Method Article

Evaluation of Bond Strength Between Premixed and Powder-Liquid Mineral Trioxide Aggregate and Various Glass Ionomer Cements: An In Vitro Study

DOI:

10.3791/69053

⸱

October 10th, 2025

 ,  ,  , 
1Department of Endodontics, Faculty of Dentistry, Marmara University

In This Article

Summary

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Here, we present an in vitro study evaluating the short-term bond strength between two formulations of mineral trioxide aggregate (powder-liquid and premixed) and two types of glass ionomer cements (conventional and resin-modified).

Abstract

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This study aims to comparatively evaluate the bond strengths of premixed and powder-liquid forms of mineral trioxide aggregate (MTA) to conventional glass ionomer cement (CGIC) and resin-modified glass ionomer cement (RMGIC).

Sixty test specimens were prepared and divided into four groups (n = 15) based on the combinations of MTA type and glass ionomer cement used. Following MTA placement and a standardized 15 min setting period, the glass ionomer materials were applied according to the manufacturers' instructions. Shear bond strength testing was performed using a universal testing machine, and failure modes were analyzed under a stereomicroscope.

The powder-liquid MTA combined with RMGIC exhibited the highest bond strength (p < 0.001). RMGIC showed significantly higher bond strength than CGIC for both MTA forms. A statistically significant difference in failure mode distribution was observed in the premixed MTA group (p = 0.020).

The findings demonstrate that both the physical form of MTA and the chemical composition of the ionomer cement significantly affect bond strength. Moreover, the distribution of failure modes differed across groups: cohesive failures predominated in the premixed MTA-RMGIC group, whereas mixed and adhesive failures were more common with CGIC. These results suggest that the powder-liquid MTA combined with RMGIC provides the most reliable adhesion and may be preferable in clinical scenarios requiring durable bonding.

Introduction

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Vital pulp therapy (VPT) is a therapeutic intervention aimed at preserving the structural integrity of compromised pulp tissue, typically due to factors such as carious lesions or traumatic injuries. VPT has become a cornerstone of contemporary endodontics due to its ability to preserve healthy pulp tissue by supporting the body's intrinsic healing and repair mechanisms. These therapeutic interventions are predicated on the inherent cellular repair mechanisms of the pulp1,2. Consequently, the utilization of dental materials in this setting is predicated on the promotion of hard tissue formation by residual pulp cells, the sealing of exposed areas, and the cultivation of an environment conducive to the preservation of pulpal vitality. Therefore, materials utilized in VPT are required to adhere to fundamental biological principles, including biocompatibility and bioactivity. Furthermore, it is imperative that they promote the proliferation of dental pulp stem cells and expedite pulpal healing3.

Mineral trioxide aggregate (MTA) is a preferred material in VPT due to its comprehensive biological properties4,5,6,7. Research has demonstrated that MTA facilitates pulpal healing, promotes dentinogenesis, and exhibits long-term sealing capabilities. The MTA has been demonstrated to possess several advantageous properties, including biocompatibility, antimicrobial activity, the capacity to preserve pulpal integrity and physiological function, the ability to induce tissue regeneration upon contact with dental pulp, and an absence of cytotoxic effects8. However, powder-liquid formulations of MTA exhibit certain drawbacks, including variations in the powder-to-liquid ratio due to operator-dependent mixing and reduced wash-out resistance9. To address these limitations, premixed MTA products in a putty form have been introduced. These products are characterized by their ready-to-use formulations, which exhibit optimal consistency and ratio. These premixed MTA materials are deemed suitable for all conventional MTA applications and are reputed to reduce the risk of washout due to their standardized composition9,10.

The efficacy of VPT is dependent upon the integrity of the seal between the biomaterial and the restorative material. Therefore, achieving a strong bond between biomaterial and restorative material is critical for minimizing bacterial microleakage and ensuring a favorable long-term prognosis4,11. From a clinical standpoint, when MTA is used in VPT, it is typically covered immediately with glass ionomer cement or composite resin7. Resin-modified glass ionomer cements (RMGICs) exhibit several advantages over conventional glass ionomer cements (CGICs), including an extended working time, rapid setting, and enhanced adhesion. Additionally, RMGICs demonstrate resilience to variations in the powder-to-liquid ratio, a prevalent concern in operator-dependent techniques12,13. However, given the presence of free monomers, the biocompatibility of RMGICs may be considered inferior to that of CGICs13. RMGICs, due to their rapid setting time and superior mechanical strength, are particularly suitable for posterior restorations subjected to occlusal stress or in clinical scenarios where moisture control is partially compromised. Conversely, CGICs are advantageous in cervical lesions, root surface restorations, and in patients with high caries risk, owing to their fluoride release and biocompatibility. Nevertheless, the adoption of these materials may be constrained by certain limitations: RMGICs are prone to polymerization shrinkage and may exhibit insufficient curing in areas with limited light access, whereas CGICs demonstrate lower mechanical strength and reduced wear resistance14.

