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Effects of staining and bleaching on color change of dental composite resins Patricia Villalta, DDS, MS,a Huan Lu, DDS, PhD,b Zeynep Okte, DDS, PhD,c Franklin Garcia-Godoy, DDS, MS,d and John M. Powers, PhDe College of Dental Medicine, Nova Southeastern University, Fort Lauderdale, Fla; Department of Restorative Dentistry and Biomaterials, University of Texas Dental Branch at Houston, Tex; University of Ankara, Faculty of Dentistry, Ankara, Turkey Statement of problem. Discoloration of resin-based composites by colored solutions is a common problem. The use of bleaching agents for discolored natural teeth is becoming increasingly popular. It is not clear if bleaching agents can remove the stain from composite resins. Purpose. The purpose of this study was to investigate the effects of 2 staining solutions and 3 bleaching systems on the color changes of 2 dental composite resins. Material and methods. Forty-five disk-shaped specimens (9 3 2.5 mm) of each of 2 composite resins, Filtek Supreme (FS) and Esthet X (EX), were prepared. The specimens were then divided into 3 groups of 15 specimens each and immersed in 2 staining solutions (coffee or red wine) or distilled water (control) for 3 hours daily over a 40-day test period. The 3 groups were then divided into 3 subgroups (n=5), and 3 bleaching agents (Crest Night Effects, Colgate Simply White Night, or Opalescence Quick) were applied to the surface of the specimens over a 14-day period. Color of the specimens was measured with a spectrophotometer using CIELAB color space relative to CIE standard illuminant D55 at baseline, after staining, and after bleaching. The color differences (DEab*) between the 3 measurements were calculated. The value DEab*=3.3 was used as an acceptable value in subjective visual evaluations. Analysis of variance and nonparametric analysis (Kruskal-Wallis test and Mann-Whitney test) were used to analyze the data. Results. After staining, FS had more color change than EX and was more affected by the wine solution. After bleaching, the color of both EX and FS specimens returned to the baseline. The color differences between bleaching and baseline were less than value DEab*=3.3 for all groups. Conclusion. The nanocomposite (FS) changed color more than the microhybrid composite (EX) as a result of staining in coffee or red wine solutions. After bleaching, discoloration was removed completely from the composite resins tested. (J Prosthet Dent 2006;95:137-42.) CLINICAL IMPLICATIONS Red wine and coffee caused discoloration of the composite resins tested. Different concentrations of carbamide peroxide appear to have clinically similar effects in removing stain on the surface of shade A2 composite resins. C omposite resins have been widely used since their introduction because of their excellent esthetic properties. However, a major disadvantage is their discoloration after prolonged exposure to the oral environment. Unacceptable color match is a primary reason for replacement of composite resin restorations.1,2 a Assistant Professor, Bioscience Research Center, College of Dental Medicine, Nova Southeastern University. b Assistant Professor, Oral Biomaterials, Department of Restorative Dentistry and Biomaterials, University of Texas Dental Branch at Houston. c Associate Professor, Department of Pedodontics, University of Ankara, Faculty of Dentistry. d Associate Dean of Research; Director, Bioscience Research Center; Director, Clinical Research Center, Bioscience Research Center, College of Dental Medicine, Nova Southeastern University. e Professor and Director, Houston Biomaterials Research Center, University of Texas Dental Branch at Houston. FEBRUARY 2006 Composite resin restorative materials undergo a series of physical changes as a result of the polymerization reaction and the subsequent interaction with the wet oral environment.3 Following polymerization, the inward movement of water molecules causes mobilization of ions within the matrix and outward movement of unreacted monomers and ions leached from fillers and activators.4-6 Elution of leachable components contributes to further shrinkage and loss of weight, whereas hygroscopic absorption of water results in a swelling of material and an increase in weight.7 This process may cause softening of the resin matrix and reduction of stain resistance.8,9 Discoloration of tooth-colored resin-based materials may be caused by intrinsic and extrinsic factors. Intrinsic factors involve the discoloration of the resin material itself, such as the alteration of the resin matrix and the interface of matrix and fillers.2 The intrinsic color of THE JOURNAL OF PROSTHETIC DENTISTRY 