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A Design of Experiment Approach to the Synthesis of Alendronate-incorporated Hydroxyapatite


A design of experiment (DoE) approach is presented for the optimization of Alendronate-hydroxyapatite nanoparticles� synthesis. The synthesis was performed using the chemical precipitation technique from calcium nitrate, diammonium hydrogen phosphate and alendronate. Synthesis temperature, reactant addition rate and ripening time were chosen as the most relevant experimental factors for our synthesis. Design of Experiments was used in order to measure these conclusive process parameters and their effect on controlling some final nanoparticles parameters, such us: alendronate incorporation efficiency (IncorporationEfficiency, %), hydroxyapatite crystallite size (Size_XRD, nm), hydroxyapatite particle size distribution (Size_DLS, �). Our study found that better HA-AL incorporation efficiency and small nonoparticles can be obtained using the following chemical process parameters: reaction temperature 30oC or smaller, ripening time 108h and addition rate 0.1mol/min. The analysis of more than one nanoparticles characteristics was possible using DoE software, MODDE 9.1. Thus, hydroxyapatite-alendronate incorporation efficiency should be expected to increase with decreasing temperature below 300C, increasing the maturate time at least 108h, at an addition rate of 0.1mol/min, in an N2 atmosphere. The same conditions will ensure nanoparticles small size that would be more desirable for the application of implants.