Even though numerous studies have been conducted on the bond strength between MTA and various overlying restorative materials, the results have proven to be inconsistent15,16,17,18. To date, however, only one study has specifically evaluated the effect of the composition and formulation of glass ionomer cements on bond strength. In the study conducted by Ergül et al., although the effect of glass ionomer cement type was examined, only one form of MTA was utilized, and the potential influence of MTA formulation was not considered4. The objective of the present study is to evaluate the bond strength between powder-liquid and premixed forms of MTA and two types of glass ionomer cements: conventional and resin-modified. The initial hypothesis of the study posits that premixed MTA will demonstrate superior bond strength when utilized with glass ionomer cements. The second hypothesis posits that, for both forms of MTA, resin-modified glass ionomer cements will demonstrate higher bond strength compared to conventional glass ionomer cements.

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Protocol

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NOTE: This in vitro study did not require ethical approval as no human or animal subjects were involved. The study was conducted in accordance with the principles of the Declaration of Helsinki.

1. Sample preparation

NOTE: Sample size calculation was based on an effect size of 0.40, α = 0.05, and power = 0.80, resulting in a minimum of 10 samples per group. To enhance statistical reliability, 15 samples per group were used.

  1. Use a total of 60 standardized metal rings, each with a cylindrical cavity of 4 mm in diameter and 3 mm in depth, to contain the MTA materials (see Figure 1).
  2. Application of powder-liquid MTA
    NOTE: The manufacturer recommends mixing the powder and liquid components in a 1:1 ratio by volume to achieve optimal handling properties and physical strength.
    1. Place the powder on a clean glass slab and gradually add the supplied liquid using a sterile dropper. Mix the components with a metallic spatula for 30-60 s until a homogeneous, putty-like consistency is achieved.
    2. Carry the mixed material into the standardized cavities using an MTA carrier.
    3. Compact gently with a plugger to avoid incorporation of air bubbles.
  3. Application of premixed MTA
    1. Dispense the material directly into the cavities using a disposable cannula attached to the syringe.
    2. Use a plugger to ensure proper adaptation and compaction of the material into the cavity.
  4. Place a cotton pellet moistened with distilled water over the material to promote setting (15 min).
    NOTE: As reported in the literature, moist conditions enhance the interfacial adaptation and bonding properties of MTA, whereas dry conditions may adversely affect this process19.

2. Cement application

  1. Mold positioning and surface standardization
    1. After the initial setting of the MTA materials, carefully position cylindrical silicone molds with internal dimensions of 2 mm in diameter and 2 mm in height over the MTA-filled cavities.
  2. Application for CGIC
    1. Dispense the powder and liquid components onto a clean, dry mixing pad using the provided scoop and dropper, following the manufacturer's specified powder-to-liquid ratio of 2.5:1 by weight (1 level scoop of powder to 2 drops of liquid)
    2. Mix the components with a plastic spatula in a circular motion for 30-45 s until a smooth, homogeneous consistency is achieved.
    3. Immediately transfer the mixed material into the mold cavity positioned over the set MTA surface, using a plastic filling instrument to minimize the inclusion of air bubbles.
    4. Allow the material to self-cure for 6 min at room temperature before removing the mold.
  3. Application of RMGIC
    1. Dispense the RMGIC directly into the mold using the preloaded syringe and disposable cannula provided.
    2. Prevent voids and ensure complete adaptation to the MTA surface.
    3. Polymerize the material using an LED curing light at 1000 mW/cm² intensity for 20 s, holding the light-curing tip approximately 1-2 mm from the material surface.
  4. Transfer the specimens to a humidified incubator and store them at 37 °C and 100% humidity for 24 h to simulate intraoral conditions and allow complete material maturation prior to mechanical testing.

