Dicalcium phosphate (CaHPO4·2H2O) precipitation through ortho- or meta-phosphoric acid-etching: effects on the durability and nanoleakage/ultra-morphology of resin-dentine interfaces

J Dent. 2013 Nov;41(11):1068-80. doi: 10.1016/j.jdent.2013.08.014. Epub 2013 Aug 29.

Abstract

Objectives: To compare the effects of two etching procedures using meta-phosphoric (MPA) or ortho-phosphoric acid (OPA) on dentine demineralisation, resin-dentine bonds durability and interface nanoleakage/ultra-morphology.

Methods: Middle-dentine specimens were etched using 37% OPA (15s) or 40% MPA (60s) and submitted to infrared spectroscopy (FTIR) or ultra-morphology dye-assisted (calcium-staining) confocal microscopy (Ca-CLSM). A three-step etch-and-rinse adhesive was formulated, applied onto dentine and light-cured for 30s before composite build-up. After 24h, the dentine-bonded specimens were cut into 1mm(2) beams; half were immediately submitted to microtensile bond strength (μTBS) and half stored in DW for six months. The μTBS results were analysed with repeated-measures ANOVA and Tukey's test (p<0.05). Further teeth were bonded and prepared for interface nanoleakage/ultra-morphology confocal evaluation.

Results: FTIR and Ca-CLSM analyses showed dicalcium phosphate dihydrate (Brushite) precipitation in MPA-etched dentine and on the bottom (front of demineralisation) of the OPA-etched dentine. Statistical analysis showed similar μTBS for both etching procedures after 24h. The μTBS of specimens in OPA-group dropped significantly (p<0.05) after six month; the specimens in the MPA group showed no statistically difference (p>0.05). CLSM depicted no evident sign of nanoleakage within the resin-dentine interface of the MPA-treated specimens, while the specimens in OPA-group presented intense nanoleakage and interface degradation.

Conclusion: The use of MPA (60s) as an alternative dentine conditioning agent in etch-and-rinse bonding procedures may be a suitable strategy to create more durable resin-dentine bonds.

Keywords: Bond durability; Calcium-staining technique; Confocal microscopy; Etch-and-rinse adhesives; FTIR vibration analysis; Meta-phosphoric acid; Resin–dentine interface ultra-morphology.

Publication types

  • Comparative Study
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acid Etching, Dental / methods*
  • Adult
  • Calcium Phosphates / chemistry*
  • Chemical Precipitation
  • Dental Bonding
  • Dental Leakage / classification*
  • Dental Stress Analysis / instrumentation
  • Dentin / ultrastructure*
  • Dentin-Bonding Agents / chemistry*
  • Fluorescein-5-isothiocyanate
  • Fluorescent Dyes
  • Humans
  • Light-Curing of Dental Adhesives / methods
  • Materials Testing
  • Methacrylates / chemistry
  • Microscopy, Confocal / methods
  • Phenols
  • Phosphoric Acids / chemistry*
  • Phosphorous Acids / chemistry*
  • Polyethylene Glycols / chemistry
  • Polymethacrylic Acids / chemistry
  • Spectroscopy, Fourier Transform Infrared
  • Stress, Mechanical
  • Sulfoxides
  • Surface Properties
  • Tensile Strength
  • Young Adult

Substances

  • Calcium Phosphates
  • Dentin-Bonding Agents
  • Fluorescent Dyes
  • Methacrylates
  • Phenols
  • Phosphoric Acids
  • Phosphorous Acids
  • Polymethacrylic Acids
  • Sulfoxides
  • triethylene glycol dimethacrylate
  • Polyethylene Glycols
  • ethoxylated bis-phenol A dimethacrylate
  • hydroxyethyl methacrylate
  • phosphoric acid
  • Fluorescein-5-isothiocyanate
  • metaphosphoric acid
  • calcium phosphate, dibasic, dihydrate
  • xylenol orange