Effect of Powder-to-Liquid Ratio on pH, Calcium Ion Release, and Solubility Behaviors of Endodontic Bioceramics: An In Vitro Study
Abstract
1. Introduction
2. Materials and Methods
2.1. Bioceramic Disc Preparation
2.2. Evaluation of pH Levels and Calcium Ion Concentration in the Eluate
2.3. Mass Change and Water Sorption
2.4. Effects of the Powder-Liquid (Or Paste) Ratio of F or BG
2.5. Statistical Analysis
2.6. Sample Size
- pH: Based on a predicted difference between F (10.5 [0.02]) and BG (9.3 [0.04]) groups observed in the pilot data (Figure S1, Table S2), six samples were enrolled per group (α = 0.05).
- Calcium ion release: Based on a difference between F (480.0 [0.0]) and NC (45.0 [1.4]) groups observed in the pilot data (Figure S2, Table S3), three samples were enrolled per group (α = 0.05).
- Mass change: Based on a difference between BG (−16.0 [0.2]) and HP (−6.0 [0.6]) groups observed in the pilot data (Figure S3, Table S4), three samples were enrolled per group (α = 0.05)
- pH and Calcium ion release: Based on differences between BG0 (pH: 9.1 [0.09]; Ca: 72.0 [8.7]) and NC (pH: 8.7 [0.10]; Ca: 0.0 [0.0]) groups observed in the pilot data (Figures S4 and S5, Tables S5 and S6), four samples were enrolled per group (α = 0.05).
- Mass change and water sorption: Based on the difference between F0 (87.2 [18.3]) and F2 (−12.0 [13.2]) groups observed in the pilot data (Figure S6, Table S7), as well as BG0 (32.5 [21.6]) and BG2 (−41.2 [8.1]) groups, four samples were used for each comparison (α = 0.05).
3. Results
3.1. pH Kinetics
3.2. Calcium Ion Release
3.3. Mass Change and Water Sorption
3.4. pH Kinetics of F and BG at Different Consistencies
3.5. Calcium Ion Release of F and BG at Different Consistencies
3.6. Mass Change and Water Sorption of F and BG at Different Consistencies
4. Discussion
4.1. The Relationship Between Decreasing Calcium Ion Release and Sustained Alkalinity
4.2. The Relationship Between Physicochemical Properties and Cytocompatibility
4.3. Comparison of HP Physicochemical Properties
4.4. The Influence of the Powder-to-Liquid Ratio of F on Biological Outcomes
4.5. The Influence of Powder-to-Paste Ratio of BG on Biological Outcomes
4.6. Comparison of Ion Release Kinetics of BG with Previous Literature
4.7. Study Limitations
4.8. Clinical Implications
5. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Abbreviations
| ANOVA | Analysis of variance |
| BG | Nishika Canal Sealer BG multi |
| F | MTA Flow White |
| HP | MTA Repair HP |
| hPDLCs | Human periodontal-ligament-derived cells |
| MTA | Mineral trioxide aggregate |
| MTT | 3-[4,5-dimethylthiazol-2-yl]-2,5 diphenyl tetrazolium bromide |
