Extrafibrillar collagen demineralization-based chelate-and-rinse technique bridges the gap between wet and dry dentin bonding

Sui Mai, Chin Chuan Wei, Li sha Gu, Fucong Tian, Dwayne D. Arola, Ji hua Chen, Yang Jiao, David Henry Pashley, Li na Niu, Franklin Chi Meng Tay

Research output: Contribution to journalArticle

6 Citations (Scopus)

Abstract

Limitations associated with wet-bonding led to the recent development of a selective demineralization strategy in which dentin was etched with a reduced concentration of phosphoric acid to create exclusive extrafibrillar demineralization of the collagen matrix. However, the use of acidic conditioners removes calcium via diffusion of very small hydronium ions into the intrafibrillar collagen water compartments. This defeats the purpose of limiting the conditioner to the extrafibrillar space to create a collagen matrix containing only intrafibrillar minerals to prevent collapse of the collagen matrix. The present work examined the use of polymeric chelators (the sodium salt of polyacrylic acid) of different molecular weights to selectively demineralize extrafibrillar dentin. These polymeric chelators exhibit different affinities for calcium ions (isothermal titration calorimetry), penetrated intrafibrillar dentin collagen to different extents based on their molecular sizes (modified size-exclusion chromatography), and preserve the dynamic mechanical properties of mineralized dentin more favorably compared with completely demineralized phosphoric acid-etched dentin (nanoscopical dynamic mechanical analysis). Scanning and transmission electron microscopy provided evidence for retention of intrafibrillar minerals in dentin surfaces conditioned with polymeric chelators. Microtensile bond strengths to wet-bonded and dry-bonded dentin conditioned with these polymeric chelators showed that the use of sodium salts of polyacrylic acid for chelating dentin prior to bonding did not result in significant decline in resin-dentin bond strength. Taken together, the findings led to the conclusion that a chelate-and-rinse conditioning technique based on extrafibrillar collagen demineralization bridges the gap between wet and dry dentin bonding. Statement of Significance The chelate-and-rinse dental adhesive bonding concept differentiates from previous research in that it is based on the size-exclusion characteristics of fibrillar collagen; molecules larger than 40 kDa are prevented from accessing the intrafibrillar water compartments of the collagen fibrils. Using this chelate-and-rinse extrafibrillar calcium chelation concept, collagen fibrils with retained intrafibrillar minerals will not collapse upon air-drying. This enables adhesive infiltration into the mineral-depleted extrafibrillar spaces without relying on wet-bonding. By bridging the gap between wet and dry dentine bonding, the chelate-and-rinse concept introduces additional insight to the field by preventing exposure of endogenous proteases via preservation of the intrafibrillar minerals within a collagen matrix. If successfully validated, this should help prevent degradation of resin-dentine bonds by collagenolytic enzymes.

Original languageEnglish (US)
Pages (from-to)435-448
Number of pages14
JournalActa biomaterialia
Volume57
DOIs
StatePublished - Jul 15 2017

Fingerprint

Dentin
Collagen
carbopol 940
Minerals
Chelating Agents
Calcium
Chelation
Phosphoric acid
Resins
Salts
Sodium
Adhesives
Fibrillar Collagens
Dental Cements
Dental Bonding
Size exclusion chromatography
Water
Calorimetry
Dynamic mechanical analysis
Acids

Keywords

  • Bonding
  • Chelation
  • Dentin
  • Extrafibrillar
  • Intrafibrillar
  • Size-exclusion

ASJC Scopus subject areas

  • Biotechnology
  • Biomaterials
  • Biochemistry
  • Biomedical Engineering
  • Molecular Biology

Cite this

Extrafibrillar collagen demineralization-based chelate-and-rinse technique bridges the gap between wet and dry dentin bonding. / Mai, Sui; Wei, Chin Chuan; Gu, Li sha; Tian, Fucong; Arola, Dwayne D.; Chen, Ji hua; Jiao, Yang; Pashley, David Henry; Niu, Li na; Tay, Franklin Chi Meng.

In: Acta biomaterialia, Vol. 57, 15.07.2017, p. 435-448.