137 THE JOURNAL OF PROSTHETIC DENTISTRY VILLALTA ET AL Table I. Resin composites and bleaching systems used Product Composite resins Filtek Supreme Esthet-X Bleaching agents Crest Night Effects Colgate Simply White Night Opalescence Quick Code Composition/type Lot No. FS EX Nanocomposite Microhybrid composite 3M ESPE, St. Paul, Minn Dentsply Caulk, Milford, Del 20040330 0410055 CNE CSWN OPAL 16% Carbamide peroxide 18% Carbamide peroxide 35% Carbamide peroxide Procter & Gamble, Cincinnati, Ohio Colgate-Palmolive, New York, NY Ultradent, South Jordan, Utah 30435614J0 P9809176 5J69 esthetic materials may change when materials are aged under various physical-chemical conditions such as thermal changes and humidity.10 Extrinsic factors such as adsorption or absorption of stains may also cause discoloration.11,12 The staining of resin-based materials by colored solutions such as coffee, tea, and other beverages,10-18 and color stability after aging in different solutions2,19-21 have been reported. Scotti et al21 simulated the oral condition by immersing specimens in synthetic saliva combined with coffee, tea, or chlorhexidine in a dark environment at 37°C, and concluded that synthetic saliva and coffee produced the greatest darkening and that the type of material also had a significant role on the stain resistance. Stober et al22 reported that red wine and coffee caused severe discoloration, with total color differences of DE.10 in all the tested composites. Um and Ruyter23 stated that discoloration by coffee was due to absorption of colorants by the tested materials. Iazzetti et al10 studied the color stability of 6 fluoridereleasing materials by immersing the specimens in coffee mixed with soluble tea and cranberry juice. The authors reported that the hydrophobic materials showed greater color stability and stain resistance than the hydrophilic materials. Lim et al20 evaluated the degree of color stability of glass ionomers and polyacid modified resin– based composites in various environmental solutions and found that glass ionomers and polyacid modified resin–based composites showed significant color changes in 0.1 mole acetic acid and 10% hydrogen peroxide solution. Since their introduction, the use of bleaching agents has become increasingly popular for whitening stained teeth.24-26 As these products contact tooth structures for extended periods of time, they may come into contact with dental materials.27 As discoloration of resinbased composites is a common problem, studies also investigated the effect of bleaching agents on toothcolored materials.28-37 Cooley and Burger28 evaluated composite resins for changes in surface hardness, roughness, and lightness after exposure to 10% carbamide peroxide gels and found that these 3 parameters increased significantly after exposure. Fay et al30 concluded that the 10% carbamide peroxide bleaching agent used in 138 Manufacturer the study removed stains from the composite resin and hybrid ionomer but was not effective in removing them from the compomer. Other studies compared the effect of carbamide versus hydrogen peroxide on composite resins. Cullen et al31 reported that 10% carbamide peroxide and 30% hydrogen peroxide had no significant effect on tensile strength of highly filled composite resins. However, microfilled composite resins were significantly affected by 30% hydrogen peroxide, resulting in a reduction in tensile strength. Canay and Cehreli34 showed that 10% hydrogen peroxide caused more color changes of composite resins compared with 10% carbamide peroxide, and the color change of all composite resins bleached with hydrogen peroxide solution was clinically detectable to the naked eye. New bleaching products continue to appear on the market that can be used effectively in bleaching human teeth.38-44 No study was identified that tested the effects of these products on stained composite resins. The aim of this study was to analyze the effects of 2 staining solutions and 3 bleaching agents on the color stability of 2 composite resins. MATERIAL AND METHODS The 2 composite resins and 3 bleaching agents used in this study are shown in Table I. An A2 color shade was selected for the 2 composite resins. Forty-five disk-shaped specimens from each material (90 specimens in total), 9 mm in diameter and 2.5 mm in depth, were prepared in polytetrafluoroethylene molds. The materials were handled according to the manufacturers’ instructions. A nylon thread was incorporated into the specimen so that the specimen could be suspended in the staining solutions. The mold with the composite resin was held between 2 glass slides, each covered with a transparent polyester strip (Mylar; Henry Schein, Melville, NY), and