Effect of graphene-based intracanal medicament on push-out bond strength of different endodontic sealers in root canal dentin – an in vitro study
DOI:
https://doi.org/10.2340/biid.v13.46558Keywords:
graphene oxide, silver nanoparticles, allicin, intracanal medicament, push-out bond strength, endodontic sealer, root canal dentinAbstract
Introduction: Graphene-based hydrogels incorporating antimicrobial agents, such as allicin and silver nanoparticles, offer potential therapeutic benefits. This study aimed to evaluate the effect of an allicin-incorporated graphene oxide–silver nanoparticle hydrogel on the push-out bond strength of endodontic sealers and the influence of different removal protocols.
Materials and methods: A total of 60 extracted human single-rooted teeth were prepared to F3 size protaper and irrigated with 3% sodium hypochlorite and 17% Ethylenediaminetetraacetic Acid (EDTA) The experimental hydrogel (allicin + graphene oxide + silver nanoparticles in 2% sodium alginate base) was placed in all canals and incubated for 7 days. Specimens were randomised by sealer type (AH Plus, Mineral Trioxide Aggregate (MTA) Fillapex, Sealapex) and removal protocol: syringe irrigation, passive ultrasonic irrigation (PUI), or XP-Endo Finisher activation. Push-out bond strength was measured using a universal testing machine. A subset of specimens (n = 3 per protocol) underwent Scanning Electron Microscopy (SEM)/Energy Dispersive X-ray Spectroscopy (EDX) analysis to evaluate residual medicament. Data were statistically analysed.
Results: Push-out bond strength was significantly influenced by both sealer type and removal protocol (p < 0.05). AH Plus exhibited the highest bond strength (mean ± standard deviation [SD]: 5.2 ± 1.4 MPa), followed by Sealapex (1.9 ± 0.3 MPa) and MTA Fillapex (1.5 ± 0.4 MPa). Activation-assisted protocols (PUI: 4.8 ± 1.2 MPa; XP-Endo Finisher: 5.0 ± 1.3 MPa) significantly increased bond strength compared to syringe irrigation alone (3.1 ± 1.0 MPa; p < 0.05). SEM/EDX analysis revealed minimal residual hydrogel after activation, without adversely affecting sealer adhesion. Bond strength was highest in the cervical third and lowest in the apical third (p < 0.05).
Conclusion: The allicin-incorporated graphene oxide–silver nanoparticle hydrogel did not compromise the push-out bond strength of the evaluated endodontic sealers when appropriate medicament removal protocols were employed. PUI and XP-Endo Finisher activation effectively facilitated hydrogel removal and maintained sealer adhesion, supporting the potential use of this material as an intracanal medicament.
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References
Gomes BPFA, Aveiro E, Kishen A. Irrigants and irrigation activation systems in endodontics. Braz Dent J. 2023;34(4):1–33. DOI: https://doi.org/10.1590/0103-6440202305577
Viapiana R, Guerreiro-Tanomaru J, Tanomaru-Filho M, Camilleri J. Interface of dentine to root canal sealers. J Dent. 2014;42(3):336–50. DOI: https://doi.org/10.1016/j.jdent.2013.11.013