3. Shear bond strength testing using a universal testing machine

  1. Switch on the universal testing machine and launch the operating software on the connected control computer prior to testing.
  2. Install the appropriate load cell (1000 N capacity) and allow the system software to calibrate it automatically.
    NOTE: A custom stainless-steel jig was mounted on the lower fixed platform of the device to securely hold the specimen. The jig was specifically designed to prevent lateral movement and ensure that the force would be applied tangentially to the MTA-glass ionomer interface.
  3. Attach a metal chisel-shaped blade (2 mm width, 0.5 mm thickness) to the upper movable crosshead of the testing machine and align the blade edge horizontally at the interface level of each sample to apply a uniform shear force.
    NOTE: Each specimen was placed within the jig so that the bonded interface between MTA and glass ionomer cement was exposed and aligned parallel to the chisel blade; the alignment was visually verified and manually adjusted to ensure that the applied load was directed strictly to the adhesive interface without introducing tensile or compressive components.
  4. Once properly secured, initiate the test protocol from the testing machine's software interface.
  5. Set the crosshead speed at 1 mm/min, consistent with international standards (e.g., ISO 29022 for dental adhesive testing20).
  6. Start the device and apply a progressive shear force to the specimen via the chisel blade until bond failure occurs.
  7. Record the maximum load value (in Newtons) automatically at the moment of debonding.

4. Data collection and calculation

  1. Divide the recorded force (N) by the bonded surface area (in mm²) to obtain the shear bond strength in megapascals (MPa).
  2. Export all measurements from the testing software.
  3. Failure mode analysis
    1. Examine each debonded specimen under a stereomicroscope at 20x magnification.
    2. Classify failure types as follows: Adhesive-separation at the MTA-GIC interface; Cohesive-failure within the MTA or GIC itself; Mixed-a combination of both (see Figure 2).
    3. Conduct the classification with two independent evaluators and consult a third evaluator to reach consensus in cases of disagreement.

5. Statistical analysis

  1. Perform the analysis using IBM SPSS Statistics v29. Assess data normality both visually and statistically.
  2. Report median and interquartile ranges for continuous variables, and frequencies and percentages for categorical variables.
  3. Use the Mann-Whitney U test to compare continuous variables and apply the chi-square test to categorical variables. Consider a type I error level of 5% as statistically significant.

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Results

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The distribution of the force values measured at the moment of separation of the glass ionomer cements from the MTA surface is presented in Table 1. The highest mean force was recorded in the group combining resin-modified glass ionomer cement with powder-liquid MTA, whereas the lowest mean force was observed in the group combining conventional glass ionomer cement with premixed MTA. When evaluated separately, the bond strength values for powder-liquid MTA were higher than those for premixed MTA in both ...

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Discussion

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The adhesion of MTA to overlying glass ionomer cement is influenced by several factors. Metallic oxides present on the MTA surface have the capacity to form strong chemical bonds with the glass ionomer matrix. Additionally, the presence of surface porosities enhances micromechanical retention by increasing the available surface area4. In the present study, the premixed MTA evaluated contains a formulation comprising tricalcium silicate, dicalcium silicate, tricalcium aluminate, calcium oxide, zirc...

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Disclosures

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The authors have no conflicts of interest to disclose.

Materials

List of materials used in this article
NameCompanyCatalog NumberComments
Bio MTA +Cerkamed, Poland1703251for obturation
BIO-C RepairAngelus, Brazil77418for obturation
Glass LinerWP Dental, Germany241328for sealing
Metal blockMoya Yap? Market,Sanliurfa,TurkeyST00103for sample preparation
Restore+D-Tech, IndiaRC030424for sealing
SPSS v29 IBM SPSS Corp, Armonk, New York, USAhttps://www.ibm.com/products/spss-statisticsStatistical analysis
StereomicroscopeLeica MZ 7.5, Leica Microsystems, Germany10450159for identify failure type
Universal Testing MachineShimadzu, AGS-X, JapanC224-E057Cfor shear bond strength measurement
VALO Cordless LED curing light Ultradent, USA5941for light curing

