Robustness testing of milling process, analyzing the particle size distribution and crystallinity of the milled samples

Abstract

The aim of this work was to discover the robustness of combined wet milling process to determine the interval of the Mel (meloxicam) amount and to predict the degree of crystallinity of the milled samples using DSC and XRPD measurements. The samples had the poly(vinyl alcohol) (PVA) as the stabilizing agent. By increasing the amount of the Mel, its crystallinity increased and close correlation was found between the degree of crystallinity and the Mel amount. To achieve the desired particle size range (100-500 nm), the Mel amount should be changed between 10.0 and 17.5% (w/w) and a PVA concentration should be used between 5.0 and 4.58% (w/w). In this specified range, the degree of crystallinity of Mel will be changed between 20 and 45%. The crystallinity of Mel investigated by DSC and XRPD did not show any significant difference at 95% significance level. During the milling process to predict the amorphous content of the active agent, the DSC method can be suggested for the fast quantification of the degree of crystallinity.