Research output: Contribution to journalArticle

Mai, Sui ; Wei, Chin Chuan ; Gu, Li sha ; Tian, Fucong ; Arola, Dwayne D. ; Chen, Ji hua ; Jiao, Yang ; Pashley, David Henry ; Niu, Li na ; Tay, Franklin Chi Meng. / Extrafibrillar collagen demineralization-based chelate-and-rinse technique bridges the gap between wet and dry dentin bonding. In: Acta biomaterialia. 2017 ; Vol. 57. pp. 435-448.
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abstract = "Limitations associated with wet-bonding led to the recent development of a selective demineralization strategy in which dentin was etched with a reduced concentration of phosphoric acid to create exclusive extrafibrillar demineralization of the collagen matrix. However, the use of acidic conditioners removes calcium via diffusion of very small hydronium ions into the intrafibrillar collagen water compartments. This defeats the purpose of limiting the conditioner to the extrafibrillar space to create a collagen matrix containing only intrafibrillar minerals to prevent collapse of the collagen matrix. The present work examined the use of polymeric chelators (the sodium salt of polyacrylic acid) of different molecular weights to selectively demineralize extrafibrillar dentin. These polymeric chelators exhibit different affinities for calcium ions (isothermal titration calorimetry), penetrated intrafibrillar dentin collagen to different extents based on their molecular sizes (modified size-exclusion chromatography), and preserve the dynamic mechanical properties of mineralized dentin more favorably compared with completely demineralized phosphoric acid-etched dentin (nanoscopical dynamic mechanical analysis). Scanning and transmission electron microscopy provided evidence for retention of intrafibrillar minerals in dentin surfaces conditioned with polymeric chelators. Microtensile bond strengths to wet-bonded and dry-bonded dentin conditioned with these polymeric chelators showed that the use of sodium salts of polyacrylic acid for chelating dentin prior to bonding did not result in significant decline in resin-dentin bond strength. Taken together, the findings led to the conclusion that a chelate-and-rinse conditioning technique based on extrafibrillar collagen demineralization bridges the gap between wet and dry dentin bonding. Statement of Significance The chelate-and-rinse dental adhesive bonding concept differentiates from previous research in that it is based on the size-exclusion characteristics of fibrillar collagen; molecules larger than 40 kDa are prevented from accessing the intrafibrillar water compartments of the collagen fibrils. Using this chelate-and-rinse extrafibrillar calcium chelation concept, collagen fibrils with retained intrafibrillar minerals will not collapse upon air-drying. This enables adhesive infiltration into the mineral-depleted extrafibrillar spaces without relying on wet-bonding. By bridging the gap between wet and dry dentine bonding, the chelate-and-rinse concept introduces additional insight to the field by preventing exposure of endogenous proteases via preservation of the intrafibrillar minerals within a collagen matrix. If successfully validated, this should help prevent degradation of resin-dentine bonds by collagenolytic enzymes.",
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author = "Sui Mai and Wei, {Chin Chuan} and Gu, {Li sha} and Fucong Tian and Arola, {Dwayne D.} and Chen, {Ji hua} and Yang Jiao and Pashley, {David Henry} and Niu, {Li na} and Tay, {Franklin Chi Meng}",
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AU - Mai, Sui

AU - Wei, Chin Chuan

AU - Gu, Li sha

AU - Tian, Fucong

AU - Arola, Dwayne D.

AU - Chen, Ji hua

AU - Jiao, Yang

AU - Pashley, David Henry

AU - Niu, Li na

AU - Tay, Franklin Chi Meng

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N2 - Limitations associated with wet-bonding led to the recent development of a selective demineralization strategy in which dentin was etched with a reduced concentration of phosphoric acid to create exclusive extrafibrillar demineralization of the collagen matrix. However, the use of acidic conditioners removes calcium via diffusion of very small hydronium ions into the intrafibrillar collagen water compartments. This defeats the purpose of limiting the conditioner to the extrafibrillar space to create a collagen matrix containing only intrafibrillar minerals to prevent collapse of the collagen matrix. The present work examined the use of polymeric chelators (the sodium salt of polyacrylic acid) of different molecular weights to selectively demineralize extrafibrillar dentin. These polymeric chelators exhibit different affinities for calcium ions (isothermal titration calorimetry), penetrated intrafibrillar dentin collagen to different extents based on their molecular sizes (modified size-exclusion chromatography), and preserve the dynamic mechanical properties of mineralized dentin more favorably compared with completely demineralized phosphoric acid-etched dentin (nanoscopical dynamic mechanical analysis). Scanning and transmission electron microscopy provided evidence for retention of intrafibrillar minerals in dentin surfaces conditioned with polymeric chelators. Microtensile bond strengths to wet-bonded and dry-bonded dentin conditioned with these polymeric chelators showed that the use of sodium salts of polyacrylic acid for chelating dentin prior to bonding did not result in significant decline in resin-dentin bond strength. Taken together, the findings led to the conclusion that a chelate-and-rinse conditioning technique based on extrafibrillar collagen demineralization bridges the gap between wet and dry dentin bonding. Statement of Significance The chelate-and-rinse dental adhesive bonding concept differentiates from previous research in that it is based on the size-exclusion characteristics of fibrillar collagen; molecules larger than 40 kDa are prevented from accessing the intrafibrillar water compartments of the collagen fibrils. Using this chelate-and-rinse extrafibrillar calcium chelation concept, collagen fibrils with retained intrafibrillar minerals will not collapse upon air-drying. This enables adhesive infiltration into the mineral-depleted extrafibrillar spaces without relying on wet-bonding. By bridging the gap between wet and dry dentine bonding, the chelate-and-rinse concept introduces additional insight to the field by preventing exposure of endogenous proteases via preservation of the intrafibrillar minerals within a collagen matrix. If successfully validated, this should help prevent degradation of resin-dentine bonds by collagenolytic enzymes.

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