References

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  1. Asgary, S., Nosrat, A. Vital pulp therapy: evidence-based techniques and outcomes. Iran Endod J. 20 (1), e2(2025).
  2. Pandey, P., Nawal, R. R., Talwar, S., Yadav, S. Vital pulp therapy: a bibliometric analysis of the 100 most-cited articles from 1966 to 2022. J Conserv Dent Endod. 27 (11), 1098-1103 (2024).
  3. Xavier, M. T., et al. Calcium silicate-based cements in restorative dentistry: vital pulp therapy clinical, radiographic, and histological outcomes on deciduous and permanent dentition-a systematic review and meta-analysis. Materials (Basel). 17 (17), 4264(2024).
  4. Ergül, R., Aksu, S., Çalışkan, S., Tüloğlu, N. Shear bond strength of calcium silicate-based cements to glass ionomers. BMC Oral Health. 24 (1), 140(2024).
  5. Acharya, S., et al. Comparison of modified NeoPutty MTA, Biodentine, and calcium hydroxide in indirect pulp therapy in deciduous teeth: an in vivo clinical study. Int J Clin Pediatr Dent. 17 (9), 1025-1029 (2024).
  6. Duncan, H. F. Present status and future directions-vital pulp treatment and pulp preservation strategies. Int Endod J. 55 (Suppl 3), 497-511 (2022).
  7. Tyagi, N., et al. Comparative evaluation of shear bond strength of resin-modified glass ionomer cement with ProRoot MTA and MTA Angelus. J Contemp Dent Pract. 25 (1), 35-40 (2024).
  8. Parirokh, M., Torabinejad, M. Mineral trioxide aggregate: a comprehensive literature review-part i: chemical, physical, and antibacterial properties. J Endod. 36 (1), 16-27 (2010).
  9. Kim, H. J., Jang, J. H., Kim, S. Y. Investigation of characteristics as endodontic sealer of novel experimental elastin-like polypeptide-based mineral trioxide aggregate. Sci Rep. 11, 10537(2021).
  10. Bio-C repair. , Angelus. https://angelus.ind.br/en/produto/bio-c-repair/ (2025).
  11. Falakaloğlu, S., Yeniçeri Özata, M., Plotino, G. Micro-shear bond strength of different calcium silicate materials to bulk-fill composite. PeerJ. 11, e15183(2023).
  12. Fleming, G. J., Farooq, A. A., Barralet, J. E. Influence of powder/liquid mixing ratio on the performance of a restorative glass-ionomer dental cement. Biomaterials. 24 (23), 4173-4179 (2003).
  13. Wilson, A. D. Resin-modified glass-ionomer cements. Int J Prosthodont. 3 (5), 425-429 (1990).
  14. Sidhu, S. K., Nicholson, J. W. A review of glass-ionomer cements for clinical dentistry. J Funct Biomater. 7 (3), 16(2016).
  15. Ipek, I., Karaağaç Eskibağlar, B., Yildiz, Þ, Ataş, O., Ünal, M. Analysis of the bond strength between conventional, putty or resin-modified calcium silicate cement and bulk fill composites. Aust Dent J. 68 (4), 265-272 (2023).
  16. Ozata, M. Y., Falakaloglu, S., Plotino, G., Adıguzel, O. The micro shear bond strength of new endodontic tricalcium silicate-based putty: an in vitro study. Aust Endod J. 49, 124-129 (2022).
  17. Singh, D., et al. Comparative evaluation of the bond strength between Bioflx, stainless steel crowns, and stainless steel bands using type 1 glass ionomer cement and resin-modified glass ionomer cement as luting agents: an in vitro study. Int J Clin Pediatr Dent. 18 (1), 70-74 (2025).
  18. Umale, K. G., Gade, V. J., Raut, A. W. Comparative evaluation of shear bond strength and modes of failure of five different reinforced glass ionomer restorative cements to TheraCal LC: an in vitro study. J Conserv Dent Endod. 27 (2), 200-204 (2024).
  19. Eid, A. A., Komabayashi, T., Watanabe, E., Shiraishi, T., Watanabe, I. Characterization of the mineral trioxide aggregate-resin modified glass ionomer cement interface in different setting conditions. J Endod. 38 (8), 1126-1129 (2012).
  20. Herrmann, G., et al. Comparison of different standardised bond strength tests and the influence of glycine powder treatment in composite resin repairs. Int Dent Res. 10 (2), 36-43 (2020).