| NC | Negative control |
| PRILE | Preferred Reporting Items for Laboratory Studies in Endodontology |
| SA/V | Surface area-to-volume |
| SD | Standard deviation |
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| Materials | Manufactures | Composition |
|---|---|---|
| MTA Repair HP (HP) | Angelus (Londrina, Brazil) | powder: calcium silicate, calcium aluminate, calcium oxide, calcium tungstate liquid: purified water, plasticizer |
| MTA Flow White (F) | Ultradent Products (South Jordan, UT, USA) | powder: tricalcium silicate, dicalcium silicate, calcium sulfate, etc. gel: purified water, thickening agent |
| Nishika Canal Sealer BG multi (BG) | Nippon Shika Yakuhin (Yamaguchi, Japan) | paste A: fatty acids, bismuth bicarbonate, silicon dioxide paste B: magnesium oxide, purified water, calcium silicate glass, silicon dioxide, etc. powder: calcium silicate glass, calcium hydroxide |
| Day | 3 | 5 | 7 | 10 | 12 | 14 | 17 | 19 | 21 | 24 | 26 | 28 |
|---|---|---|---|---|---|---|---|---|---|---|---|---|
| F | 11.3 (0.7) a | 11.2 (0.7) a | 11.1 (0.7) ab | 11.2 (0.5) a | 11.2 (0.6) a | 11.1 (0.4) a | 11.0 (0.4) a | 11.0 (0.3) a | 11.0 (0.4) ab | 10.9 (0.3) ab | 10.9 (0.4) ab | 10.8 (0.5) ab |
| HP | 10.4 (0.3) b | 10.4 (0.3) b | 10.4 (0.3) b | 10.6 (0.3) b | 10.4 (0.3) b | 10.4 (0.2) b | 10.4 (0.4) b | 10.5 (0.3) b | 10.6 (0.4) b | 10.7 (0.3) b | 10.5 (0.3) b | 10.4 (0.3) b |
| BG | 9.4 (0.1) c | 9.4 (0.1) c | 9.4 (0.1) c | 9.4 (0.1) c | 9.4 (0.1) c | 9.3 (0.1) c | 9.3 (0.1) c | 9.4 (0.0) c | 9.4 (0.1) c | 9.4 (0.1) c | 9.3 (0.2) c | 9.3 (0.1) c |
| NC | 8.7 (0.1) d | 8.8 (0.1) d | 8.7 (0.1) d | 8.7 (0.1) d | 8.8 (0.1) d | 8.7 (0.1) d | 8.7 (0.1) d | 8.8 (0.2) d | 8.8 (0.2) d | 8.8 (0.1) d | 8.7 (0.0) d | 8.7 (0.1) d |
| Day | 3 | 5 | 7 | 10 | 12 | 14 | 17 | 19 | 21 | 24 | 26 | 28 |
|---|---|---|---|---|---|---|---|---|---|---|---|---|
| F | 523.3 (32.1) a | 466.7 (55.1) a | 386.7 (49.3) a | 306.7 (90.7) a | 260.0 (90.0) a | 176.7 (55.1) a | 156.7 (55.1) a | 146.7 (23.1) a | 150.0 (26.5) a | 190.0 (26.5) a | 163.3 (15.3) a | 173.3 (15.3) a |
| HP | 47.0 (7.5) c | 66.3 (14.6) c | 62.3 (9.7) c | 59.0 (8.2) c | 50.3 (7.4) c | 43.3 (5.5) b | 45.0 (3.6) c | 43.3 (4.7) c | 42.7 (2.5) c | 51.7 (4.9) c | 48.3 (4.5) c | 45.3 (5.1) b |
| BG | 123.3 (5.8) b | 110.0 (0.0) b | 94.0 (1.0) b | 85.3 (3.5) b | 75.7 (2.1) b | 68.0 (1.7) b | 65.0 (1.0) b | 63.3 (2.3) b | 66.7 (2.1) b | 69.0 (2.6) b | 67.0 (4.0) b | 60.3 (2.5) b |
| NC | 0.0 (0.0) d | 0.0 (0.0) d | 0.0 (0.0) d | 0.0 (0.0) d | 0.0 (0.0) d | 0.0 (0.0) c | 0.0 (0.0) d | 0.0 (0.0) d | 0.0 (0.0) d | 0.0 (0.0) d | 0.0 (0.0) d | 0.0 (0.0) c |
| Material | Property | 1 | 2 | 3 | Mean ± SD |
