Ion release, antimicrobial and physio-mechanical properties of glass ionomer cement containing micro or nanosized hexametaphosphate, and their effect on enamel demineralization

  • Thayse Yumi Hosida
  • Alberto Carlos Botazzo Delbem
  • Leonardo Antônio Morais
  • João Carlos Silos Moraes
  • Cristiane Duque
  • José Antônio Santos Souza
  • Denise PedriniEmail author
Original Article



To evaluate the effects of hexametaphosphate microparticles (mHMP) or nanoparticles (nHMP) incorporated in glass ionomer cement (GIC) on antimicrobial and physico-mechanical properties, fluoride (F) release, and enamel demineralization.

Material and methods

HMP solutions were obtained at concentrations of 1, 3, 6, 9, and 12%, for screening of antimicrobial activity. Next, mHMP or nHMP at 6, 9, and 12% were incorporated into a resin-modified GIC and the antibacterial activity was evaluated. The resistance to diametral tensile and compressive strength, surface hardness, and degree of monomer conversion as well as F and HMP releases of GICs were determined. Furthermore, specimens were attached to enamel blocks and submitted to pH-cycling, and mineral loss was determined. Parametric and non-parametric tests were performed, after checking data homoscedasticity (p < 0.05).


HMP solutions at 6, 9, and 12% demonstrated the best antibacterial activity. GIC containing HMP showed better antibacterial effects at 9 and 12% for nHMP. Regarding F and HMP releases, the highest levels of release occurred for groups containing 9 and 12% nHMP. With the increase in HMP concentration, there was lower mineral loss. However, the incorporation of mHMP or nHMP in GIC reduced values of physico-mechanical properties when compared to the control GIC.


nHMP improves antimicrobial activity and fluoride release, and decreases enamel demineralization, but reduces the physico-mechanical properties of GIC.

Clinical relevance

The association of GIC/HMP could be an alternative material for patients at high risk for dental caries and could be indicated for low-stress regions or provisional restorations.


Glass ionomer cements Phosphates Nanoparticles Polymerization Compressive strength Antibacterial agents 



The authors acknowledge the financial support of the scholarship provided by the National Council of Technological and Scientific Development (CNPq 134267/2014-1) and wish to thank Dr. Emerson Rodrigues Camargo for his help in the synthesis of nanosized HMP.


The study was supported by the scholarship provided by the National Council of Technological and Scientific Development (CNPq 134267/2014-1).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Ethical approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed consent

This article does not contain any studies with human participants performed by any of the authors.