  21. Alqahtani, A. S., Sulimany, A. M., Alayad, A. S., Alqahtani, A. S., Bawazir, O. A. Evaluation of the shear bond strength of four bioceramic materials with different restorative materials and timings. Materials (Basel). 15 (13), (2022).
  22. Duman, S., Çalışkan, A., Çalışkan, S. Comparison of Medcem MTA, Medcem pure Portland cement and NeoMTA to pediatric restorative materials for shear bond strength. NEU Dent J. 3 (3), 115-121 (2021).
  23. Palma, P. J., et al. Does delayed restoration improve shear bond strength of different restorative protocols to calcium silicate-based cements. Materials (Basel). 11 (11), 2216(2018).
  24. Nandini, S., Ballal, S., Kandaswamy, D. Influence of glass-ionomer cement on the interface and setting reaction of mineral trioxide aggregate when used as a furcal repair material using laser Raman spectroscopic analysis. J Endod. 33 (2), 167-172 (2007).
  25. Saridena, U. S. N. G., et al. An overview of advances in glass ionomer cements. Int J Dent Mater. 4 (4), 89-94 (2022).
  26. Kazemipoor, M., Azizi, N., Farahat, F. Evaluation of microhardness of mineral trioxide aggregate after immediate placement of different coronal restorations: an in vitro study. J Dent (Tehran). 15 (2), 116-122 (2018).
  27. Cantekin, K., Avci, S. Evaluation of shear bond strength of two resin-based composites and glass ionomer cement to pure tricalcium silicate-based cement (Biodentine). J Appl Oral Sci. 22 (4), 302-306 (2014).
  28. Durmazpinar, P. M., Recen, D., Çeliksöz, Ö, Yazkan, B. Micro shear bond strength of mineral trioxide aggregate to different innovative dental restorative materials. Proc Inst Mech Eng H. 237 (6), 762-769 (2023).
  29. Biçer, H., Bayrak, Ş Vital pulpa tedavisinde kullanılan kalsiyum silikat içerikli biyomateryallerin restoratif materyallere bağlanma dayanımının değerlendirilmesi. Selcuk Dent J. 6, 271-279 (2019).
  30. Altunsoy, M., Tanrıver, M., Ok, E., Kucukyilmaz, E. Shear bond strength of a self-adhering flowable composite and a flowable base composite to mineral trioxide aggregate, calcium-enriched mixture cement, and Biodentine. J Endod. 41 (10), 1691-1695 (2015).
  31. Boby, A., Pai, D., Ginjupalli, K., Gaur, S. Comparison of shear bond strength of light cure mineral trioxide aggregate and light cure calcium hydroxide with nanofilled composite: a stereomicroscopic and scanning electron microscope analysis. J Indian Soc Pedod Prev Dent. 38 (1), 56-63 (2020).
  32. Mehra, S., Gupta, A. K., Singh, B. P., Kaur, M., Kumar, A. To evaluate shear bond strength of resin composite to Theracal LC, Biodentine, and resin-modified glass ionomer cement and mode of fracture: an in vitro study. Dent J Adv Stud. 8 (2), 49-54 (2020).
  33. Samman, M., Barakat, O., Fares, H. Bonding ability of different liners to bulk-fill resin composite using silane-containing adhesive. Egypt Dent J. 63 (3), 2905-2913 (2017).
  34. Alhowaish, L., Salama, F., Al-Harbi, M., Abumoatti, M. Shear bond strength of a resin composite to six pulp capping materials used in primary teeth. J Clin Pediatr Dent. 44 (4), 234-239 (2020).
  35. Alzraikat, H., Taha, N. A., Qasrawi, D., Burrow, M. F. Shear bond strength of a novel light-cured calcium silicate-based cement to resin composite using different adhesive systems. Dent Mater J. 35 (6), 881-887 (2016).
  36. Sulwińska, M., Szczesio, A., Bołtacz-Rzepkowska, E. Bond strength of a resin composite to MTA at various time intervals and with different adhesive strategies. Dent Med Probl. 54 (2), 155-160 (2017).
  37. Celiksoz, O., Irmak, O. Delayed vs. immediate placement of restorative materials over Biodentine and RetroMTA: a micro-shear bond strength study. BMC Oral Health. 24 (1), 130(2024).

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Mineral Trioxide AggregateGlass Ionomer CementBond StrengthPowder Liquid MTAPremixed MTAResin Modified Glass IonomerShear Bond StrengthFailure ModesUniversal Testing MachineCohesive Failure

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