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Journal of Applied Oral Science

Print version ISSN 1678-7757On-line version ISSN 1678-7765

J. Appl. Oral Sci. vol.11 no.4 Bauru Oct./Dec. 2003 



Effect of tooth age on bond strength to dentin


Efeito da idade na resistência de união



Marcelo GianniniI; Patrícia ChavesII; Marcelo Tavares de OliveiraIII

IAssistant Professor, Department of Restorative Dentistry, Piracicaba Dental School, University of Campinas, Brazil
IIMaster Degree, Department of Restorative Dentistry, Piracicaba Dental School, University of Campinas, Brazil
IIIGraduate Student (Master Degree), Department of Restorative Dentistry, Piracicaba Dental School, University of Campinas, Brazil





This in vitro study evaluated the effect of tooth age on the tensile bond strength of Prime & Bond NT adhesive system to dentin. Human third molars from the five age groups were analyzed: A- 17 to 20yrs, B- 21 to 30yrs, C- 31 to 40yrs, D- 41 to 50yrs and E- 51 to 63yrs. The occlusal enamel was removed using a diamond saw under water cooling and the dentin surface was wet-ground with 600-grit SiC paper to obtain flat surfaces. The adhesive system was applied according to the manufacturer's instructions and a 6-mm high resin "crown" was built-up with resin composite. Teeth were stored for 24 hours in distilled water at 37oC and prepared for micro-tensile testing. Each specimen was mounted in a testing jig attached to a universal testing machine and stressed in tension at a crosshead speed of 0.5mm/min until failure. The means of tensile bond strength were (MPa): A- 21.42 ± 7.52a; B- 30.13 ± 10.19a; C- 31.69 ± 11.78a; D- 30.69 ± 8.47a and E- 35.66 ± 9.54a. No statistically significant difference was observed among the age groups (p > 0.05). The results suggested that the tensile bond strength of the adhesive system was not significantly affected by dentin aging.

Uniterms: Dentin; Tooth age; Adhesive system; Bond strength.


Este estudo avaliou, in vitro, o efeito da idade na resistência à tração do sistema adesivo Prime & Bond NT no substrato dentinário. Foram utilizados terceiros molares humanos de cinco faixas etárias: A- 17 a 20, B- 21 a 30, C- 31 a 40, D- 41 a 50 e E- 51 a 63. O esmalte oclusal foi removido utilizando disco de diamante e a superfície dentinária abrasionada e planificada com lixa de SiC (600) sob refrigeração. O sistema adesivo foi aplicado de acordo com as recomendações do fabricante e um bloco de resina composta de 6 mm de altura foi confeccionado na superfície dentinária. Os dentes foram armazenados em água por 24 horas a 37oC e preparados para o ensaio de micro-tração. Cada espécime foi fixado no dispositivo de micro-tração que estava acoplado a uma máquina universal de ensaio e testado numa velocidade de 0,5 mm/min. As médias de resistência à tração foram (MPa): A- 21,42 ± 7,52a; B- 30,13 ± 10,19a; C- 31,69 ± 11,78a; D- 30,69 ± 8,47a e E- 35,66 ± 9,54a. Nenhuma diferença significativa foi observada entre os grupos formados pelas faixas etárias (p > 0,05). Os resultados sugerem que a idade não altera significativamente a resistência de união do sistema adesivo à dentina.

Unitermos: Dentina; Idade; Sistema adesivo; Resistência de união.




Dentin is a hydrated biological composite structure composed of dentinal tubules, intertubular and peritubular matrices17,30. Each dentinal tubule is lined by peritubular dentin, which is characterized by a high mineral content. Intertubular dentin is found peripheral to the peritubular dentin separating the tubules, and its matrix contains 90 per cent type I collagen filled with apatite crystals3,17. Close to the pulp in newly erupted teeth, the dentin matrices are less mineralized and represent a small fraction of dentin area, whereas the tubules occupy a large area6,14.

The main age-related change in older teeth includes a gradual enlargement of the peritubular dentin and intratubular mineral deposits, which often result in narrowed or completely occluded tubules20,25. Dentin sclerosis increases in teeth that have been subjected to attrition, to oral exposure of the dentin, to caries or dental restorative procedures12,15,16,17. Moreover, alterations in the organic fractions of dentin such as acid mucopolysaccharides, which are more predominant in mature teeth, may be found in certain instances with increased mineralization17. Therefore, a normal distribution of structural units depends on the developmental stage of the teeth4,17,30.

Hybrid layer formation represents the main bonding mechanism of current dentin adhesives. This hybrid dentin-polymer structure is formed by impregnation of monomers into the demineralized intertubular dentin with subsequent polymerization. Resin infiltration into the dentinal tubules or resin tags also contributes to bonding. Studies show hybridization of the tubules' walls in the funnel-shaped portion, produced by acid etching28,29.

