THE JOURNAL OF - Dentsply

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Blunck/Zaslansky Table 1 Tested adhesive system/composite resin combinations Group Adhesive system Composite resin Adhesive manufacturer Multi-bottle systems Syntac Artemis Ivoclar Vivadent; Schaan, (control) Liechtenstein OptiBond FL Herculite XR Kerr; Danbury, CT, USA Clearfil SE Bond Clearfil AP-X Kuraray; Tokyo, Japan All-in-one Prompt L-Pop 1999 Tetric Ceram ESPE; Seefeld, Germany adhesive systems Prompt L-Pop 2000 Tetric Ceram ESPE with mixing Adper Prompt L-Pop Tetric Ceram 3M ESPE; St Paul, MN, USA Adper Prompt L-Pop Filtek Z250 3M ESPE Futurabond NR Grandio Voco; Cuxhaven, Germany One-up Bond F Estilite Tokuyama; Tokyo, Japan Xeno III Tetric Ceram Dentsply DeTrey; Konstanz, Germany Xeno III Dyract eXtra Dentsply DeTrey Xeno III Quixfil Dentsply DeTrey All-in-one AQ Bond Metafil CX Morita; Irvine, CA, USA adhesive systems G-Bond Gradia GC; Tokyo, Japan without mixing Hybrid Bond Metafil Morita iBond Charisma Heraeus Kulzer, Hanau, Germany tri-S bond Clearfil AP-X Kuraray plying multi-bottle or one-bottle adhesives, and self-etching systems that contain acid monomers which can condition both enamel and dentin simultaneously with no rinsing. 36 Self-etching adhesive systems can be applied in two consecutive steps or as so-called all-in-one adhesives. The latter are available in two forms: those that require mixing and those that do not. The effectiveness of adhesive systems can be tested in vitro by bond strength measurements of various kinds, by penetration tests of Class V/II fillings with different substances, and by evaluating the margin quality of Class I/II/V or cylindrical fillings under a microscope. 17 In this study, visual inspection of discontinuities at the margins was performed using a scanning electron microscope (SEM), dedicated to the identification and quantification of dental margin qualities. 26 This method has several advantages, such as the high level of detail revealed and marked accuracy, allowing it to be used for evaluating the same margins at different times. This is particularly useful for testing the effects of water storage or stress on the same specimens. This paper considers the effectiveness of all-in-one adhesive systems in comparison to reference multi-bottle adhesive systems, as judged by evaluating the marginal integrity in dentin and enamel after different periods of water storage. The effects of short- vs long-term storage were exemplified by applying thermal stress in order to expose marginal degradation differences. This was used to study the state of the restoration margins at 3 weeks, 1 year and 3 years, and consider some aspects of the dynamics of adhesive aging. MATERIALS AND METHODS This work reflects the current status of a large ongoing study. Teeth, anonymously collected following routine dental treatment, were stored in 0.1% thymol solution at room temperature prior to and during the experimental period. One hundred thirty-six caries-free extracted human anterior teeth were used, and typical Class V cavities were prepared with a diamond bur (diamond bur No. 838/314/014; Gebr. Brasseler; Lemgo, Germany) at high speed using water as a coolant. Oval preparations were a standard size: approximately 4 mm high, 1.5 mm deep, and 3 mm wide (2 mm apical to the cementoenamel junction spanning across the CEJ and into enamel). The enamel portions were bevelled with a finishing diamond bur (Composhape H-15, Intensiv; Viganello-Lugano, Switzerland) and the cavosurface margins in dentin finished to a 90-degree angle with a finishing diamond (No. 8838/314/012, Gebr. Brasseler). The teeth were randomly divided into 17 groups of 8 teeth each. Each group of teeth was assigned to one of 17 treatments. These included 14 combinations of all-in-one adhesive system/composite resins and three multi-bottle adhesive systems (Syntac and OptiBond FL, etch-and-rinse technique, and Clearfil SE Bond, self-etching technique). The adhesives were all applied and restored with composite resin according to the manufacturer’s instructions as detailed in Table 1. In an attempt to ensure optimal performance of the adhesives, the composite used was generally that recommended by the adhesive manufacturer, although for some of the adhesives (Adper Prompt L-Pop and Xeno III), several 232 The Journal of Adhesive Dentistry
Blunck/Zaslansky composites were used. The composite resin was inserted in two increments (initially placed at the cervical margin), and each increment was light cured (Astralis 10 light-curing unit, Ivoclar Vivadent; Ellwangen, Germany) for 40 s. After finishing and polishing (Sof-Lex Pop-on Nr. 1981 SF/F/M/C 3M ESPE; St Paul, MN, USA), the teeth were returned to water storage for 21 days, followed by 2000 cycles of thermocycling (TC) between +5 and +55°C. Prior to and after TC, impressions were taken with a polyvinylsiloxane material (Silagum light body, DMG; Hamburg, Germany) and replicas of the restoration and surrounding tooth structures were produced. These were cast with an epoxy resin following precise manufacturer guidelines (Stycast 1266 Part A + B; Emerson and Cumming; Westerlo-Oevel, Belgium). Once fully cured, each