Helium pycnometry as a tool for assessment of sealing efficiency in microencapsulation

There is a need for a fast and reliable method to evaluate the development in coating quality during coating, especially for fast dissolving coatings. In the present study, pycnometric density was evaluated as a tool for assessment of coating quality in terms of sealing efficiency for microspheres coated with polymeric aqueous solutions. Further, it was investigated if the method could be used to study effects of spray variables on the sealing efficiency of coated microspheres. The microcrystalline cellulose particles Ethispheres250 were coated with aqueous solutions of Hypromellose 5 and Povidone K-90F by Wurster bottom-spray technique. End products and samples drawn during coating were analysed in terms of pycnometric helium density and scanning electron microscopy (SEM). Experiments constituted a 2(3) factorial design with the following spray related variables: atomisation air flow, polymer type, and solution concentration/viscosity. Helium pycnometric density was seen to lower gradually during coating in all experiments and to follow a common pattern. The quantitative lowering in density was further seen to correlate to sealing of voids by gradual covering of the microsphere surface and thus the sealing efficiency. Hence, the present data suggests helium pycnometry as a tool for assessment of coating quality in terms of sealing efficiency. This goes particularly for testing of products coated with water-soluble coatings, where dissolution testing obviously is compromised. The specific data on sealing efficiency might also add to other analytical methods in the analysis of coating quality, in general. End point densities of coated microspheres were seen to reveal differences in sealing efficiency between polymers. Measured densities of final products were also generally seen to reflect differences in coating permeability caused by variations in spray conditions. Thus, the measurement of density is a potential a tool for evaluation of spray conditions with respect to sealing of microspheres and identification of critical spray conditions.