The dentinal structure undergoes histological and physiological alterations with aging or maturation in vital teeth4,12,17,20,25,26. Thus, permanent teeth of elderly patients may have different morphology and composition, which may affect the results of acid etching or infiltration of resin monomer. The purpose of this study was to investigate the influence of age changes on the tensile bond strength of a one-bottle total etch adhesive system to dentin. In addition, SEM investigated regional variations of etched dentin as a function of the age of teeth.



Twenty-five extracted sound erupted third molars stored in distilled water containing thymol crystals were used within 4 months of extraction. The teeth were obtained according to protocols (46/2000) approved by the appropriate institutional review board of the Piracicaba Dental School – University of Campinas, and with the informed consent of the donors.

Teeth were grouped according to the patient's age and divided into five groups (n = 5). The age groups were: 17 to 20yrs, 21 to 30yrs, 31 to 40yrs, 41 to 50yrs and 51 to 63yrs. The occlusal enamel of the teeth was removed by a section perpendicular to the long axis of the tooth using a low-speed diamond saw under water cooling (Buehler Ltd., Lake Bluff, IL, USA) to expose areas of mid-coronal dentin. The flat dentin surfaces were wet-polished with 600-grit silicon carbide paper.

The dentin surfaces were bonded with Prime & Bond NT adhesive system (Dentsply De Trey, Konstanz, Germany) according to the manufacturer's instructions. The composition and application steps are described in Table 1. After bonding, TPH Spectrum resin composite (Dentsply De Trey, Konstanz, Germany) was incrementally applied to build up a 6-mm high crown. Three increments were applied and each one was light cured for 40s with a light-curing unit (Degulux Soft-Start, Degussa Hüls AG, Hanau, Germany). The bonded teeth were then stored in water at 37oC.



After 24h, the teeth were serially sectioned into slabs with approximately 0.8 mm in thickness along the long axis of the tooth. Each slab was further vertically sectioned to produce some bonded sticks of approximately 0.7mm2. Sections were made through the composite buildups and dentin using a low-speed diamond saw under water cooling (Isomet 1000, Buehler Ltd., Lake Bluff, IL, USA.), according to the "non-trimming" technique developed by Shono, et al.24. Five specimens were tested for each tooth.

The specimens were individually affixed with cyanoacrylate cement to the grips of the testing device, which was placed in a universal testing machine (Model 4411, Instron Co., Canton, MA, USA.). The sticks were pulled to failure in tension at a crosshead speed of a 0.5mm/min. The load at failure divided by the cross-sectional area at the site of fracture for each specimen was used to calculate the tensile bond strength in MPa. Data were statistically analyzed by one-way ANOVA and individual bond strength values were correlated with the tooth age by linear regression. Statistical significance was established at a = 0.05.

The dentin side of failed specimens was lightly wet-abraded with 1000- and 2000-grit SiC paper to remove remnants of the adhesive agent, etched with 36% phosphoric acid for 15s and rinsed with water. For scanning electron microscopy (SEM), the samples were fixed in Karnovsky solution, post-fixed in osmium tetroxide solution, dehydrated in ascending alcohol concentrations, critical-point dried (CPD 030, Balzers, Balzer, Leichtenstein) and sputter-coated with gold (MED 010, Balzers, Balzer, Leichtenstein). Specimens were examined with a SEM (DSM 940A, Zeiss, Oberkochen, Germany), operated at 15 kV, and representative areas of the dentinal surfaces were photographed at 5,000 x and 10,000 x magnification.



The one-way ANOVA (Table 2) revealed no statistically significant difference on the tensile bond strength to dentin among the age groups (p = 0.248). The mean tensile bond strength values and standard deviations for the age groups are presented in Table 3. The lack of influence of patient's age on bonding to dentin was confirmed by the absence of significant correlation between tensile bond strength and aging (p = 0.162 and r = 0.335).





Illustrative SEM photomicrographs of etched dentin are presented in Figures 1 to 4. Acid etching opened the dentinal tubules and demineralized the intertubular and peritubular dentin for all age groups. In general, intertubular demineralization tended to decrease with aging. For younger teeth, the presence of intense exposed collagen fibrils after acid etching can be noted (Figures 1 and 2). Exposed outer peritubular collagen fibrils are shown in Figures 2 and 3. Figure 4 is a representative photomicrograph of old etched dentin. Some areas exhibit collagen fibrils embedded in mineral content due to a less aggressive or lower demineralizing effect of etching on the elderly groups.










The bonding mechanism of resin to dentin is dependent on the microstructure of the substrate at the site of bonding9,11,19,21,22. Since dentin is a dynamic substrate21, the quality of bonding has been analyzed as a function of aging. Studies have shown that the effectiveness in minimizing microleakage at the tooth-restoration interface, microgap formation and retention failures of dentin-bonded restorations can be influenced by dentin age8,13,23.

