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A Soft-Chemistry Approach to the Synthesis of Amorphous Calcium Ortho/Pyrophosphate Biomaterials of Tunable Composition

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A Soft-Chemistry Approach to the Synthesis of Amorphous Calcium Ortho/Pyrophosphate Biomaterials of Tunable Composition OATAO is an open access repository that collects the work of Toulouse researchers and makes it freely available over the web where possible This is an author’s version published in: http://oatao.univ-toulouse.fr/27596 Official URL: https://doi.org/10.1016/j.actbio.2019.12.027 To cite this version: Mayen, Laëtitia and Jensen, Nicholai D. and Laurencin, Danielle and Marsan, Olivier and Bonhomme, Christian and Gervais, Christel and Smith, Mark E. and Coelho, Cristina and Laurent, Guillaume and Trebosc, Julien and Gan, Zhehong and Chen, Kuizhi and Rey, Christian and Combes, Christèle and Soulié, Jérémy A soft-chemistry approach to the synthesis of amorphous calcium ortho/pyrophosphate biomaterials of tunable composition. (2020) Acta Biomaterialia, 103. 333-345. ISSN 1742-7061 Any correspondence concerning this service should be sent to the repository administrator: [email protected] A soft-chemistry approach to the synthesis of amorphous calcium ortho/pyrophosphate biomaterials of tunable composition Laëtitia Mayen a.1 , Nicholai D. Jensen b,c, 1, Danielle Laurencin b, Olivier Marsan a, Christian Bonhommec, Christel Gervaisc, Mark E. Smith<l, Cristina Coelho c, Guillaume Laurent', Julien Trebosce, Zhehong Gan r. Kuizhi Chen r. Christian Rey a, Christèle Combesa, Jérémy Souliéa,+ •C/RJMAT. Université de Toulouse, CNRS, INPT-ENSIACET,Toulouse, France b /CGM, CNRS-UM-ENSCM, Université de Montpellier; Montpellier; France <Sorbonne Université, CNRS, LCMCP. Paris, France d Depamnenr of Chemisrry, Lancaster Universiry, Lancaster, UK • Université de Lille, UMR 8181, UCCS: Unir of Caralysis and Chemisrry of So!ids, Lille, France r National High Magneric Field Laborarory, Tallahassee, FL, USA ARTICLE INFO ABSTRACT Keywords: The development of amorphous phosphate-based materials is of major interest in the field of bioma­ Amorphous materials terials science, and especially for bone substitution applications. ln this context, we herein report the Mixed calcium orrho/pyrophosphate synthesis of gel-derived hydrated amorphous calcium/sodium ortho/pyrophosphate materials at ambi­ Soft chemistry ent temperature and in water. For the first time, such materials have been obtained in a large range Biomaterials of tunable orthophosphate/pyrophosphate molar ratios. Multi-scale characterization was carried out thanks to various techniques, including advanced multinuclear solid state NMR. lt allowed the quantifi­ + cation of each ionic/molecular species leading to a general formula for these materials: [(Ca2+y Na , + 3 4 H 3+"-2y-z)(P04 -)1.x(P2O7 -),d(H2O)u. Beyond this formula, the analyses suggest that these amorphous solids are formed by the aggregation of colloids and that surface water and sodium could play a rote in the cohesion of the whole material. Although the full comprehension of mechanisms of formation and structure is still to be investigated in detail, the straightforward synthesis of these new amorphous ma­ terials opens up many perspectives in the field of materials for bone substitution and regeneration. Statement of significance The metastability of amorphous phosphate-based materials with various chain length often improves their (bio)chemic.al reactivity. However, the contrai of the ratio of the different phosphate entities has not been yet described especially for small ions (pyrophosphate/orthophosphate) and using soft chem­ istry, whereas it opens the way for the tuning of enzyme- and/or pH-driven degradation and biologi­ cal properties. Our study focuses on elaboration of amorphous gel-derived hydrated calcium/sodium or­ tho/pyrophosphate solids at 70 °C with a large range of orthophosphate/pyrophosphate ratios. Multi-scale characterization was carried out using various techniques such as advanced multinuclear SSNMR (31 P, 23Na, 1 H, 43Ca). Analyses suggest that these solids are formed by colloids aggregation and that the loca­ tion of mobile water and sodium could play a rote in the material cohesion. 1. Introduction Among inorganic materials for bone substitution, amorphous solids have attracted a lot of attention. Indeed, their metastability • Corresponding author. often improves their (bio)chemical reactivity. The subsequent re­ E-mail addresses: [email protected], [email protected] U­ Iease of active ions (1 ], and/or dissolution/precipitation reactions Soulié). Iead to neoformed apatite, that positively impacts osteoconduc- 1 These authors contributed equally to the work. hnps :/ /doi.org/1 0.1016/j.actbio.2019.12.