Abstract
Secondary protonated calcium phosphates such as brushite (CaHPO4·2H2O) or monetite (CaHPO4) have a higher resorption potential in bone defects than sintered ceramics, e.g. tricalcium phosphate or hydroxyapatite. However, processing of these phosphates to monolithic blocks or granules is not possible by sintering due to thermal decomposition of protonated phosphates at higher temperatures. In this study a low temperature technique for the preparation of spherical brushite granules in a cement setting reaction is presented. These granules were synthesized by dispersing a calcium phosphate cement paste composed of β-tricalcium phosphate and monocalcium phosphate together with a surfactant to an oil/water emulsion. The reaction products were characterized regarding their size distribution, morphology, and phase composition. Clinically relevant granule sizes ranging from 200 μm to 1 mm were obtained, whereas generally smaller granules were received with higher oil viscosity, increasing temperature or higher powder to liquid ratios of the cement paste. The hardened granules were microporous with a specific surface area of 0.7 m2/g and consisted of plate-like brushite (>95 % according to XRD) crystals of 0.5–7 μm size. Furthermore it was shown that the granules may be also used for drug delivery applications. This was demonstrated by adsorption of vancomycin from an aqueous solution, where a load of 1.45–1.88 mg drug per g granules and an almost complete release within 2 h was obtained.
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Niedhart C, Pingsmann A, Jurgens C, Marr A, Blatt R, Niethard FU. Komplikationen nach Entnahme autologen Knochens aus dem ventralen und dorsalen Beckenkamm-eine prospektive, kontrollierte studie. Z Orthop Grenzgeb. 2003;141:481–6.
Mazock JB, Schow SR, Triplett RG. Posterior iliac crest bone harvest: review of technique, complications and use of an epidural catheter for post-operative pain control. J Oral Maxillofac Surg. 2003;61:1497–503.
Wenisch S, Stahl JP, Horas U, Heiss C, Kilian O, Trinkaus K, Hild A, Schnettler R. In vivo mechanisms of hydroxyapatite ceramic degradation by osteoclasts: Fine structural microscopy. J Biomed Mater Res. 2003;67:713–8.
Mangano C, Piattelli A, Perrotti V, Lezzi G. Dense hydroxyapatite inserted into postextraction sockets: A histologic and histomorphometric 20-year case report. J Periodontol. 2008;79:929–33.
Horch HH, Sader R, Kolk A. Synthetische, phasenreine Beta-Tricalciumphosphat-Keramik (Cerasorb) zur Knochenregeneration bei der rekonstruktiven Chirurgie der Kiefer - Eine klinische Langzeitstudie mit Literaturübersicht. Deutsche Zahnärztliche Zeitschrift. 2004;59:680–6.
Theiss F, Apelt D, Brand B, Kutter A, Zlinszky K, Bohner M, Matter S, Frei C, Auer JA, von Rechenberg B. Biocompatibility and resorption of a brushite calcium phosphate cement. Biomaterials. 2005;26:4383–94.
Tamimi F, Torres J, Lopez-Cabarcos E, Bassett DC, Habibovic P, Luceron E, Barralet JE. Minimally invasive maxillofacial vertical bone augmentation using brushite based cements. Biomaterials. 2009;30:208–16.
Grover LM, Knowles JC, Fleming GJP, Barralet JE. In vitro ageing of brushite calcium phosphate cement. Biomaterials. 2003;24:4133–41.
Grover LM, Gbureck U, Wright AJ, Tremayne M, Barralet JE. Biologically mediated resorption of brushite cement in vitro. Biomaterials. 2006;27:2178–85.
Xia Z, Grover LM, Huang Y, Adamopoulos IE, Gbureck U, Triffitt JT, Shelton RM, Barralet JE. In vitro biodegradation of three brushite calcium phosphate cements by a macrophage cell-line. Biomaterials. 2006;27:4557–65.
Tamimi FM, Torres J, Tresguerres I, Clemente C, Lopez-Cabarcos E, Blanco LJ. Bone augmentation in rabbit calvariae: comparative study between Bio-Oss (R) and a novel beta-TCP/DCPD granulate. J Clin Periodontol. 2006;33:922–8.
Marinno FT, Torres J, Tresguerres I, Jerez LB, Cabarcos EL. Vertical bone augmentation with granulated brushite cement set in glycolic acid. J Biomed Mater Res A. 2007;81A:93–102.
Tamimi F, Torres J, Kathan C, Baca R, Clemente C, Blanco L, Lopez-Cabarcos E. Bone regeneration in rabbit calvaria with novel monetite granules. J Biomed Mater Res A. 2008;87A:980–5.
Mirtchi AA, Lemaitre J, Munting E. Calcium phosphate cements - action of setting regulators on the properties of the beta-tricalcium phosphate monocalcium phosphate cements. Biomaterials. 1989;10:634–8.
Blume O, Krekeler G, Schilli W. Indikation und Beispiele für die Anwendung von alpha-Tricalciumphosphat als resorbierbarer, alloplastischer Knochenersatz. Unfallchirurg. 1998;265:303–11.
Zijderveld SA, Zerbo IR, van den Bergh JP, Schulten EA, ten Bruggenkate CM. Maxillary sinus floor augmentation using a β-tricalcium phosphate (Cerasorb) alone compared to autogenous bone grafts. Int J Oral Maxillofac Implant. 2005;20:432–40.
Briem D, Linhart W, Lehmann W, Meenen NM, Rueger JM. Langzeitergebnisse nach Anwendung einer porösen Hydroxylapatitkeramik (Endobon) zur operativen Versorgung von Tibiakopffrakturen. Unfallchirurg. 2002;105:128–33.
Tamimi F, Sheikh Z, Barralet JE. Dicalcium phosphate cements: Brushite and monetite. Acta Biomater. 2012;8:474–87.
Ginebra MP, Espanol M, Montufar EB, Perez RA, Mestres G. New processing approaches in calcium phosphate cements and their applications in regenerative medicine. Acta Biomater. 2010;6:2863–73.
Barralet JE, Grover LM, Gbureck U. Ionic modification of calcium phosphate cement viscosity Part II: Hypodermic injection and strength improvement of brushite cements. Biomaterials. 2004;25(11):2197–203.
Gbureck U, Hölzel T, Klammert U, Würzeler K, Müller FA, Barralet JE. Resorbable dicalcium phosphate bone substitutes made by 3D powder printing. Adv Funct Mater. 2007;17:3940–5.
Torres J, Tamimi F, Alkhraisat M, Prados-Frutos JC, Rastikerdar E, Gbureck U, Barralet JE, López-Cabarcos E. Vertical bone augmentation with 3D-synthetic monetite blocks in the rabbit calvaria. J Clin Periodont. 2011;38:1147–53.
Misiek DJ, Kent JN, Carr RF. Soft tissue responses to hydroxylapatite particles of different shapes. J Oral Maxillofac Surg. 1984;42:150–60.
Gbureck U, Vorndran E, Müller FA, Barralet JE. Low temperature direct 3D printed bioceramics and biocomposites as drug release matrices. J Controlled Release. 2007;122:173–80.
Hofmann M, Mohammed AR, Perrie Y, Gbureck U, Barralet JE. High strength resorbable brushite bone cement with controlled drug releasing capabilities. Acta Biomater. 2009;5:43–9.
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Moseke, C., Bayer, C., Vorndran, E. et al. Low temperature fabrication of spherical brushite granules by cement paste emulsion. J Mater Sci: Mater Med 23, 2631–2637 (2012). https://doi.org/10.1007/s10856-012-4740-1
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DOI: https://doi.org/10.1007/s10856-012-4740-1