks.
Material and methods Forty discs of each of the following
materials were prepared: GrandioSO (GR), Esthet X (EX),
Dyract EXTRA (DY), Ceram X duo (CX), and Admira
Fusion (AD). The discs were polished and stored in distilled
water during 24 h at 37 °C. Color according to the CIEL*a*b*
scale was recoded. Ten randomly selected samples of each
material were immersed in red wine (RW), coffee (CF), cola
(CK), and distilled water (DW). The color was recorded after
1, 7, 21 and 28 days of immersion. The ΔE values between
the baseline color and each of the study timepoints were cal-
culated. The data were analyzed based on the Kruskal-Wallis
test, Wilcoxon test, and Mann-Whitney U test.
Results After 1 day of immersion, all the materials showed
ΔE > 3.3, except EX, CF, and CX in CK. RD was the most
staining beverage (ΔE 15.36 to 31.09). EX and CX were
significantly less stained than the rest of the materials
(p < 0.05).
Conclusions All the staining solutions produced darkening
beyond clinically acceptable limits. EX and CX were the ma-
terials who experimented less staining, followed by GD. AD
and DY were the materials more stained. RW was the drink
that produced more staining, followed by CF and CK.
* Carmen Llena
llena@uv.es
1
Department of Stomatology, Universitat de València, Gascó Oliag n°
1, 46010 Valencia, Spain
Clinical relevance After 24 h of immersion in all the solu-
tions, equivalent to 1 month of exposure in the mouth, the
evaluated materials showed clinically unacceptable ΔE
values.
Keywords Compomer . Composite resins . Ormocer . Color
stability
Introduction
Composite resins have evolved in recent years with the aim of
improving not only their physical and mechanical character-
istics but also their esthetic properties. In this regard, color
stability is one of the leading concerns, especially when re-
storing teeth in the anterior sector [1–5]. Such materials are
intended to reproduce the appearance of natural teeth—this
being related to the opacity or translucency of the material,
its opalescence or iridescence, and fluorescence.
Over time, other factors such as color stability, roughness,
and brightness prove decisive for the satisfactory outcome of
restorations [1, 4, 5], inadequate color being one of the most
common causes of restoration replacement, particularly in the
anterior sector [6].
Discoloration can be extrinsic or intrinsic. In this respect,
extrinsic discoloration can be related to insufficient polymer-
ization, the absorption of water or the adsorption of water-
soluble food coloring agents such as coffee, tea, red wine,
etc., deficient oral hygiene, or smoking [1, 6–9].
Provided such stains are superficial, and they can be
removed by polishing the material. However, deeper stains
are practically irreversible [1]. Intrinsic discoloration is
conditioned by staining of the composite resin itself, which
is related to the type of resin matrix involved. In this re-
gard, methacrylate resins are more resistant to staining than