|---|---|---|---|---|---|
| F | Mass change (%) | −20.6 | −21.3 | −15.5 | −19.2 ± 3.1 a |
| Water sorption (%) | 31.9 | 29.1 | 28.2 | 29.7 ± 1.9 a | |
| HP | Mass change (%) | −15.2 | −14.8 | −13.4 | −14.5 ± 0.9 a |
| Water sorption (%) | 35.7 | 28.2 | 30.5 | 31.4 ± 3.8 a | |
| BG | Mass change (%) | −10.9 | −17.3 | −16.8 | −15.0 ± 3.6 a |
| Water sorption (%) | 20.4 | 22.0 | 23.0 | 21.8 ± 1.3 b |
| Day | 3 | 5 | 7 | 10 | 12 | 14 | 17 | 19 | 21 | 24 | 26 | 28 |
|---|---|---|---|---|---|---|---|---|---|---|---|---|
| F0 | 11.0 (0.1) a | 11.2 (0.5) a | 10.5 (0.4) a | 10.6 (0.4) a | 10.7 (0.2) a | 10.8 (0.2) a | 10.6 (0.2) a | 10.6 (0.3) a | 10.6 (0.3) a | 10.6 (0.4) a | 10.6 (0.3) a | 10.5 (0.3) a |
| F1 | 11.0 (0.0) a | 10.9 (0.1) a | 10.6 (0.3) a | 10.6 (0.2) a | 10.6 (0.1) a | 10.7 (0.0) a | 10.6 (0.0) a | 10.7 (0.0) a | 10.7 (0.0) a | 10.7 (0.1) a | 10.6 (0.1) a | 10.6 (0.1) a |
| F2 | 10.8 (0.0) a | 10.7 (0.1) a | 10.5 (0.2) a | 10.5 (0.2) a | 10.5 (0.2) a | 10.6 (0.2) a | 10.5 (0.1) a | 10.5 (0.2) a | 10.5 (0.1) a | 10.4 (0.1) a | 10.5 (0.1) a | 10.5 (0.1) a |
| BG0 | 9.3 (0.1) b | 9.3 (0.1) b | 9.2 (0.1) b | 9.2 (0.0) b | 9.2 (0.0) b | 9.2 (0.1) b | 9.1 (0.1) b | 9.1 (0.1) b | 9.1 (0.1) b | 9.1 (0.1) b | 9.1 (0.1) b | 9.1 (0.1) b |
| BG1 | 9.3 (0.0) b | 9.3 (0.0) b | 9.3 (0.0) b | 9.3 (0.0) b | 9.3 (0.0) b | 9.3 (0.0) b | 9.2 (0.0) b | 9.2 (0.0) b | 9.1 (0.0) b | 9.1 (0.0) b | 9.1 (0.0) b | 9.1 (0.0) b |
| BG2 | 9.4 (0.0) b | 9.3 (0.1) b | 9.3 (0.0) b | 9.3 (0.0) b | 9.3 (0.0) b | 9.3 (0.0) b | 9.2 (0.0) b | 9.2 (0.0) b | 9.2 (0.0) b | 9.2 (0.1) b | 9.2 (0.1) b | 9.1 (0.1) b |
| NC | 7.8 (0.0) c | 7.9 (0.1) c | 7.8 (0.1) c | 7.9 (0.1) c | 8.0 (0.1) c | 8.3 (0.3) c | 8.4 (0.2) c | 8.4 (0.3) c | 8.3 (0.2) c | 8.2 (0.2) c | 8.2 (0.2) c | 8.3 (0.2) c |
| Day | 3 | 5 | 7 | 10 | 12 | 14 | 17 | 19 | 21 | 24 | 26 | 28 |
|---|---|---|---|---|---|---|---|---|---|---|---|---|
| F0 | 470.0 (20.0) a | 430.0 (20.0) a | 417.5 (20.6) a | 392.5 (9.6) a | 395.0 (17.3) a | 382.5 (28.7) a | 370.0 (27.1) a | 350.0 (25.8) a | 280.0 (29.4) a | 257.5 (26.3) a | 245.0 (25.2) a | 225.0 (12.9) a |
| F1 | 470.0 (20.0) a | 420.0 (23.1) a | 400.0 (24.5) a | 377.5 (28.7) a | 360.0 (32.7) a | 355.0 (25.2) a | 342.5 (41.9) a | 327.5 (42.7) a | 292.5 (51.9) a | 265.0 (44.3) a | 247.5 (35.9) a | 227.5 (22.2) a |
| F2 | 500.0 (23.1) a | 410.0 (20.0) a | 392.5 (33.0) a | 392.5 (34.0) a | 382.5 (34.0) a | 377.5 (36.9) a | 370.0 (29.4) a | 355.0 (23.8) a | 265.0 (59.7) a | 252.5 (55.0) a | 232.5 (45.7) a | 202.5 (33.0) a |
| BG0 | 117.5 (5.0) b | 107.5 (5.0) b | 102.0 (5.4) b | 97.8 (4.5) b | 96.3 (4.5) b | 93.3 (11.6) b | 65.5 (14.3) b | 75.3 (15.3) b | 61.3 (9.8) b | 59.5 (10.9) b | 59.5 (9.9) b | 58.0 (9.5) b |
