A method for preparing uniquely sized nanoparticles of CaF2 by simultaneously spray drying a first NH4F and a biocompatible salt solution and a second Ca(OH)2 and biocompatible salt solution to form CaF2 solid particles in a soluble salt matrix wherein the salt is more soluble than CaF2. The salt matrix may then be dissolved and the separate CaF2 nanosized particles collected for use as a dental therapeutic material. The technique is useful in the preparation of other discrete, nanoparticle sized compounds and combinations by carefully choosing the solvents and solutes of the two spray dried solutions.