Bis-GMA resins, thanks to their lesser viscosity and degree
of water absorption [9, 10]. In general, increased resin wa-
ter absorption is associated with increased staining poten-
tial [10]. Staining is also conditioned by the filler particle
size—smaller particle sizes being correlated to lesser stain-
ing susceptibility of the material [1]. In this respect, surface
roughness, which can result from particle loss during
polishing, influences the staining potential of the material.
Accordingly, the smaller the particle size, the lesser the
surface roughness resulting from particle loss during
polishing [5, 11]. Photoinitiators and other components
can also influence composite resin staining [12].
Materials based on the use of ormocer (organically
modified ceramic) technology are inorganic-organic hy-
brid polymers that form a siloxane network selectively
modified through the incorporation of organic groups. A
characteristic feature of these materials is the combination of
polysiloxane groups with photopolymerizable methacrylate
groups covalently bonded to silica. Photopolymerization
forms a mixed polymer that can be classified as a classical
reticulated inorganic silicate or as an organic polymer, de-
pending on its qualities. Because of this structural relation to
silicate ceramic or glass, such materials are also known as
organoceramics [13]. While composites consist of an organic
matrix with inorganic filler particles—classically the same
matrix based on Bis-GMA, methacrylate, or other organic
resins—ormocers are characterized by the presence of silica
plus four oxygen atoms (siloxane) in which the oxygen is
replaced by organic groups, resulting in a three-
dimensionally polymerized material with a lesser amount of
organic resin than the conventional composites. This in turn
affords superior biocompatibility due to the absence of free
monomers, lesser polymerization contraction, superior resis-
tance to abrasion, increased opacity, and improved polishing
and handling characteristics [14].
Only limited information is available on the color sta-
bility over time of ormocer-type organoceramics. We
therefore designed a study to analyze ormocer discolor-
ation caused by commonly consumed beverages, following
methodology similar to that used in studies involving clas-
sical composites [15–17]. Specifically, an in vitro study
was carried out to evaluate the color stability of two
nanohybrid resin-based composites, two organic modified
ceramic resin composites (ormocers) and a compomer, fol-
lowing their immersion during 4 weeks in red wine (RW),
coffee (CF), cola (CK), and distilled water (DW). A spec-
trophotometer was used to record the color based on the
CIEL*a*b* scale.
Three null hypotheses were considered: (a) color sta-
bility is not influenced by the type of material; (b) color
stability is not influenced by the type of staining bever-
age; and (c) the duration of immersion does not influence
color stability.
Clin Oral Invest
Material and methods
A total of 200 discs, each measuring 10 mm in diameter
and 2 mm in thickness, were prepared in a standardized
mold using the materials described in Table 1, with color
code A3 (n = 40 for each material). Those materials with
a single color were placed in a single increment, while
those requiring the combination of different components
in order to obtain the desired tone (A3 in our study) were
placed in several increments following the recommenda-
tions of the manufacturer (Table 1), polymerizing each
layer independently.
Polymerization was carried out using a LED lamp
(1200 mW/cm2) (Radii plus, SDI, Victoria, Australia). After
placing the materials in the molds, they were covered with a
transparent matrix (Mylar, DuPont, Wilmington, USA); a
glass lamina measuring 1 mm in thickness was placed on
top; pressure was applied to eliminate the excess; and poly-
merization was carried out following the instructions of the
manufacturer (Table 1)—in all cases at a distance of 1 mm.
The samples were immersed in distilled water at 37 °C during
24 h to complete polymerization.
The upper surfaces of all the specimens were then se-
quentially polished with medium (15 s), fine (15 s), and
super-fine (30 s) aluminum oxide-impregnated disks (Sof-
Lex; 3M ESPE, St. Paul, MN, USA) using a slow-speed
handpiece, at 10, 10, and 30,000 rpm, respectively, under
dry conditions. After each polishing step, the specimens
were thoroughly rinsed with water for 10 s to remove
debris, air dried for 5 s, and then polished with another
disc of lower grit for the same period of time as a final
polishing. The lower surface of each disc was marked
with a number to identify each sample and monitor the
color change in the different study phases. Discs were
stored in distilled water during 5 days before staining.
The 40 discs corresponding to each material were divided
into groups of 10 discs each according to the type of beverage
in which they were to be immersed (Fig. 1), and were again
stored in distilled water until the staining process was started.
The staining solutions used were red wine (RW)
(Tempranillo, Ciudad Real, Spain), coffee (CF) (Nescafe
Classic®, Nestle, Spain), cola (CK) (Coca-Cola®, The Coca-
Cola Company, Valencia, Spain), and distilled water (DW)
(Lasda, S.A., Valencia, Spain) as control. All the solutions
were used at room temperature. The coffee solution was ob-
tained by adding a spoonful of soluble coffee to 250 ml of
water at 40 °C, followed by stirring and cooling to room
temperature.
Four containers with 10 ml of staining solution were pre-
pared for each of the materials (20 containers in total). Ten
discs of each material were placed in each of the solutions, and
the latter were replaced every 2 days in order to avoid micro-
bial growth [15]. The discs were removed from the staining
Clin Oral Invest