| BG1 | 117.5 (5.0) b | 105.0 (5.8) b | 89.0 (8.2) b | 90.3 (5.3) b | 86.5 (6.0) b | 83.5 (7.4) b | 54.0 (12.1) b | 62.0 (8.2) b | 48.0 (4.3) b | 45.0 (3.5) b | 45.8 (2.2) b | 43.8 (3.0) b |
| BG2 | 125.0 (5.8) b | 102.5 (5.0) b | 80.5 (8.7) b | 81.8 (10.2) b | 82.0 (9.6) b | 78.0 (9.9) b | 53.5 (13.8) b | 55.0 (6.8) b | 44.0 (3.3) b | 43.0 (5.0) b | 45.5 (2.5) b | 42.5 (2.1) b |
| NC | 0.0 (0.0) c | 0.0 (0.0) c | 0.0 (0.0) c | 0.0 (0.0) c | 0.0 (0.0) c | 0.0 (0.0) c | 0.0 (0.0) c | 0.0 (0.0) c | 0.0 (0.0) c | 0.0 (0.0) c | 0.0 (0.0) c | 0.0 (0.0) c |
| Material | Property | 1 | 2 | 3 | 4 | Mean ± SD |
|---|---|---|---|---|---|---|
| F0 | Mass change (%) | −12.8 | −11.3 | −7.0 | −13.1 | −11.1 ± 2.8 b |
| Water sorption (%) | 19.5 | 21.6 | 17.6 | 24.1 | 20.7 ± 2.8 b | |
| F1 | Mass change (%) | −5.1 | −3.6 | −8.5 | −7.2 | −6.1 ± 2.2 b |
| Water sorption (%) | 12.2 | 9.3 | 15.2 | 12.5 | 12.3 ± 2.4 b | |
| F2 | Mass change (%) | 19.7 | 19.2 | 13.7 | 12.7 | 16.3 ± 3.7 a |
| Water sorption (%) | 5.2 | 5.3 | 6.7 | 4.1 | 5.3 ± 1.1 a | |
| Material | Property | 1 | 2 | 3 | 4 | Mean± SD |
| BG0 | Mass change (%) | −9.5 | −9.9 | −14.4 | −13.2 | −11.8 ± 2.4 a |
| Water sorption (%) | 18.0 | 18.9 | 19.8 | 16.9 | 18.4 ± 1.2 a | |
| BG1 | Mass change (%) | −10.7 | −9.7 | −6.7 | −11.7 | −9.7 ± 2.2 a |
| Water sorption (%) | 16.4 | 15.8 | 11.1 | 14.5 | 14.5 ± 2.3 ab | |
| BG2 | Mass change (%) | −10.5 | −13.7 | −12.5 | −8.5 | −11.3 ± 2.3 a |
| Water sorption (%) | 8.1 | 5.2 | 10.6 | 13.0 | 9.2 ± 3.4 b |
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Aka, A.; Matsuura, T.; Yoshimura, A. Effect of Powder-to-Liquid Ratio on pH, Calcium Ion Release, and Solubility Behaviors of Endodontic Bioceramics: An In Vitro Study. J. Funct. Biomater. 2026, 17, 220. https://doi.org/10.3390/jfb17050220
Aka A, Matsuura T, Yoshimura A. Effect of Powder-to-Liquid Ratio on pH, Calcium Ion Release, and Solubility Behaviors of Endodontic Bioceramics: An In Vitro Study. Journal of Functional Biomaterials. 2026; 17(5):220. https://doi.org/10.3390/jfb17050220
Chicago/Turabian StyleAka, Asuka, Takashi Matsuura, and Atsutoshi Yoshimura. 2026. "Effect of Powder-to-Liquid Ratio on pH, Calcium Ion Release, and Solubility Behaviors of Endodontic Bioceramics: An In Vitro Study" Journal of Functional Biomaterials 17, no. 5: 220. https://doi.org/10.3390/jfb17050220
APA StyleAka, A., Matsuura, T., & Yoshimura, A. (2026). Effect of Powder-to-Liquid Ratio on pH, Calcium Ion Release, and Solubility Behaviors of Endodontic Bioceramics: An In Vitro Study. Journal of Functional Biomaterials, 17(5), 220. https://doi.org/10.3390/jfb17050220

