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Andr Poitevin a , Jan De Munck a , Annelies Van Ende a , Yuji Suyama a,b , Atsushi Mine a,c ,
Marleen Peumans a,d , Bart Van Meerbeek a,d,
a KU Leuven BIOMAT, Department of Oral Health Sciences, KU Leuven (University of Leuven), Leuven, Belgium
b Toranomon Hospital, Tokyo, Japan
c Department of Oral and Maxillofacial Rehabilitation, Okayama University Graduate School of Medicine, Dentistry and Pharmaceutical
a r t i c l e i n f o a b s t r a c t
Article history: Self-adhesive composites (SACs) are claimed to bond to tooth substrate without a separate
Received 1 March 2012 adhesive. Bonding effectiveness data are however still limited.
Received in revised form Objectives. In SubProject 1, the hypothesis was tested that the micro-tensile bond strength
2 October 2012 (TBS) to dentin of two owable SACs was alike that of a one-step self-etch adhesive (1-SEa)
Accepted 2 October 2012 combined with a owable composite (owC). In SubProject 2, the hypothesis was tested that
the nature of the smear layer did not affect the TBS of the SACs to dentin/enamel.
Methods. SubProject 1: The TBS to bur-cut dentin of two SACs (Fusio Liquid Dentin, Pentron;
Keywords: Vertise Flow, Kerr) was measured and compared to that of four 1-SEa/owC combinations
Self-adhesive (AdheSe One/Tetric EvoFlow, Ivoclar Vivadent; Adper Prompt L-Pop/Filtek Supreme XT Flow-
Composite able, 3M ESPE; iBond/Venus ow, Heraeus Kulzer; Xeno V/X-ow, Dentsply) and of one 3-step
Micro-tensile bond strength etch-and-rinse adhesive (3-E&Ra: OptiBond FL, Kerr) combined with Premise Flowable (Kerr).
Dentin The effect of pre-etching dentin with phosphoric acid on the TBS of the SAC Vertise Flow
Enamel (Kerr) was measured as well. SubProject 2: The TBS of the two SACs and one 1-SEa/owC
Smear layer combination (Adper Prompt L-Pop/Filtek Supreme XT Flowable, 3M ESPE) to either bur-cut
or SiC-paper ground dentin/enamel was measured. The effect of pre-etching enamel with
phosphoric acid on the TBS of the SAC Vertise Flow (Kerr) was also measured.
Results. SubProject 1: The TBS to dentin of both SACs was signicantly lower than that of the
1-SEa/owC and the 3-E&Ra/owC combinations, of which the latter performed best. The
SAC Fusio Liquid Dentin (Pentron) bonded signicantly better to dentin than Vertise Flow
(Kerr), except when dentin had additionally been pre-etched with phosphoric acid. SubPro-
ject 2: Surface smear did not interfere with bonding of the SACs to dentin/enamel, while
their TBS remained signicantly lower than that of the 1-SEa/owC combination. Prior
phosphoric-acid etching of dentin/enamel signicantly ameliorated the bonding effective-
ness of Vertise Flow (Kerr).
Signicance. The bonding effectiveness of owable SACs underscores that of 1-SEas and one
gold-standard 3-E&Ra when combined with their proprietary owable composite. Conse-
quently, routine clinical application of SACs should be carefully considered.
2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Corresponding author at: KU Leuven BIOMAT, Department of Oral Health Sciences, KU Leuven (University of Leuven), Kapucijnenvoer 7,
blok a bus 7001, BE-3000 Leuven, Belgium. Tel.: +32 16 337587; fax: +32 16 332752.
E-mail address: bart.vanmeerbeek@med.kuleuven.be (B. Van Meerbeek).
0109-5641/$ see front matter 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.dental.2012.10.001
222 d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230
One-step self-etch AdheSe One (Ivoclar Derivatives of bis-acrylamide, water, bis-methacrylamide dihydrogen Brush onto the surface for >30 s; disperse excess with a
adhesive Vivadent, Schaan, phosphate, amino acid acrylamide, hydroxyalkyl-methacrylamide, highly strong stream of air; light cure for 10 s.
