Characterization of chlorhexidine-releasing, fast-setting, brushite bone cements

Abstract

The effect of antibacterial chlorhexidine diacetate powder (CHX) on the setting kinetics of a brushite-forming β-tricalcium phosphate/monocalcium phosphate monohydrate (β-TCP/MCPM) cement was monitored using attenuated total reflection Fourier transform infrared spectroscopy. The final composition of the set cement with up to 12 wt.% CHX content before and after submersion in water for 24 h, the kinetics of chlorhexidine release and the total sample mass change in water over four weeks was monitored using Raman mapping, UV spectroscopy and gravimetry, respectively. Below 9 wt.%, CHX content had no significant effect on brushite formation rate at 37 °C, but at 12 wt.% the half-life of the reaction decreased by one-third. Raman mapping confirmed that brushite was the main inorganic component of the set cements irrespective of CHX content, both before and after submersion in water. The CHX could be detected largely as discrete solid particles but could also be observed partially dispersed throughout the pores of the set cement. The percentage of CHX release was found to follow Fick’s law of diffusion, being independent of its initial concentration, proportional to the square root of time and, with 1 mm thick specimens, 60% was released at 24 h. Total set cement mass loss rate was not significantly affected by CHX content. On average, cements exhibited a loss of 7 wt.% assigned largely to surface phosphate particle loss within the initial 8 h followed by 0.36 wt.% per day.