ü27 tion and osteoinduction [2] . The most famous example of amor- mineral formation. In osteoblast cultures especially, pyrophosphate phous biomaterials is probably that of the bioactive silicate-based inhibition occurs by binding to the mineral, up-regulating osteo- glasses (either sol-gel or melt-derived), which have been exten- pontin, and inhibiting alkaline phosphatase activity [25] . It has sively studied [2 , 3] . The present paper, however, focuses on new been observed, however, that, in vivo , the pyrophosphate level is types of phosphate-based amorphous materials for bone regenera- rather well controlled and that its variations, due to physical ac- tion. Two main families of materials belonging to this category are tivity for example, are regulated [26] . More generally, in humans, studied by different scientific communities and are referenced in the total production of pyrophosphate ions per day is evaluated, the literature as phosphate-based glasses and amorphous calcium from 0.7 to several kg [26] and more that 170 biological reactions phosphates. involving pyrophosphate ions have been identified [26] . On the one hand, phosphate-based glasses are generally made Therefore, the control of the ortho/pyrophosphate ratio within by fusion. Considering pure binary P2 O5 –CaO glasses [4], the na- an amorphous material (synthesized at a temperature of only 70 °C ture of the phosphate units (as expressed by the Q n terminology, and without any additives) could potentially be an interesting ad- where n is the number of bridging oxygen atoms per PO4 tetra- justable parameter for tuning the kinetics of biomaterial degrada- hedron) can be controlled through the atomic Ca/P ratio. This ra- tion and bone mineral formation. tio can vary from ultraphosphates (phosphate 3D network mainly In this work, we thus investigate in detail the effect of the based on Q 3 species) to metaphosphate glasses (linear phosphate ortho/pyrophosphate content on the nature, structure and mor- chains, mainly Q 2 ) and eventually to invert glasses (isolated py- phology of newly-synthesized amorphous biomaterials, using com- rophosphates and orthophosphates, Q 1 and Q 0 respectively). This plementary characterization techniques and in particular advanced range of composition and the use of additives allow the elabora- multinuclear solid state NMR. Advanced solid state NMR are of tion of such glasses and the control of their dissolution [5–9] . paramount importance in the studies of amorphous derivatives On the other hand, amorphous calcium phosphate powders can such as bioglasses for which XRD data are much less informative. be synthesized by precipitation in solution at room temperature, The smart use of the NMR interactions (indirect J couplings and most of the time in water and without further high tempera- spatial dipolar couplings, D) allows to safely establish through- ture treatment [10] . These are generally obtained by double de- bond and through-space connectivities. In this work, 31P INADE- composition between soluble calcium and phosphate salt precur- QUATE MAS experiments were explored to disentangle the contri- sors, and some processes lead to dense liquid “coacervates” [11] . butions of ortho- and pyrophosphates groups in 1D 31P MAS ex- Several kinds of phosphate precursors have been used: long-chain periments (especially for amorphous materials). Most importantly, polyphosphates (polyP) [12 , 13] , cyclic polyphosphates [14] , diphos- homo- (31P-31P) and heteronuclear (23Na-31P) 2D correlation 4 − phates (also called pyrophosphates: P2 O7 ) [15–17] or orthophos- experiments were implemented to highlight the presence/absence 3 − phates (PO4 ) [10]. Without any high temperature treatment, the of segregated domains (both from the anionic, ie ortho- and polyP associations are preserved in the final materials, which re- pyrophosphates, and cationic, ie Na + and Ca 2 + , points of view). main amorphous. In contrast, crystallization can occur when only orthophosphates or pyrophosphates (smaller anions) are present. 2. Experimental section In this case, the amorphous/crystalline nature depends on the syn- thetic parameters used (pH, concentration…) [16–18] . 2.1. Precursors In this context, we recently reported the synthesis of different compositions of monolithic calcium and potassium pyrophosphate Calcium chloride dihydrate (CaCl • 2H O, Merck) and tri-sodium materials (PYG materials, PYrophosphate Glasses) prepared using 2 2 phosphate dodecahydrate (Na PO • 12H O, GRP rectapur, VWR soft conditions (in aqueous solution with a drying step at 70 °C) 3 4 2 + − Chemicals) were used as received, as calcium and orthophos- [17] . We showed that an increase of the Ca 2 /P O 4 ratio in the 2 7 phate sources, respectively. The pyrophosphate precursor, anhy- precursor batch solution resulted in an increase of the proportion drous tetrasodium pyrophosphate (Na P O ), was prepared by of crystalline calcium pyrophosphate phase in the final material. 4 2 7 heating disodium hydrogen phosphate powder
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