Liechtenstein) dispersed silicon dioxide, catalysts, stabilizers [L49718]
Adper Prompt L-Pop (3M First blister: methacrylic phosphates, bis-GMA photo initiator [412924] Brush onto the surface; massage for 15 s applying
d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230
ESPE, Seefeld, Germany) Second blister: water, HEMA, polyalkenoic acid polymer [412924] pressure; gentle stream of air to thoroughly dry to a thin
lm; apply a second coat without massage; gentle stream
of air to thoroughly dry to a thin lm; light cure for 10 s.
iBond (Heraeus Kulzer, UDMA, 4-meta, glutaraldehyde, acetone, water, photoinitiators, stabilizer Application for 20 s with agitation; start with gentle air
Hanau, Germany) [010075] blow, followed by a strong air blow for at least 5 s; light
cure for 20 s.
Xeno V (Dentsply, Bifunctional acrylic amides, acryloamido alkylsulfonic acid, functionalized Apply adhesive twice; gently agitate for 20 s; carefully air
Konstanz, Germany) phosphoric acid ester, acrylic acid, camphorquinone, butylated blow for 5 s; light cure for 20 s.
benzenediol, water, tert-butanol, photoinitiators, stabilizer [0908001751]
Three-step OptiBond FL (Kerr, Orange, Etching: 37.5% phosphoric acid, silica thickener [3034827] Etch for 15 s; rinse thoroughly for 15 s; gently air dry for
etch-and-rinse CA, USA) Primer: HEMA, GPDM, PAMM, ethanol, water, photo-initiator [3457744] 3 s; apply primer with light brushing motion for 15 s; air
adhesive Adhesive: TEGDMA, UDMA, GPDM, HEMA, bis-GMA, ller, photo initiator dry for 5 s; apply adhesive with light brushing motion for
[3461592] 15 s; air thin for 3 s; light cure for 20 s.
Flowable composite Filtek Supreme XT Flowable Bis-GMA, TEGDMA, bis-EMA, functionalized dimethacrylate polymer, Apply in layers of max 2 mm and light cure for 20 s.
(3M ESPE, St. Paul, MN, USA) silane treated ceramic, silane treated silica, silane treated zirconium oxide
[N110837]
Premise Flowable (Kerr, Bis-EMA, TEGDMA, silica nanoller [3044072] Apply in layers of max 2 mm and polymerize for 20 s.
Orange, CA, USA)
Tetric EvoFlow (Ivoclar Bis-GMA, UDMA, decamethylene dimethacrylate, barium glass, ytterbium Apply in layers of max 2 mm and light cure for 20 s
Vivadent, Schaan, triuoride, highly dispersed silicon dioxide, mixed oxide and copolymer (>500 mW/cm2 ) or 10 s (>1000 mW/cm2 ).
Liechtenstein) [L36209]
Venus ow (Heraeus-Kulzer, Bis-GMA, TEGDMA, barium glass [010122] Apply in thin layers (max 2 mm, baseliner max 1 mm);
Hanau, Germany) apply a gentle stream of air and light cure for 20 s.
X-ow (Dentsply, Konstanz, DGDMA, di- and multifunctional acrylate and methacrylate resins, Incremental placement in 2 mm layers or less;
Germany) strontium alumino sodium uoro phosphor silicate glass, highly dispersed polymerization for at least 20 s.
silicon dioxide, UV stabilizer, ethyl-4-dimethylaminobenzoate,
camphorquinone, butylated hydroxyl toluene, iron pigments, titanium
oxide [0808001149]
a
Composition as provided by respective manufacturer: bis-EMA, ethoxylated bisphenol A glycol dimethacrylate; bis-GMA, bisphenol-glycidyl methacrylate; DGDMA, diethylene glycol dimethacry-
late; GPDM, glycerol phosphate dimethacrylate; HEMA, hydroxyethylmethacrylate; PAMM, phthalic acid monoethyl methacrylate; TEGDMA, triethylene glycol dimethacrylate; UDMA, urethane
223
dimethacrylate; 4-MET, 4-methacryloxyethyltrimetellitic acid.