  1. 1.
    Bjørndal L, Larsen T (2000) Changes in the cultivable flora in deep carious lesions following a stepwise excavation procedure. Caries Res 34:502–508. CrossRefPubMedGoogle Scholar
  2. 2.
    Maltz M, Oliveira EF, Fontanella V, Carminatti G (2007) Deep caries lesions after incomplete dentine caries removal: 40-month follow-up study. Caries Res 41:493–496. CrossRefPubMedGoogle Scholar
  3. 3.
    Oliveira EF, Carminatti G, Fontanella V, Maltz M (2006) The monitoring of deep caries lesions after incomplete dentine caries removal: results after 14-18 months. Clin Oral Invest 10:134–139. CrossRefGoogle Scholar
  4. 4.
    Duque C, Negrini TC, Sacomo NT, Spolidorio DMP, Costa CAS, Hebling J (2009) Clinical and microbiological performance of resin-modified glass-ionomer liners after incomplete dentine caries removal. Clin Oral Invest 13:465–471. CrossRefGoogle Scholar
  5. 5.
    Weerheijm KL, Kreulen CM, de Soet JJ, Groen HJ, van Amerongen WE (1999) Bacterial counts in carious dentine under restorations: 2-year in vivo effects. Caries Res 33:130–134. CrossRefPubMedGoogle Scholar
  6. 6.
    Khoroushi M, Keshani F (2013) A review of glass-ionomers: from conventional glass-ionomer to bioactive glass-ionomer. Dent Res J (Isfahan) 10(4):411–420Google Scholar
  7. 7.
    Gruythuysen R, van Strijp G, Wu MK (2010) Long-term survival of indirect pulp treatment performed in primary and permanent teeth with clinically diagnosed deep carious lesions. J Endod 36:1490–1493. CrossRefPubMedGoogle Scholar
  8. 8.
    Preston AJ, Mair LH, Agalamanyi EA, Higham SM (1999) Fluoride release from aesthetic dental materials. J Oral Rehahil 26:123–129. CrossRefGoogle Scholar
  9. 9.
    Karantakis P, Helvatjoglou-Antoniades M, Theodoridou-Pahini S, Papadogiannis Y (2000) Fluoride release from three glass ionomers, a compomer, and a composite resin in water, artificial saliva, and lactic acid. Oper Dent 25:20–25PubMedGoogle Scholar
  10. 10.
    Tiveron ARF, Delbem ACB, Gaban G, Sassaki KT, Pedrini D (2013) Effect of resin composites with sodium trimetaphosphate with or without fluoride on hardness, ion release and enamel demineralization. Am J Dent 26:201–206PubMedGoogle Scholar
  11. 11.
    Barbour ME, Shellis RP, Parker DM, Allen GC, Addy M (2008) Inhibition of hydroxyapatite dissolution by whole casein: the effects of pH, protein concentration, calcium, and ionic strength. Eur J Oral 116:473–478. CrossRefGoogle Scholar
  12. 12.
    da Camara DM, Miyasaki ML, Danelon M, Sassaki KT, Delbem AC (2014) Effect of low-fluoride toothpastes combined with hexametaphosphate on in vitro enamel demineralization. J Dent 42:2562–2562. CrossRefGoogle Scholar
  13. 13.
    da Camara DM, Pessan JP, Francati TM, Souza JA, Danelon M, Delbem AC (2016) Fluoride toothpaste supplemented with sodium hexametaphosphate reduces enamel demineralization in vitro. Clin Oral Investig 20:1981–1985. CrossRefPubMedGoogle Scholar
  14. 14.
    de Castilho AR, Duque C, Negrini TC, Sacono NT, de Paula AB, de Souza Costa CA, Spolidório DM, Puppin-Rontani RM (2013) In vitro and in vivo investigation of the biological and mechanical behaviour of resin-modified glass-ionomer cement containing chlorhexidine. J Dent 41:155–163. CrossRefPubMedGoogle Scholar
  15. 15.
    Ferreira JM, Pinheiro SL, Sampaio FC, Menezes VA (2013) Use of glass ionomer cement containing antibiotics to seal off infected dentin: a randomized clinical trial. Braz Dent J 24:68–73 – 15. doi: CrossRefGoogle Scholar
  16. 16.
    Vaara M (1992) Agents that increase the permeability of the outer membrane. Microbiol Rev 56:395–411 - 13PubMedPubMedCentralGoogle Scholar
  17. 17.
    Xu HH, Weir MD, Sun L, Moreau JL, Takagi S, Chow LC, Antonucci JM (2010) Strong nanocomposites with Ca, PO(4), and F release for caries inhibition. J Dent Res 89:19–28–16. CrossRefPubMedPubMedCentralGoogle Scholar
  18. 18.
    Hook ER, Owen OJ, Bellis CA, Holder JA, O’Sullivan DJ, Barbour ME (2014) Development of a novel antimicrobial-releasing glass ionomer cement functionalized with chlorhexidine hexametaphosphate nanoparticle. J Nanobiotechnology 12:3. 17. CrossRefPubMedPubMedCentralGoogle Scholar
  19. 19.
    Bellis CA, Nobbs AH, O'Sullivan DJ, Holder JA, Barbour ME (2016) Glass ionomer cements functionalised with a concentrated paste of chlorhexidine hexametaphosphate provides dose-dependent chlorhexidine release over at least 14 months. J Dent 45:53–58. CrossRefPubMedGoogle Scholar
  20. 20.
    Duque C, Negrini TC, Hebling J, Spolidorio DM (2005) Inhibitory activity of glass-ionomer cements on cariogenic bacteria. Oper Dent 30:636–6340 19PubMedGoogle Scholar
  21. 21.
    Silva KG, Pedrini D, Delbem ACB, Cannon M (2007) Effect of pH variations in a cycling model on the properties of restorative materials. Oper Dent 32:328–335- 20. CrossRefPubMedGoogle Scholar
  22. 22.
    Fiske CH, Subbarow Y (1925) The colorimetric determination of phosphorus. J Biol Chem 66:375–400 - 21Google Scholar
  23. 23.