Alhajj MN, Daud F, Al‐Maweri SA, Johari Y, Ab‐Ghani Z, Jaafar M, et al. Effects of calcium hydroxide intracanal medicament on push‐out bond strength of endodontic sealers: a systematic review and meta‐analysis. J Esthet Restor Dent. 2022;34(8):1166–78. DOI: https://doi.org/10.1111/jerd.12974
Maan S, Bhatt V, Singh R, Gupta S, Noorain S, Gill A, et al. The effect of four different intracanal medicaments on the push-out bond strength of root canal sealers. J Med Life. 2022;15:448–53. DOI: https://doi.org/10.25122/jml-2020-0104
Ordinola‐Zapata R, Noblett WC, Perez‐Ron A, Ye Z, Vera J. Present status and future directions of intracanal medicaments. Int Endod J. 2022;55(Suppl. 3):613–36. DOI: https://doi.org/10.1111/iej.13731
Zou X, Zheng X, Liang Y, Zhang C, Fan B, Liang J, et al. Expert consensus on irrigation and intracanal medication in root canal therapy. Int J Oral Sci. 2024;16(1):23. DOI: https://doi.org/10.1038/s41368-024-00280-5
Kim D, Kim E. Antimicrobial effect of calcium hydroxide as an intracanal medicament in root canal treatment: a literature review – Part II. in vivo studies. Restor Dent Endod. 2015;40(2):97. DOI: https://doi.org/10.5395/rde.2015.40.2.97
Amin S, Seyam R, El-Samman M. The effect of prior calcium hydroxide intracanal placement on the bond strength of two calcium silicate-based and an epoxy resin-based endodontic sealer. J Endod. 2012;38:696–9. DOI: https://doi.org/10.1016/j.joen.2012.02.007
Bhatt S, Pathak R, Punetha VD, Punetha M. Recent advances and mechanism of antimicrobial efficacy of graphene-based materials: a review. J Mater Sci. 2023;58(19):7839–67. DOI: https://doi.org/10.1007/s10853-023-08534-z
Eskandari F, Abbaszadegan A, Gholami A, Ghahramani Y. The antimicrobial efficacy of graphene oxide, double antibiotic paste, and their combination against Enterococcus faecalis in the root canal treatment. BMC Oral Health. 2023;23(1):20. DOI: https://doi.org/10.1186/s12903-023-02718-4
Karobari M, Lakshmi D, Adil A, Arshad S, Devaraj E, Mallineni S, et al. Antimicrobial properties of silver nitrate nanoparticle and its application in endodontics and dentistry: a review of literature. J Nanomater. 2021;2021:12. DOI: https://doi.org/10.1155/2021/9132714
Rathna P, Ranjan M, Sherwood A, Mishra P, Ranganathan P, Shalini H. Development and characterization of allicin-incorporated graphene oxide–silver nanoparticle hydrogels as a potential intracanal medicament: an in vitro study. World J Dent. 2025;16(5):427–34. DOI: https://doi.org/10.5005/jp-journals-10015-2560
Cao M, Wu D, Tu H, Mou B, Kang J, Liao J, et al. Injectable hydrogel as intracanal medication for root canal disinfection. J Dent Res. 2025;104(5):503–12. DOI: https://doi.org/10.1177/00220345241309865
Usta SN, Erdem BA, Gündoğar M. Comparison of the removal of intracanal medicaments used in regenerative endodontics from root canal system using needle, ultrasonic, sonic, and laser-activated irrigation systems. Lasers Med Sci. 2024;39(1):27. DOI: https://doi.org/10.1007/s10103-024-03980-w
Neelakantan P, Sriraman P, Gutmann JL. Removal of calcium hydroxide intracanal medicament by different irrigants and irrigating techniques: a cone beam computed tomography analysis. Gen Dent. 2017;65(6):45–9.