Table 1 Study materials and their composition

Composite Compositiona Manufacturer and batch Color Polymerization

time

Grandio®SO (GR) Nanohybrid composite (89 % wt inorganic fillers: glass VOCO, Cuxhaven, A3 20 s
Nanohybrid ceramic filler (particle size 1 μm), silicon dioxide Germany
nanoparticles (20–40 nm), Bis-GMA, Bis-EMA, 1,444,262
TEGDMA, initiators, inorganic pigments, BHT
Dyract®XTRA (DY) UDMA, TCB resin, TEGDMA, trimethacrylate resin, Dentsply GmbH A3 10 s
Compomer camphorquinone, ethyl-4- dimethylaminobenzoate, Konstanz, Germany
BHT, UV stabilizer, strontium-alumino-sodium- 1,410,000,823
fluorophosphor-silicate glass, highly dispersed
silicon dioxide, strontium fluoride, iron oxide
and titanium dioxide pigments (mean filler
size: 0.8, filler volume 47 %)
Esthet·X®HD Bis-GMA, UDMA, TEGDMA Barium alumino-fluoro- Dentsply GmbH YE + A3 + A2- 20 s each capa
(EX) silicate glass (BAFG),1 lm; BAFG 0.02–2.5 lm Konstanz, Germany O
Nanohybrid (mean 0.6–0.8); nanosized silicon dioxide 140,607
(10–20 nm) 76 % wt (60 % vol.) 140,422
1,406,091
Ceram X®·duo(CX) Methacrylate modified polysiloxane, Dimethacrylate Dentsply GmbH Konstanz, E2 + D3 10 s
Ormocer Barium–aluminum–borosilicate glass, SiO2 (mean Germany 20 s
filler size 2–3 nm, filler volume 76 %) 1,410,000,984
1,408,000,369
Admira Resin matrix: aromatic and aliphatic dimethacrylates, VOCO, Cuxhaven, A3 20 s
Fusion® methacrylate-functionalized polysiloxane Germany
Ormocer Inorganic filler: Ba-Al-glass, pyrogenic SiO2, filler 1,434,168
load: 78 mass %. Photoinitiator: camphorquinone.
Synergist: NI

Bis-GMA bisphenol A glycidyl methacrylate, Bis-EMA bisphenol A ethoxylate dimethacrylate, TEGDMA diethyleneglycol dimethacrylate, BHT
butylated hydroxytoluene, UDMA urethane dimethacrylate, TBC resin dimethacrylate modified with carboxylic acid, BAFG barium alumino-fluoro-
silicate glass, YE translucent veneer, A3 intermediate body, A2–0 opaque dentin, E2 enamel, D3 dentin

solution, washed for 10 s with distilled water, dried with paper Statistical analysis
for 5 s, before color measuring.
Color recording was made using a Compact Vita A statistical analysis was performed using the SPSS version
EasyShade spectrophotometer (Vita Zahnfabrik, Bad 22.0 statistical package for MS Windows (SPSS Inc.,
Säckingen, Germany), calibrated before starting and again Chicago, IL, USA). Variables lacking a normal distribution
after the measurement of every 10 samples. The spectropho- were assessed using the Kolmogorov-Smirnov test. The non-
tometer consisted of a base unit and a handpiece with a 5-mm- parametric Kruskal-Wallis test was used for comparisons be-
diameter probe tip. Specimen was illuminated with spectro- tween groups. After the different immersion periods, the
photometer light, and reflected light was analyzed by the spec- Mann-Whitney U test was used to compare the color changes
trophotometer. Composite discs were placed on a flat white among the materials in the four different solutions, while the
surface inside of a black box where the spectrophotometer was
the only source of illumination. The spectrophotometer tip
was always placed perpendicularly to the disc surface [16].
Color recording of the polished discs was made before the
staining process (baseline) (T0) and after 1 (T1), 7 (T2), 14
(T3), 21(T4), and 28 days (T5) of immersion in the solution.
All color measurements were made by the same operator.
The variation in color was established based on the coordi-
nates: L (lightness, 0–100), a (−a* = green, +a* = red) and b
(−b* = blue, +b* = yellow) of the CIEL*a*b* scale.
Calculations were made of ΔL, Δa and Δb between baseline
and each of the study timepoints (1, 7, 14, 21, and 28 days), as
well as of ΔE or [(La-Lb)2 + (aa-ab)2 + (ba-bb)2]1/2 between Fig. 1 Distribution of the study groups. Red wine (RW), coffee (CF),
baseline and the 5 study timepoints. cola (CK), Distilled water (DW)