224 d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230
were recorded as either cohesive in dentin, adhesive at the dentin with phosphoric acid signicantly increased the TBS
interface with the self-adhesive owable composite or adhe- of the SAC Vertise Flow (Kerr; p < 0.001).
sive, cohesive in the adhesive, adhesive at the interface Failure analysis in SubProject 1 predominantly revealed
between the adhesive and owable composite, and cohe- adhesive failures at the interface of both the SACs when
sive in the (self-adhesive) owable composite. Representative they were bonded to BUR-CUT dentin, and even for Vertise
specimens were selected for fractographic examination by Flow (Kerr) when dentin was pre-etched with phosphoric acid
Feg-SEM (Philips XL30, Eindhoven, The Netherlands), and (Table 2). A clearly more non-adhesive failure pattern was
processed appropriately, including xation in glutaraldehyde, recorded for the 1-SEa/owC and 3-E&Ra/owC combinations.
dehydration in ascending concentrations of ethanol, and The bonding effectiveness data of SubProject 2, in which
chemical drying following the protocol described in detail by potential interference of a thick versus thin smear layer on
Perdigo et al. [22]. the bonding effectiveness to dentin and enamel was tested,
are shown in Tables 3 and 4, and Figs. 3 and 4 for dentin and
2.4. Statistical analysis enamel, respectively.
When bonded to dentin (Table 3 and Fig. 3), the nature of
One-way analysis of variance (ANOVA) in SubProject 1 and the smear layer had no effect on the bonding effectiveness
two-way ANOVA in SubProject 2, and Tukey HSD multiple
comparisons test (both subprojects) were used to determine
statistical differences in TBS. All data were analyzed at a
signicance level of 0.05 using a software package (R2.12, R
Foundation for Statistical Computing, Vienna, Austria).
3. Results
d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230
XT Flowable
iBond/Venus ow 23.9 (10.3) 1/31 24.7 4 29 0 33 34
Xeno V/X-Flow 29.4 (11.7) 0/30 29.4 6 2 0 2 90
Table 3 Micro-tensile bond strength (TBS) and failure analysis for the adhesive materials bonded to BUR-CUT versus SiC-GROUND dentin (SubProject 2).
Adhesive material TBS (SD) ptf/n TBS (excl. Failure mode
(ptf = 0 MPa) ptf)
225
226 d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230
(self-adhesive)
Cohesive in
composite
owable
0
13
27
17
3
20
15
4
Table 4 Micro-tensile bond strength (TBS) and failure analysis for the adhesive materials bonded to BUR-CUT versus SiC-GROUND enamel (SubProject 2).
owable composite
interface between
adhesive and
Adhesive at
0
Failure mode
in adhesive
Cohesive
0
Cohesive Adhesive at interface
97
80
6
74
0
0
79
22
BUR-CUT (p = 0.01783 for Fusio Liquid Dentin; p < 0.001 for Ver-
13.0
11.0
23.1
28.0
10.8
15.3
22.6
25.5
tise Flow) and SiC-GROUND (p < 0.001 for both SACs) dentin
ptf/n
0/33
0/29
0/35
0/25
(ptf = 0 MPa)
TBS (SD)
13.0 (4.3)
11.0 (4.2)
23.1 (7.1)
28.0 (9.8)
10.8 (5.8)
15.3 (6.0)
22.6 (7.6)
25.5 (8.2)
Adhesive material
L-Pop/Filtek Supreme
L-Pop/Filtek Supreme
H3 PO4 + Vertise Flow
Adper Prompt
Vertise Flow
Vertise Flow
XT Flowable
XT Flowable
SiC-GROUND
Fig. 5 Feg-SEM photomicrographs of fractured micro-specimens. (a) Feg-SEM of the fractured BUR-CUT dentin side of a
representative specimen prepared with Fusio Liquid Dentin (Pentron); I, interface. Arrow, osmosis droplets. (b) Feg-SEM of
the fractured BUR-CUT dentin side of a representative specimen prepared with Vertise Flow (Kerr). (c) Feg-SEM of the
fractured BUR-CUT dentin side of a representative specimen prepared with Adper Prompt L-Pop/Filtek Supreme XT
Flowable; Ar, adhesive resin; C, composite. (d) Feg-SEM of the fractured BUR-CUT dentin side of a representative specimen
prepared with Xeno V/X-ow (Dentsply).
than the 1-SEa/owC (control) combination Adper Prompt except when enamel was pre-etched with phosphoric acid.