    Rodrigues E, Delbem ACB, Pedrini D, Oliveira MSR (2008) pH-cycling model to verify the efficacy of fluoride-releasing materials in enamel demineralization. Oper Dent 33:658–665. CrossRefPubMedGoogle Scholar
  24. 24.
    Vogel Vogel GL, Chow LC, Brown WE (1983) A microanalytical procedure for the determination of calcium, phosphate and fluoride in enamel biopsy samples. Caries Res 17:23–31CrossRefGoogle Scholar
  25. 25.
    Souza MDB, Pessan JP, Lodi CS, Souza JAS, Camargo ER, Souza Neto FN, Delbem ACB (2017) Toothpaste with nanosized trimetaphosphate reduces enamel demineralization. JDR Clin Trans Res. CrossRefGoogle Scholar
  26. 26.
    Kura G, Ohashi S, Kura S (1974) Complex formation of cyclic phosphate anions with bivalent cations. J Inorg Nucl Chem 36:1605–1609 -22CrossRefGoogle Scholar
  27. 27.
    Choi IK, Wen WW, Smith RW (1993) Technical note the effect of a long chain phosphate on the adsorption of collectors on kaolinite. Miner Eng 6:1191–1197 23CrossRefGoogle Scholar
  28. 28.
    Changgen L, Yongxin L (1983) Selective flotation of scheelite from calcium minerals with sodium oleate as a collector and phosphates as modifiers. II. The mechanism of the interaction between phosphate modifiers and minerals. Int J Miner Process 10:219–235 24CrossRefGoogle Scholar
  29. 29.
    Shibata H, Morioka T (1982) Antibacterial action of condensed phosphates on the bacterium Streptococcus mutans and experimental caries in the hamster. Arch Oral Biol 27:809–816 25CrossRefGoogle Scholar
  30. 30.
    Forss H, Jokinen J, Spets-Happonen S, Seppa L, Luoma H (1991) Fluoride and mutans streptococci in plaque grown on glass-ionomer and composite. Caries Res 25(454–458):26Google Scholar
  31. 31.
    Crisp S, Pringuer MA, Wardlerworth D, Wilson AD (1974) Reactions in glass ionomer cements: II. An infrared spectroscopic study J Dent Res 53:1414–1419 27CrossRefGoogle Scholar
  32. 32.
    da Camara DM, Pessan JP, Francati TM, Santos Souza JA, Danelon M, Delbem AC (2015) Synergistic effect of fluoride and sodium hexametaphosphate in toothpaste on enamel demineralization in situ. J Dent 43(10):1249–1254. CrossRefPubMedGoogle Scholar
  33. 33.
    van Dijk JW, Borggreven JM, Driessens FC (1980) The effect of some phosphates and a phosphonate on the electrochemical properties of bovine enamel. Arch Oral Biol 25:591–595Google Scholar
  34. 34.
    De Gee AJ (1999) Physical properties of glass-ionomer cements: setting shrinkage and wear. In: Davidson CL, Mjor IA (ed) Advances in glass-ionomer cements. Quintessence, Illinois, pp51–65 -29Google Scholar
  35. 35.
    Xie D, Chung ID, Wu W, Mays J (2004) Synthesis and evaluation of HEMA-free glass-ionomer cements for dental applications. Dent Mater 20:470–478 30. CrossRefPubMedGoogle Scholar
  36. 36.
    Xie D, Zhao J, Park JG (2007) A novel light-cured glass-ionomer system for improved dental restoratives. J Mater Sci Mater Med 18:1907–1916 31. CrossRefPubMedGoogle Scholar
  37. 37.
    Mobarak E, Elsayad I, Ibrahim M, El-Badrawy W (2009) Effect of LED light-curing on the relative hardness of tooth-colored restorative materials. Oper Dent 34:65–71. 32CrossRefPubMedGoogle Scholar
  38. 38.
    Cefaly DF, de Mello LL, Wang L, Lauris JR, D’Alpino PH (2009) Effect of light curing unit on resin-modified glass-ionomer cements: a microhardness assessment. J Appl Oral Sci 17(150–154):33–154. CrossRefGoogle Scholar
  39. 39.
    Khouw-Liu VH, Anstice HM, Pearson GJ (1999) An in vitro investigation of a poly (vinyl phosphonic acid) based cement with four conventional glass-ionomer cements. Part 1: Flexural strength and fluoride release. J Dent 27:351–357-28. CrossRefGoogle Scholar
  40. 40.
    Al Zraikat H, Palamara JE, Messer HH, Burrow MF, Reynolds EC (2011) The incorporation of casein phosphopeptide-amorphous calcium phosphate into a glass ionomer cement. Dent Mater 27:235–243 34. CrossRefPubMedGoogle Scholar
  41. 41.
    Dancey CP, Reidy J (2011) Statistics without maths for psychology. 5th edn. Pearson, London 620p. 35Google Scholar
  42. 42.
    Soh MS, Yap AU, Siow KS (2003) The effectiveness of cure of LED and halogen curing lights at varying cavity depths. Oper Dent 28(707–715):36Google Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Thayse Yumi Hosida
    • 1
  • Alberto Carlos Botazzo Delbem
    • 1
  • Leonardo Antônio Morais
    • 1
  • João Carlos Silos Moraes
    • 2
  • Cristiane Duque
    • 1
  • José Antônio Santos Souza
    • 1
  • Denise Pedrini
    • 3
    • 4
    Email author
  1. 1.Department of Pediatric Dentistry and Public HealthSchool of Dentistry, Araçatuba, São Paulo State University (UNESP)AraçatubaBrazil
  2. 2.Department of Physics and ChemistrySão Paulo State University (UNESP)Ilha SolteiraBrazil
  3. 3.Department of Surgery and Integrated ClinicSchool of Dentistry, Araçatuba, São Paulo State University (UNESP)AraçatubaBrazil
  4. 4.Disciplina de Clínica IntegradaFaculdade de Odontologia de Araçatuba – UNESPAraçatubaBrazil

Personalised recommendations