the microscope slides were gently pressed together to remove excess material. Specimens were polymerized by a conventional halogen lightpolymerizing unit (ESPE Elipar Trilight; 3M ESPE, St. Paul, Minn) with light intensity of 450 mW/cm2, using 40 seconds of exposure to top and bottom surfaces, respectively. The distance between the light VOLUME 95 NUMBER 2 VILLALTA ET AL THE JOURNAL OF PROSTHETIC DENTISTRY Table II. Mean values (SDs) of color change (DEab*) Coffee CSWN Esthet X Filtek Supreme STBL BBL BST STBL BBL BST 3.6 0.7 4.0 6.3 1.4 5.1 (0.3)* (0.5) (0.7)* (2.2)* (0.9) (1.5)* CNE 3.9 1.1 3.2 6.2 2.4 3.8 (0.4)* (0.5) (0.4) (0.5)* (0.4) (0.4)* Wine OPAL 4.1 1.4 5.2 6.5 1.0 5.7 (0.5)* (0.3) (0.8)* (0.9)* (0.5) (0.6)* CSWN 3.5 2.0 5.3 9.2 0.7 8.9 (0.5)* (0.7) (0.9)* (1.2)* (0.2) (1.2)* CNE 3.9 0.9 3.3 15.5 3.1 12.4 (0.8)* (0.6) (0.4)* (5.0)* (1.0) (5.0)* Water OPAL 4.3 2.3 6.4 11.5 2.1 10.1 (0.6)* (0.9) (1.4)* (5.2)* (1.8) (5.3)* CSWN 0.7 0.8 0.4 1.0 0.9 0.4 (0.3) (0.1) (0.2) (0.3) (0.3) (0.2) CNE 0.6 1.1 0.8 0.6 0.9 0.9 (0.2) (0.2) (0.5) (0.3) (0.6) (0.6) OPAL 1.0 1.3 0.6 1.1 0.6 0.8 (0.8) (1.0) (0.3) (0.3) (0.2) (0.2) STBL, Interval between staining and baseline; BBL, interval between bleaching and baseline; BST, interval between bleaching and staining; CSWN, Colgate Simply White Night; CNE, Crest Night Effects; OPAL, Opalescence Quick. * Indicates clincially unacceptable value (DEab*$3.3). source and specimen was standardized by the use of a 1-mm glass slide. The end of the light guide was in contact with the cover glass during the light-polymerization process. Afterward, all specimens were stored in distilled water for 24 hours at 37°C to ensure complete polymerization. The top surfaces of all specimens were then polished with fine and superfine polishing disks (Sof-lex; 3M ESPE) with a slow-speed handpiece. Color testing Color of the specimens was measured with a spectrophotometer (Color Eye 7000; GretagMacbeth LLC, New Windsor, NY) against a white background using CIELAB color space relative to CIE standard illuminant D55 at baseline, after staining, and after bleaching. The color differences (DEab*) between the 3 measurements were calculated as follows45: DEab  ¼ ½ðDL  Þ2 1 ðDa  Þ2 1 ðDb  Þ2 1=2 where L* is lightness, a* is green-red (2a*=green; 1a*= red), and b* is blue-yellow (2b*=blue; 1b*=yellow). A perceptible discoloration that is DEab*.1.0 will be referred to as acceptable up to the value DEab*=3.3 in subjective visual evaluations made in vitro under optimal lighting conditions.15,30 Staining process Forty-five specimens of each composite resin were separated into 3 groups (n=15). All specimens in each group were immersed in 1 of the 2 staining solutions (coffee or red wine) or distilled water (control) for 3 hours per day at room temperature over a 40-day test period. Solutions were changed daily. Coffee group specimens were immersed in vials containing 50 mL of freshly brewed regular coffee per vial (Auroma Paramount Coffee, Lansing, Mich); wine group specimens were immersed in vials containing 50 mL of red wine (Concha y Toro Frontera Cabernet Sauvignon 2002; Merlon, Chile); and control group specimens were immersed in distilled water. The vials were sealed with parafilm (Pechiney Plastic Packaging Inc, FEBRUARY 2006 Menasha, Wis) to prevent evaporation of the staining solution. After each staining period, the specimens were gently rinsed with distilled water, air dried, and stored in distilled water at 37°C. Bleaching process Three bleaching agents were used in this study (Table I). The 15 specimens in each staining group were further divided into 3 subgroups. Specimens in each subgroup (n=5) were bleached by one of the bleaching agents. The bleaching agents were painted on the top surface of the specimen according to the manufacturers’ instructions. All bleaching agents were applied at room temperature for 8 hours per day for 14 days to simulate the bleaching process. To be consistent with the other 2 paint-on products, Opalescence Quick was applied for a time period that far exceeded the manufacturer’s recommended time of no more than 2 hours per session. After bleaching, the specimens were rinsed with tap water for 1 minute to remove the bleaching agents, blotted dry, and stored in distilled water at 37°C. A limit of DEab*#3.3 was interpreted as a clinically acceptable difference in this study.46 One-way and 2way analysis of variance (ANOVA) tests were used to analyze the data if the normality and equal variance assumptions were met. Statistical software (SPSS 11.5 for Windows; SPSS Inc, Chicago, Ill) was used to perform the analysis. Fisher’s protected least significant difference (PLSD) intervals were