Wilcoxon signed rank test was used for comparisons between
the evaluation periods for each experimental group. A p value
of <0.05 was considered significant.
Results
The mean values and standard deviations of the color changes
(ΔE) of the materials after 28 days of immersion in the differ-
ent solutions are shown in Table 2. In relation to the staining
solutions, RW showed the strongest staining potential in ap-
plication to all the materials except AD, which was most ex-
tensively stained by CF—though the differences were not sta-
tistically significant (p > 0.05) The material most intensively
stained by RW was DY (ΔE = 31.09), while the least stained
material was EX (ΔE = 15.56). The second most intensely
staining solution was CF—AD being the most intensely
stained material (ΔE = 26.05), while EX was the material with
the best color stability (ΔE = 5.57). Cola was found to exert a
greater staining effect upon DY (ΔE = 12.21), with significant
differences versus the rest of the materials (p < 0.05). The least
stained material was CX (ΔE = 2.39). Immersion in distilled
water resulted in significant staining of AD compared with the
rest of the materials (p > 0.05). EX and CX were the materials
least stained by RW and CF (p < 0.05), while EX, CX, and GR
were stained to a similar extent by CK (p > 0.05).
Figure 2 shows the evolution of the color changes (ΔE) in
the course of the study for each material and staining solution.
Progression of the color gain with RW was much more noto-
rious than with the rest of the solutions, with variations in ΔE
at the end of the study of between 11.57 points for CX and
23.61 for DY. With CF, the color variations were in the order
of three points, except for AD, where ΔE was found to be
17.82 points. Lastly, in the case of CK, the ΔE values ranged
between 3.51 points with AD and −1.08 with GR.
On analyzing the color change for each material indepen-
dently of the staining solution used, EX and CX showed sig-
nificantly less staining than the rest of the materials after 1 and
7 days of immersion (p < 0.05) (Fig. 3). In contrast, from
14 days onwards, AD showed significantly greater staining
than GR, EX or CX (p > 0.05), while GR and DY were found
Table 2 Mean (standard deviation) of the color change (ΔE) of the materials at the end of the study
Red wine (RW)
Grandio®SO (GR) 25.08(3.52)b
Dyract®XTRA (DY) 31.09(3.06)
Esthet·X®HD (EX) 15.56(2.87)a
Ceram X®·duo (CX) 16.20(2.11)a
Admira®Fusion (AD) 24.04(2.48)b1
Same superscript letters in the same column indicate nonsignificant difference (p > 0.05). Same subscript number in the same row indicate nonsignificant
difference (p > 0.05)
Clin Oral Invest
to be similar, in the same way as AD and DY. In order of
descending color stability, the materials were found to be dis-
tributed as follows: EX > CX > GD > DY > AD.
Discussion
Dental restoration materials are constantly exposed to the oral
environment and are subjected to changes in temperature and
pH, abrasion, water-soluble coloring agents, dental plaque,
etc. All this results in a series of extrinsic and intrinsic changes
in the materials that can modify their physical and mechanical
characteristics and esthetic properties [2, 18].
The color stability of composite materials has been inves-
tigated in both in vitro and in vivo studies [19–24], and is
conditioned by a range of factors including the type of resin
matrix used, particle size, polymerization depth, filler loading,
and contact with coloring agents [10, 17, 25, 26]. Composite
staining capacity is directly related to the hydrophilic proper-
ties of the resin. In this regard, the more hydrophilic a given
resin, the greater its capacity to absorb not only water but also
water-soluble coloring agents [1, 10].
In the present study, we used commonly consumed bever-
ages, all with a known capacity to stain both natural teeth and
restorative materials [22–25]. The maximum immersion inter-
val was 4 weeks, since according to Ertas et al. [19], this
period is equivalent to 2.5 years of use—the minimum 24 h
contemplated in our study being equivalent to 1 month of
exposure in the mouth.
It is currently accepted that a color differences of ΔE < 1.0
is imperceptible to the human eye while values of ΔE > 3.3
are regarded as clinically unacceptable [10, 27]. A recent
study has shown ΔE threshold perceptibility and acceptability
of 1.2 and 2.7, respectively, in dentists, evaluated on ceramics
samples. Significant differences were observed among the
different professional groups which participated in the study
[28]. In our study, all the materials showed clinically unac-
ceptable ΔE values even from the first 24 h of immersion in
all of the solutions except CX immersed in CK, where the
final value was ΔE = 2.39. Indeed, even immersion in dis-
tilled water yielded ΔE = 8.99 for AD. These results do not
Cola (CK) Coffee (CF) Distilled water (DW)
3.24(1.03)a1 13.09(3.92)a 1.60(0.66)a1
12.21(2.88)1 9.86(3.03)a,b1 2.71(0.68)a
3.70(2.55)a1 5.57(2.47)c1 2.87(1.57)a1
2.39(1.14)a1 6.88(3.18)b,c2 3.38(1.33)a1,2
6.63(2.45)a2 26.05(4.96)1 8.99(2.33)2
Clin Oral Invest
Fig. 2 Evolution of the color variation (ΔE) for each material and
staining solution over the course of the study. Red wine (RW), coffee
(CF), cola (CK), distilled water (DW); GrandioSO (GD), Dyract XTRA
(DY), Esthet·X HD (EX), Ceram-X duo (CX), Admira Fusion (AD); 1 day
(ΔE1), 7 days (ΔE2), 14 days (ΔE3), 28 days (ΔE4)
coincide with those of other authors who consider that water
absorption alone does not visibly alter the color of composite