L-Pop/Filtek Supreme XT Flowable (3M ESPE). A clearly more non-adhesive failure pattern was recorded
When bonded to enamel (Table 4 and Fig. 4), the nature of for the 1-SEa/owC combination Adper Prompt L-Pop/Filtek
the smear layer had no effect on the bonding effectiveness Supreme XT Flowable (3M ESPE).
for any of the adhesive materials tested. Both SACs did not In general, Feg-SEM of the most representative failures
bond statistically different, irrespective of the nature of the in each experimental group conrmed the failure patterns
smear layer (p = 0.9312 for Fusio Liquid Dentin; p = 0.2312 for observed using the optical microscope. Specic fracture char-
Vertise Flow). Pre-etching enamel with phosphoric acid sig- acteristics were observed and are illustrated in Fig. 5, namely
nicantly increased the TBS of the SAC Vertise Flow (Kerr) both the SACs failed predominantly at the interface and were
to both BUR-CUT (p < 0.01) and SiC-GROUND enamel (p < 0.01), unable to remove the smear plugs out of the tubules.
of which the TBS was no longer signicantly different from
the respective bond of the 1-SEa/owC (control) combination
Adper Prompt L-Pop/Filtek Supreme XT Flowable (3M ESPE) to 4. Discussion
BUR-CUT (p = 0.0665) and SiC-GROUND enamel (p = 0.7614).
Failure analysis in SubProject 2 predominantly revealed So far, no independent data are available regarding the TBS
adhesive failures at the interface of both the SACs when of the recently developed composite technology claiming to
they were bonded to both BUR-CUT and SiC-GROUND dentin self-adhere to tooth tissue. With this study, we have tested
(Table 3). A clearly more non-adhesive failure pattern was the bonding effectiveness of the today only two commercially
recorded for the 1-SEa/owC combination Adper Prompt L- available self-adhesive owable composites.
Pop/Filtek Supreme XT Flowable (3M ESPE), when bonded to Hypothesis 1, as tested in SubProject 1, that the TBS to
both BUR-CUT and SiC-GROUND dentin. When bonded to BUR-CUT dentin of the two owable SACs was alike that of
BUR-CUT and SiC-GROUND enamel (Table 4), the predominant the 1-SEa/owC combinations, should be rejected. One could
failure pattern was adhesive at the interface for both SACs, expect, and even accept, that the very simple-to-use SACs,
228 d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230
applied without a separate adhesive, would bond less effec- the two SACs tested appeared also from the number of pre-
tively to dentin than when a owC would be bonded to dentin testing failures recorded (see also below), being respectively
using the multi-step gold-standard 3-E&Ra (OptiBond FL, 67% and 45% when Vertise Flow was bonded to BUR-CUT and
Kerr) [1,21]. However, in light of a potentially universal use as SiC-GROUND dentin, versus no pre-testing failures for Fusio
a restorative material, one could argue that the bonding effec- Liquid Dentin (Pentron). In this respect, it is also noteworthy
tiveness of a SAC should minimally meet that of a 1-SEa/owC that no pre-testing failures were recorded for any of the SACs
combination; this is the reason why we selected four such 1- when bonded to enamel (SubProject 2).
SEa/owC combinations in this study as references/controls. SubProject 2 conrmed the results obtained in SubPro-
While the SAC Vertise Flow (Kerr) underperformed three out ject 1. Hypothesis 2, as tested in SubProject 2, that the
of the four 1-SEa/owC combinations, the other SAC Fusio Liq- nature of the smear layer did not affect the TBS of the SACs
uid Dentin (Pentron) only underperformed two 1-SEa/owC to dentin and enamel, was accepted. Indeed, no difference
combinations, and was equally effective and even signicantly in bonding effectiveness to BUR-CUT versus SiC-GROUND
more effective than the other two 1-SEa/owC combinations. enamel and dentin was recorded, though one could have
Self-evidently, for comparison we combined the 1-SEas with expected that the SACs would have bonded better to the
the owable composite produced by the same manufacturer, latter thinner, more regular and less compact smear-layer
as the kind of composite (and the actual brand) is known to covered tooth substrates. Preliminary research characteriz-
signicantly inuence the TBS [23]. ing the interface of the SAC Vertise Flow (Kerr) with enamel
Differences in bonding effectiveness between the two and dentin using TEM revealed an interface with tiny micro-
SACs tested can in principle be ascribed to many factors, tags formed at bur-cut enamel [27]. In addition, also a rather
among which probably the actual composition and the kind supercial interaction was observed at dentin, where Vertise
of functional monomer contained in the material formula- Flow (Kerr) was observed not to have removed smear plugs
tion might be most determining (Table 1). The SAC Fusio out of the tubules for BUR-CUT, nor for SiC-GROUND dentin
Liquid Dentin (Pentron) contains the functional monomer [27]. The predominantly adhesive failures at the interface
4-methacryloxyethyltrimetellitic acid (4-MET) that has been of the SAC with the tooth substrate conrm the relatively
attributed chemical bonding potential to hydroxyapatite (HAp) supercial interaction achieved. This kind of supercial inter-
and tooth tissue [24], the latter however signicantly less action should be regarded as very alike that documented
strong than for instance 10-methacryloyloxydecyl dihydrogen for self-adhesive luting composites [812], as well as that
phosphate (10-MDP). The functional monomer used in Ver- reported for another experimental self-adhesive lling mate-
tise Flow (Kerr) is glycerol phosphate dimethacrylate (GPDM). rial [28].