calculated (a=.05) to compare the group mean values. If the data did not meet the assumptions for ANOVA, a nonparametric analysis (Kruskal-Wallis test and Mann-Whitney test) was used to analyze the data. RESULTS Mean values and SDs of DEab*s for intervals of staining and baseline, bleaching and baseline, and bleaching and staining are listed in Table II. After staining, FS and EX both had clinically significant discoloration (DEab*.3.3) for the coffee and wine groups, and FS 139 THE JOURNAL OF PROSTHETIC DENTISTRY VILLALTA ET AL Table III. One-way ANOVA of color change from baseline after staining for EX (control group included) Source Corrected model Intercept Stain Error Total Corrected total Type III Sum of squares df Mean square F P 98.083(a) 362.895 98.083 12.501 473.480 110.585 2 1 2 42 45 44 49.042 362.895 49.042 .298 64.761 1219.186 164.761 ,.001 ,.001 ,.001 P,.05 denotes statistically significant difference. Table IV. Two-way ANOVA of color change from baseline after bleaching for EX Source Corrected model Intercept Stain Bleach Stain 3 Bleach Error Total Corrected total Type III Sum of squares df Mean square F P 11.713(a) 74.061 4.379 3.262 4.072 12.987 98.761 24.700 8 1 2 2 4 36 45 44 1.464 74.061 2.189 1.631 1.018 .361 4.058 205.292 6.069 4.520 2.822 .002 ,.001 .005 .018 .039 P,.05 denotes statistically significant difference. was more affected by the wine solution. Overall, the control group (distilled water) had the least color change in the 3 intervals for both materials. After bleaching, the color of both EX and FS specimens returned to the baseline. The color differences between bleaching and baseline were less than 3.3 for all the groups. The data for EX met the equal variance assumption, and a 1-way ANOVA was performed for the color change after staining (Table III), while a 2-way ANOVA was used to analyze the color change after bleaching (Table IV). Fisher’s PLSD intervals (P=.05) for comparisons of mean values among the 3 stain solutions (including control group) was 0.20. The results of the statistical analysis showed that the staining solution had significant influence (P,.001) on the color change for EX specimens. There was no difference between coffee and wine groups, whereas these groups were significantly different (P,.05) from the control group. For the color change between bleaching and baseline, the staining solutions, bleaching agents, and interaction between the 2 variables all had significant influence (P,.05). Data for FS did not meet the equal variance requirement of ANOVA. For the color change after staining, the Kruskal-Wallis test showed that the stain solution had significant influence on the color change (P,.05) of the specimens; the Mann-Whitney test indicated that all 3 stain solutions (coffee, wine, and water) were significantly different from each other (P,.01) with respect to the color change of FS specimens. Wine had the most significant discoloration effect on FS, whereas the specimens in water showed the least color change. As there is no nonparametric equivalent of the 2-way 140 ANOVA, the data relating to color change after bleaching was not analyzed by a statistical method. The data showed that all 3 bleaching products had a clinically significant effect on the removal of stain from discolored FS specimens. The color differences between bleaching and baseline for all the groups were less than 3.3 (the clincially acceptable color change), even for the significantly discolored specimens in coffee or wine groups (Table II). DISCUSSION After staining, both composite resins tested had perceptible color changes (DEab* between 3.5 and 15.5). Low pH and alcohol may affect the surface integrity of composite resins and cause staining. These results are similar to those reported by Stober et al.22 The effect of staining solutions on color changes of composite resins was material dependent. This result is consistent with another study.11 The staining susceptibility of a material may be attributed to its resin or filler type. As purported by the manufacturer, Filtek Supreme (FS) is a nanocomposite with a primary 20-nm silica filler and loosely bonded cluster zirconia/silica particle size ranging from 0.6 to 1.4 mm. Its resin matrix is composed of Bis-GMA, UDMA, Bis-EMA, and TEGDMA. As purported by the manufacturer, Esthet X (EX) is a microhybrid composite containing BisGMA, BisEMA, and TEGDMA, and 0.6- to 0.8-mm-sized fillers. FS demonstrated more discoloration than EX for the 2 staining solutions, especially for the wine group. As FS and EX had different compositions, FS might absorb a staining VOLUME 95 NUMBER 2 VILLALTA ET AL substance such as coffee or red wine more easily than EX, as seen in other