Periodic Mesoporous Organosilicas (PMOs) have been successfully spray dried for the first time using a novel cyclic multifunctional organosilane molecule. By reducing the siloxane bridge formation both in the polymerisation and in the anchoring of the side groups an organic/ inorganic hybrid material was designed, depicting inherently improved chemical stability and much increased organic content. The spherical silica particles were applied as a hydrolytically stable stationary phase in reversed phase HPLC. They proved to be both highly retentive and stable in a pH range from 1.75 to 12 and up to 150 degrees C in 60 v% water. Both the backbone and the functionalities of the material exhibit this high stability.