Seracchiani M, Miccoli G, Reda R, Bhandi S, Gambarini G, Testarelli L, et al. A comprehensive in vitro comparison of mechanical properties of two rotary endodontic instruments. World J Dent. 2020;11(3):185–8. DOI: https://doi.org/10.5005/jp-journals-10015-1729
Guiotti FA, Kuga MC, Duarte MAH, Sant’Anna Júnior A, Faria G. Effect of calcium hydroxide dressing on push-out bond strength of endodontic sealers to root canal dentin. Braz Oral Res. 2014;28(1):1–6. DOI: https://doi.org/10.1590/S1806-83242014.50000002
Li X, Yu B, Chen J, Huo D, Liu J, Nan D. Optimized functionalization of graphene oxide for enhanced mechanical properties in epoxy resin composites. Coatings. 2024;14:609. DOI: https://doi.org/10.3390/coatings14050609
Vinola SM, Mahalaxmi S. Characterisation and evaluation of physical properties of AH-Plus sealer with and without the incorporation of petasin, pachymic acid, curcumin and shilajit – an in vitro study. BMC Oral Health. 2024;24:352. DOI: https://doi.org/10.1186/s12903-024-04108-w
AlFawaz Y, Almutairi B, Kattan H, Zafar M, Farooq I, Naseem M, et al. Dentin bond integrity of hydroxyapatite containing resin adhesive enhanced with graphene oxide nano-particles – an SEM, EDX, micro-raman, and microtensile bond strength study. Polymers. 2020;12:2978. DOI: https://doi.org/10.3390/polym12122978
Srimaneepong V, Skallevold HE, Khurshid Z, Zafar MS, Rokaya D, Sapkota J. Graphene for antimicrobial and coating application. Int J Mol Sci. 2022;23(1):499. DOI: https://doi.org/10.3390/ijms23010499
Ahmed HA, Sadek HS, Morsy DA. Effect of nano-silver gel and calcium hydroxide paste on the bond strength of epoxy-resin based sealer to root canal dentin in anterior teeth: an in vitro study. Int J Appl Dent Sci. 2023;9(2):1–10. DOI: https://doi.org/10.22271/oral.2023.v9.i2a.1703
Piriyanga R, Ranjan M, Sherwood A, Fareed M, Karobari MI. Effect of allicin-incorporated graphene oxide hydrogel on dentin microhardness. BMC Oral Health. 2025;25(1):461. DOI: https://doi.org/10.1186/s12903-025-05870-1
Nadeem MS, Kazmi I, Ullah I, Muhammad K, Anwar F. Allicin, an antioxidant and neuroprotective agent, ameliorates cognitive impairment. Antioxidants (Basel). 2021;11(1):87. DOI: https://doi.org/10.3390/antiox11010087
Donnermeyer D, Dornseifer P, Schäfer E, Dammaschke T. The push-out bond strength of calcium silicate-based endodontic sealers. Head Face Med. 2018;14:13. DOI: https://doi.org/10.1186/s13005-018-0170-8
Fan J, Shi Z, Lian M, Li H, Yin J. Mechanically strong graphene oxide/sodium alginate/polyacrylamide nanocomposite hydrogel with improved dye adsorption capacity. J Mater Chem A. 2013;1(25):7433–43. DOI: https://doi.org/10.1039/c3ta10639j
An J, Zhang Y, Zhang X, He M, Zhou J, Zhou J, et al. Structure and properties of epoxy resin/graphene oxide composites prepared from silicon dioxide-modified graphene oxide. ACS Omega. 2024;9(15):17577–91. DOI: https://doi.org/10.1021/acsomega.4c00707
Zanza A, Reda R, Vannettelli E, Donfrancesco O, Relucenti M, Bhandi S, et al. The influence of thermomechanical compaction on the marginal adaptation of 4 different hydraulic sealers: a comparative ex vivo study. J Comp Sci. 2023;7(1):10. DOI: https://doi.org/10.3390/jcs7010010
Chou K, George R, Walsh LJ. Effectiveness of different intracanal irrigation techniques in removing intracanal paste medicaments. Aust Endod J. 2014;40(1):21–5. DOI: https://doi.org/10.1111/aej.12055
Kurup D, Nagpal AK, Shetty S, Mandal TK, Anand J, Mitra R. Data on the push–out bond strength of three different root canal treatment sealers. Bioinformation. 2021;17(1):67–72. DOI: https://doi.org/10.6026/97320630017067
Sevagaperumal A, Lakshmi MKG, Piriyanga RSR, Priyadharshini SS, Abirami AA, Sherwood IA. Comparing the antimicrobial properties of graphene oxide silver nanoparticles as a root canal irrigant: a randomized controlled trial. Endodontology. 2024;36(1):16–24. DOI: https://doi.org/10.4103/endo.endo_35_23
Barbosa MDA, Antunes LS, Meyfarth SRS, Tomazinho FSF, Gabardo MCL, Antunes LAA. Does calcium hydroxide interfere with root canal sealer penetration in dentinal tubules? A systematic review and meta-analysis. J Evid Based Dent Pract. 2025;25(3):102046. DOI: https://doi.org/10.1016/j.jebdp.2024.102046
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