Regarding the effect of dentin aging on the bond strength, Nakajima, et al.18 showed much higher bond strength values to occlusal dentin of old molars than to young molars. The present findings confirm other reports on which similar tensile bond strengths to both young and old teeth were obtained for most adhesive systems2,27. In this study, although young teeth obtained lower bond strength means, no statistical differences were noted as well. The teeth used were free of caries and restorations; therefore, no natural alterations influenced the tensile bond strength of Prime & Bond NT.

Natural effects of physiological processes and microstructural changes in dentin as a function of tooth age include progressive deposition of peritubular dentin and tubule closure, which results in a significant reduction in the density of tubules and a decrease in dentin permeability4,12,26. Using earlier dentin bonding agents, studies have reported that the increased mineralization due to the aging phenomenon results in a less receptive or unfavorable substrate for bonding5,8. On the other hand, better dentin bond strength values were found in older teeth, due to the characteristics of collagen fibrils exposed on the dentin surface after acid etching18.

Scanning electron microscopic studies of natural aged surfaces of cervical sclerotic dentin lesions submitted to acid pre-etching revealed that acid etchants did not adequately etch the aged sclerotic dentin surfaces for mechanical retention of the adhesive systems. Acid etchants were unable to effectively demineralize intertubular dentin and dissolve mineral salts or sclerotic casts within the tubules. This less effective conditioning may compromise resin infiltration in aged dentin and consequently the long-term durability of the restoration5,10. In the present study, the smear layer and smear plugs were completely removed by the acid, and collagen fibrils could be seen along the surface of the intertubular dentine, since the dentinal surfaces used for bonding were from intact internal mid-coronal occlusal dentin.

The application of Prime & Bond NT requires previous etching with 36% phosphoric acid. Scanning electron microscopy showed that the intertubular demineralization tended to decrease with age, and that the collagen fibrils after acid-etching, seemed to be more exposed in young teeth, probably because dentin has not become highly mineralized yet. However, such characteristics of exposed collagen fibrils did not affect the tensile bond strength. Tay, et al.29 determined that a minimum pH value of 2.8 is required for the adhesive to effectively demineralize intact dentin within 30s. Thus, the acidity of this adhesive system (pH = 1.8) may be enough to promote a second demineralization of the underlying old dentin and allow a deep penetration of the resin monomer. This self-etching effect in highly mineralized zones may explain the fact that similar tensile bond strength values were obtained for the five age groups for Prime & Bond NT adhesive system, despite the effects of aging.

Among the multiple factors that can influence the effectiveness of dentin adhesives, age changes in teeth did not affect the resin-dentin bond strength. This becomes important because of the increased need for the restoration of elderly patients' teeth1,7, due to a growing proportion of the dentate adult population.



The authors are indebted to Dr. E. W. Kitajima (NAP-MEPA/ESALQ-USP) for technical electron microscopy support and to Laboratory of Dental Materials (FOP-UNICAMP). This study was supported by grant 0574/00 from the FAEP-PRP/UNICAMP, Brazil.



1- Beck JD, Hunt RJ. Oral health status in the United States: Problems of special patients. J Dental Educ 1985: 49(6): 407-26.         [ Links ]

2- Burrow MF, Takakura H,Nakajima, M, Inai, M, Tagami J, Takatsu T. The influence of age and depth of dentin on bonding. Dent Mater 1994: 10(4): 241-6.         [ Links ]

3- Butler WT. Dentin extracelular matrix and dentinogenesis. Oper Dent 1992: 5(Supplement): 18-23.         [ Links ]

4- Carrigan PJ, Morse DR, Furst ML., Sinai IH. A scanning electron microscopic evaluation of human dentinal tubules according to age and location. J Endod, 1984: 10(8): 359-63.         [ Links ]

5- Duke ES, Lindemuth J. Polymeric adhesion to dentin: Contrasting substrates. Amer J Dent 1990; 3(6): 2264-70.         [ Links ]

6- Garberoglio R, Brännström M. Scanning electron microscopic investigation of human dentinal tubules. Arch Oral Biol 1976: 21(6): 355-62.         [ Links ]

7- Hand JS, Hunt RJ, Beck JD. Incidence of coronal and root caries in an older adult population. J Public Health Dent, 1988: 48(1): 14-9.         [ Links ]

8- Heymann HO, Sturdevant JR, Brunson WD. Twelve-month clinical study of dentinal adhesives in class V cervical lesions. J Amer Dent Assoc 1988; 116(2):179-83.         [ Links ]

9- Heymann HO, Bayne SC. Current concepts in dentin bonding: focusing on dentinal adhesion factors. J Amer Dent Assoc 1993; 124(5):27-36.         [ Links ]