studies.17,18 It is interesting to note that the color of stained specimens returned to baseline after bleaching for all the groups tested even after a large discoloration due to staining, especially for the wine group of FS. The results of this study showed how effective the bleaching agents were in removing the exterior stainings for dental resin composites. Although the post hoc test showed that there were significant differences among the bleaching agents, the color differences between bleaching and baseline were acceptable clinically (DE,3.3). However, a limitation of this study is that no negative control was used during the bleaching stage, as the purpose of this study was to compare the effect of 3 commercial bleaching products. Thus, the study fails to prove that the stained specimens would not return to their original color with an innert paste. Therefore, the tentative conclusion of the study was that carbamide peroxide was responsible for removing stain from the surface of the specimens, and that the different concentrations of carbamide peroxide (16%, 18%, and 35% for Crest Night Effects, Colgate Simply White Night, and Opalescence Quick, respectively) had clinically similar effects on the color change of composite resins tested. When composite resins were immersed in water, the color differences were imperceptible and clinically acceptable. This observation confirms that water sorption by itself did not alter the color of composites to a considerable extent.16 The results after bleaching showed that bleaching did not affect the composite resins, even after 8 hours of application of Opalescence Quick over a period of 14 days. These results are consistent with previous studies for the low concentration of carbamide peroxide bleaching products,34-36 but not for the high concentrated bleaching agent.34,37 Monaghan et al37 and Canay and Cehreli34 reported perceptible color change for the composite resins bleached by 35% hydrogen peroxide and 10% hydrogen peroxide, respectively. This observation could be the reason for the disparities between that study and the present study, as other components in commercial products may contribute to the bleaching process as well.30 The bleaching mechanism for teeth is that the active agents (peroxide solutions) can flow freely through the enamel and dentin and oxidize the pigments in the teeth.24 The results of the present study indicated that the color change of composite resins after bleaching was probably due to superficial cleansing of the specimens, not intrinsic color change. Opalescence Quick is an in-office bleaching system with a recommended treatment time of no more than 2 hours. It was applied on the surface of specimens for 8 hours per day in this study to be consistent with the other 2 paint-on products tested. It appears that FEBRUARY 2006 THE JOURNAL OF PROSTHETIC DENTISTRY prolonged contact with composite resins did not increase the bleaching effect. Although bleaching agents can successfully remove the exterior staining from composite resins, they will not bleach them, whereas they can effectively bleach teeth.25,26 Therefore, after bleaching, the composite resin restoration may not match the surrounding bleached tooth structure. Also, bleaching can increase the surface roughness of composite resins; therefore, the restoration may stain more easily after bleaching.32,33 Bleaching agents should be used cautiously to remove the exterior stain on the surface of composite resin restorations. This study evaluated only A2 shades of both materials; thus, the results may not be applicable to other shades. CONCLUSIONS Different composite resins reacted differently in the 2 staining solutions. FS and EX specimens had clinically significant discoloration (DEab*.3.3) in both the coffee and wine solutions, and FS was more affected by the wine. 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Efficacy, side-effects and patients’ acceptance of different bleaching techniques (OTC, in-office, at-home). Oper Dent 2005;30:156-63. 45. Wyszecki G, Stiles WS, Wyszecki GN. Color science: concepts and methods, quantitative data and formulae. 2nd ed. New York: John Wiley; 1982. p. 166-9. 46. Ruyter IE, Nilner K, Möller B. Color stability of dental composite resin materials for crown and bridge veneers. Dent Mater 1987;3:246-51. Reprint requests to: DR PATRICIA VILLALTA BIOSCIENCE RESEARCH CENTER, COLLEGE NOVA SOUTHEASTERN UNIVERSITY 3200 SOUTH UNIVERSITY DRIVE FT LAUDERDALE, FL 33329 FAX: 945-262-1782 E-MAIL: pvillalt@nova.edu OF DENTAL MEDICINE 0022-3913/$32.00 Copyright Ó 2006 by The Editorial Council of The Journal of Prosthetic Dentistry. doi:10.1016/j.prosdent.2005.11.019 VOLUME 95 NUMBER 2