resins [6, 10, 29]. However, Erdemir et al. recorded staining
values above the acceptable limits for some composites after
immersion in distilled water only [17].
Janda et al. [30] evaluated the color stability of different
materials according to the polymerization technique used
(constant versus exponential), followed by immersion in dis-
tilled water, and observed less color stability when an expo-
nential technique was used. According to these authors, the
best polymerization mode for ensuring greater color stability
is constant light applied for 20 s. This was the polymerization
time used in our study.
Fig. 3 Mean (standard deviation) of the color change (ΔE) of each
material over the course of the study. GrandioSO (GD), Dyract XTRA
(DY), Esthet·X HD (EX), Ceram-X duo (CX), Admira Fusion (AD); 1 day
(ΔE1), 7 days (ΔE2), 14 days (ΔE3), 21 days (ΔE4), 28 days (ΔE5)
The present study evaluated the color stability of two
nanohybrid composites, two ormocers and a compomer fol-
lowing immersion for between one and 28 days in staining
solutions commonly found in the diet (red wine, coffee, cola),
and used distilled water as control. In view of the results ob-
tained, our first null hypothesis must be rejected, since not all
the materials behaved in the same way in terms of color sta-
bility. In this respect, DY was the material with the poorest
color stability, a fact that may be explained by its composition,
since it contains hydrophilic resins such as Bis-GMA and
HEMA, and carboxyl groups that confer increased water af-
finity [20]. The second most intensely stained material was
GR, which contains a Bis-GMA based organic matrix with
greater hydrophilicity than methacrylate materials [9, 10].
Surprisingly, AD showed strong staining capacity. This could
be explained by inadequate integration between the pre-
polymerized microfiller particles and the siloxane particles
around the resin. While not intrinsically hydrophilic, this type
of structure could suffer discoloration if the interphase is not
correctly silanized and integrated within the resin matrix, thus
allowing the infiltration of water and coloring agents [24].
However, CX, which also contains siloxane, showed the
greatest color stability along with EX, which contains little
Bis-GMA and has a smaller particle size than GR.
On the other hand, regarding placement of the material, EX
and CX were placed in three and two increments, respectively,
in order to obtain the standardized color A3 for this study,
while the rest of the materials were placed and polymerized
in a single increment during 20 s—a factor that also may have
contributed to greater color stability in these two groups of
materials [31].
Our second null hypothesis also must be rejected, since the
color stability of the materials was influenced by the type of
staining solution, in coincidence with the observations of other
authors [22–24]. The solutions can be distributed in order of
increasing staining potential as follows: DW < CK < CF < RW.
Surprisingly, the ΔE values obtained with CK were similar to
those of the control group, except in application to DY. However,
according to Um et al. [27], this could be explained by the fact that
although theacidpH of CK can deterioratethe composite surface,
this solution contains few low-polarity yellow pigments. On the
other hand, the acidic nature of CK could deteriorate the
compomer surface more than the surface of the composite mate-
rials, and this would explain the greater color stability loss seen
with DY. Red wine was the solution with the strongest capacity to
stain all the analyzed materials, followed by CF. Different studies
have indicated that ethanol is able to degrade the organic matrix,
which would contribute to the greater staining potential of RW.
Tsitrou et al. [32] evaluated the capacity of ethanol to dissolve
monomers of different resins, including EX and AD. These au-
thors found a larger amount of bis-GMA in AD than in EX, which
could explain the important discoloration produced by RW in
application to AD. However, the many pigments contained in

RWalso must be taken into account [5]. The combination of both
factors could be the cause of the greater discoloration produced
by RW in all the evaluated materials. Coffee contains abundant
yellow pigments, with strong affinity for the polymers, and the
combination of both factors may be the reason for staining [15].
Finally, our third null hypothesis also must be rejected,
since the duration of immersion influenced the intensity of
staining, particularly in the case of RW and CF. As can be
seen in Fig. 2, the color changes intensified over time—a fact
that could be explained by more prolonged interaction be-
tween the staining solutions and the resin, together with great-
er resin penetration of the coloring agents [10, 12–17, 20, 33].
It can be concluded that all the staining solutions produced
darkening beyond clinically acceptable limits. EX and CX
were the materials who experimented less staining, followed
by GD. AD and DY were the materials more stained. RW was
the drink that produced more staining, followed by CF and
CK.
Compliance with ethical standards
Conflict of interest The authors declare that they have no conflict of
interest.
Funding The work was supported by the authors.
Ethical approval This article does not contain any studies with human
participants or animals performed by any of the authors.
Informed consent For this type of study, formal consent is not
required.
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