Effects of γ-irradiation and accelerated aging on composition-structure–property relationships for radiopaque embolic microspheres

Abstract Si–Ca–Zn–La–Ti–Mg–Sr–Na glasses have demonstrated excellent biocompatibility both in vitro using the MTT/LDH assays (with L929 mouse fibroblast cells and human blood platelets), and in vivo using New Zealand White rabbits. However, the biological evaluation of the materials was performed on as-manufactured glass granules that were autoclaved, rather than aged or γ-irradiated glass microspheres; the sterilization procedure required prior to implantation of these materials in its final form inside the human body. Given the fact that when a glass is subjected to aging either accelerated or natural changes in its physical properties can take place, it is imperative to determine whether the structure of such glasses will be altered over time in order to substantiate shelf-life claims. The structure of such glasses may also be altered as a result of exposure to the typical amounts of γ-irradiation required to sterilize such materials prior to implantation. This paper therefore examines the structure of Si–Ca–Zn–La–Ti–Mg–Sr–Na glasses using XRD, DSC, pycnometry, 29 Si MAS-NMR and ICP–OES to evaluate both the effect of accelerated aging and multiple cycles of 30 kGy γ-irradiation on their structure and subsequent radiopacity. The 29 Si MAS-NMR results indicate that the peak maxima for each glass remain between − 83 ppm and − 86 ppm; a chemical shift for 29 Si associated with Q 2 to Q 3 units in silicate glasses, and that the local environment around the 29 Si isotope remains unaltered as a result of aging or exposure. Additional analysis (XRD, DSC, pycnometry, ICP–OES and radiopacity) showed that the glass transition temperature, T g (676 ± 4 °C) typically remains unchanged, as a result of exposure to both accelerated aging and ionizing radiation, as do the density (3.63 ± 0.02 g/cm 3 ) radiopacity (7049 ± 847HU), chemical composition and XRD diffractograms for each glass. Therefore it can be concluded that the accelerated aging conditions tested herein or use of 30 kGy γ-irradiation dose or subsequent effects does not affect the local environment of the 29 Si isotope in the glasses, nor does it significantly alter the XRD diffraction patterns, chemical composition, T g , density or the radiopacity values for the glass composition (0.562Si–0.035Ca–0.188Zn–0.068La–0.042Ti–0.035 Mg–0.035Sr–0.035Na) described in this work.