replica was sputter-gold coated (SCD 030, Balzers Union; Balzers, Liechtenstein) in preparation for inspection by SEM. Similar impression and TC procedures were repeated after 1 year of water storage, and for 11 products also after 3 years. The effectiveness of each bonding system was assessed by evaluating the margins of the restorations at the dentin/composite and enamel/composite interface. Measurements were performed using a dedicated SEM (AMRAY 1810, Amray; Bedford, MA, USA) and all replicas were viewed at a magnification of 200X, and classified according to the state of the margin in different areas in order to numerically quantify the marginal qualities, as detailed in Table 2. By using this method, each segment of the tooth/restoration interface was imaged and ranked according to defined quality criteria. These were then converted into percentage of the total margin length, in dentin and enamel independently. Statistical evaluation was performed using an SPSS statistical software package (SPSS Software; München, Germany). Within each sample group, significant differences were determined using the nonparametric Wilcoxon test. For comparison between the different treatment groups, the nonparametric Kruskal-Wallis test was used followed by Bonferroni adjustment. The statistics were calculated for the parameter margin quality 1 (MQ1 = “excellent” or “continuous” margin). Origin 7.0 SR0 (Originlab; Northampton, MA, USA) was used for the weighted regression and Microsoft Excel (2000) was used to determine the slopes between MQ1 rankings at different stages of the experiment. RESULTS The results of the 14 test groups were compared with those of the 3 reference multi-bottle adhesives OptiBond FL, Syntac, and Clearfil SE Bond. Figure 1 is a box-and-whiskers plot of the marginal quality MQ1results determined for the enamel margins, depicting the median, 25 and 75 percentiles. The main result seen here is that after 1 year of water storage (Fig 1a) and following a second TC, a reduction (significant at p < 0.05) in the amounts of “continuous margins” (MQ1) is seen for G-Bond, AQ-Bond, Hybrid Bond, and Oneup Bond F Plus. No significant difference was found between any other of the groups and the reference adhesives. After 3 years of water storage and a third TC, only AQ Bond had a substantially lower MQ1 score (p < 0.05). Table 2 Criteria for the marginal analysis in the SEM Margin quality Definition 1 Margin not or hardly visible, no or slight marginal irregularities*; no gap 2 No gap but severe marginal irregularities* 3 Gap visible (hairline crack up to 2μm, no marginal irregularities* 4 Severe gap (more than 2μm), slight and severe marginal irregularities* * The term "marginal irregularities" refers to porosities, marginal restoration fracture, or bulge in the restoration Figure 2 shows the MQ1 results that were obtained for each product in dentin following each of the three TC treatments. Following the first TC (Fig 2a), no statistically significant differences were found for any of the groups. The TC after 1 year of water storage (Fig 2b) revealed a decrease in MQ1 for Prompt L-Pop in the 1999 version, Adper Prompt L- Pop/Tetric Ceram, and One-up Bond F Plus (p < 0.05). After three years of water storage and a 3rd TC both Prompt L-Pop (1999) and Adper Prompt L-Pop/Tetric Ceram were found to have substantially lower MQ1 scores than the reference groups (p < 0.05). Data for One-up Bond F Plus, G-Bond, AQ- Bond, Hybrid Bond, and tri-S Bond are missing for three years, as these materials were not available for the full duration of the present study. To better understand the dynamics of the results presented in Fig 2 and to obtain insights into the effects of TC and water storage, plots were produced of MQ1 for each group before and after TC at 21 days (T1 and T2), after 1 year of water storage (T3 and T4) and after 3 years of water storage (T5 and T6). Only the plots for the reference multi-bottle products are shown as examples in Fig 3. Each data point (T1-T6) represents the median MQ1 values with the corresponding error bars that are the standard error of the mean (SE). It must be emphasized that in these plots, the time intervals between the data points are not equal. The trends of the T1-T2, T2-T4, and T4-T6 segments were calculated in each graph, because the effects of water storage alone (segment T2-T3 after 1 year and segment T4-T5 after 2 additional years) were too small to be directly and reliably visualized. Thus, the purpose of TC was to challenge the bonds of the restorations in order to test the marginal integrity. Further analysis was then used to explore the joint effects of TC after the different water storage periods. The T1-T2, T2-T4, and T4-T6 slopes as well as the statistical significance (p) of the difference between each pair of the corresponding MQ1 values (obtained with the nonparametric Wilcoxon rank test) are presented in Table 3, columns A to F (shown as 1 st water storage [WS] vs 1 st TC, 1 st TC vs 2 nd TC, 2 nd TC vs 3 rd TC). We also calculated trends in the overall adhesive effectiveness by fitting linear regression lines (error Vol 9, Supplement 2, 2007 233
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