This monomer is also used in the 3-step etch-and-rinse adhe- Pre-etching enamel and dentin signicantly improved the
sive OptiBond FL (Kerr) that in laboratory as well as clinical bonding effectiveness of the SAC Vertise Flow (Kerr), by which
research has proven to belong among the currently top- hypothesis 3 was rejected. This was expected when bond-
performing adhesives [21,23]. To our knowledge, no data on ing to enamel, since phosphoric acid signicantly enhances
chemical analytic data on the bonding potential of GPDM are the surface energy of enamel and thus provides signicantly
available. Recent interfacial analysis of its two-step successor more micro-retention [1]. The nature of the smear layer did
OptiBond XTR (Kerr) that also contains GPDM, nevertheless of course not play a role, since phosphoric acid is strong
revealed a 2-m deep hybrid layer free of HAp (unpublished enough to dissolve and, upon rinsing, remove both the thicker
observations); following the AD-concept [25,26], this most BUR-CUT as well as the thinner SiC-GROUND smear layer.
likely indicates that GPDM etches rather than bonds to A similar improved bonding effectiveness following before-
HAp. To achieve self-adhesiveness, we believe that a relatively hand phosphoric-acid etching was previously found when
viscous (owable) composite should contain a functional a self-adhesive luting composite was bonded to enamel [8].
monomer that rather possesses an effective chemical bonding In addition, Rengo et al. [17] found that pre-etching enamel
potential, as it cannot penetrate deeply. To fully elucidate the had no inuence on micro-leakage. A benecial effect of
bonding mechanisms of both the SACs tested, further in-depth pre-etching dentin with phosphoric acid on the bonding
chemical interfacial analysis is denitely needed to comple- effectiveness of Vertise Flow (Kerr) was not so expected, as
ment some interfacial ultra-structure data already available previous bond-strength tests for the same above-mentioned
(see below). self-adhesive luting composite revealed the opposite and thus
Besides compositional differences, the rheological proper- detrimental effect [8]. In that study, TEM revealed that phos-
ties of the two SACs tested differed completely, with Fusio phoric acid clearly exposed collagen up to a few micrometers
Liquid Dentin (Pentron) being signicantly more uid than depth. The relatively viscous luting composite could not ade-
Vertise Flow (Kerr). This should in part be ascribed to the lower quately hybridize the collagen mesh, the reason why the
ller content in range of 65 wt% for Fusio Liquid Dentin (Pen- signicant reduction in bonding effectiveness was measured
tron) versus 70 wt% for Vertise Flow (Kerr). In this respect, [8]. Likewise, Rengo et al. reported that pre-etching dentin sig-
Fusio Liquid Dentin (Pentron) was found to be placed more nicantly affected the marginal sealing potential of Vertise
easily onto the tooth surface; it showed less stickiness to the Flow (Kerr) [17]. Eventually, it remains to assess how good the
application instrument, and wetted better both dentin and bond of SACs to enamel and dentin, even when beforehand
enamel. Such apparent easier handling may at least in part etched with phosphoric acid, will resist biodegradation on the
have contributed to the better bonding effectiveness of Fusio long term. One study evaluating Vertise Flow (Kerr) recently
Liquid Dentin (Pentron) versus that of Vertise Flow (Kerr). revealed a remarkable decline in shear bond strength upon
This signicant difference in bonding effectiveness between aging [20].
d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230 229
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