10- Kwong SM, Tay FR, Yip HK, Key LH, Pashley DH. An ultrastructural study of the application of dentine adhesives to acid-conditioned sclerotic dentin. J Dent 2000: 28(7): 515-28.         [ Links ]

11- Marshall GW, Marshall SJ, Kinney JH, Balooch M. The dentin substrate: structure and properties related to bonding. J Dent 1997; 25: 441-58.         [ Links ]

12- Mendis BR, Darling AI. Distribution with age and attrition of peritubular dentine in the crowns of human teeth. Arch Oral Biol 1979; 24(2): 131-9.         [ Links ]

13- Mixon JM, Richards ND, Mitchell RJ. Effects of dentin age and bonding on microgap formation. Amer J Dent 1993; 6(2): 72-6.         [ Links ]

14- Mjör IA.. Microradiography of human coronal dentine. Arch Oral Biol 1966; 11(2): 225-34.         [ Links ]

15- Mjör IA. Histologic studies of human coronal dentine following cavity preparations and exposure of ground facets in vivo. Arch Oral Biol 1967; 12(2): 247-63.         [ Links ]

16- Mjör IA. Histologic studies of human coronal dentine following the insertion of various materials in experimentally prepared cavities. Arch Oral Biol 1967; 12(4): 441-52.         [ Links ]

17- Mjör IA. Human coronal dentine: structure and reactions. Oral Surg Oral Med Oral Pathol 1972; 33(5): 810-23.         [ Links ]

18- Nakajima M, Takada T, Tagami J, Hosoda H. A study on bonding to dentin in various teeth and sites. Japan J Cons Dent 1991; 34(1): 266-74.         [ Links ]

19- Nakajima M, Sano H, Burrow MF, Tagami J, Yoshiyama M, Ebisu S, et al. Tensile bond strength and SEM evaluation of caries-affected dentin using dentin adhesives. J Dent Res 1995; 74(10): 1679-88.         [ Links ]

20- Nalbadian J, Gonzales,F, Sognnaes RR. Sclerotic age changes in root dentin of human teeth as observed by optical, electron and x-ray microscopy. J Dent Res, 1960; 39(3): 598-607.         [ Links ]

21- Pashley DH, Carvalho RM. Dentine permeability and dentine adhesion. J Dent, 1997; 25(5): 355-72.         [ Links ]

22- Pereira PNR, Okuda M, Sano H, Yoshikawa T, Burrow MF, Tagami J. Effect of intrinsic wetness and regional difference on dentin bond strength. Dent Mater, 1999; 15(1): 46-53.         [ Links ]

23- Sidhu SK, Soh G, Henderson LJ. Effect of dentin age on effectiveness of dentin bonding agents. Oper Dent 1991; 16(6): 218-22.         [ Links ]

24- Shono Y, Ogawa T, Terashita M, Carvalho RM, Pashley EL, Pashley DH. Regional measurement of resin-dentin bonding as an array. J Dent Res 1999; 78(2): 699-705.         [ Links ]

25- Stanley HR, Pereira JC, Spiegel E, Broom C, Schultz M. The detection and prevalence of reactive and physiologic sclerotic dentin, reparative dentin, and dead tracts beneath various types of dental lesions according to tooth surface and age. J Oral Pathol 1983; 12(4): 257-89.         [ Links ]

26- Tagami J, Hosoda H, Burrow MF, Nakajima M. Effect of aging and caries on dentin permeability. Proc Finn Dent Soc 1992: 88(Supplement1): 149-54.         [ Links ]

27- Tagami J, Nakajima M, Shono T, Takatsu T, Hosoda H. Effect of aging on dentin bonding. Amer J Dent 1993: 6(3): 145-7.         [ Links ]

28- Tay FR, Moulding KM, Pashley DH. Distribution of nanofillers from a simplified-step adhesive in acid-conditioned dentin. J Adhes Dent 1999: 1(2): 103-17.         [ Links ]

29- Tay FR, Sano H, Carvalho RM, Pashley EL, Pashley DH. An ultrastructural study of the influence of acidity of self-etching primers and smear layer thickness on bonding to intact dentin. J Adhes Dent 2000: 2(2): 83-98.         [ Links ]

30- Tronstad L. Ultrastructural observations on human coronal dentin. Scand J Dent Res 1973; 81(2):101-11.         [ Links ]



Correspondence to
Marcelo Giannini
Faculdade de Odontologia de Piracicaba – UNICAMP
Área de Dentística – Departamento de Odontologia Restauradora
Av. Limeira, 901 – Areião – Piracicaba – SP CEP 13414-018
e- mail:
Fone: 19-34125340 Fax: 19-34125218

Recebido para publicação em: 12/06/2003
Enviado para reformulações em: 09/09/2003
Pronto para publicação em: 21/10/2002

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