Patent ID: 8128909

Claim:
A process for the preparation of sterile formulations in the form of aqueous suspensions for pulmonary administration by inhalation comprising a micronised crystalline beclomethasone dipropionate monohydrate as an active ingredient, the process comprising: i) preparing a solution of the active ingredient in ethanol in a suitable reactor (A); ii) sterilizing the solution by filtration; iii) in parallel, preparing a sterile aqueous phase containing suitable excipients in a turboemulsifier (B) and transferring the sterile aqueous phase to a suitable reactor (C); iv) adding the sterile organic solution to the sterile aqueous phase in a manner suitable to provide the active ingredient in crystalline form in a suspension; v) eliminating the ethanol; and vi) subjecting the aqueous suspension to a wet micronization treatment in a high pressure homogenizer (H) to further reduce the particle size of the active ingredient; wherein: at least 90% of the suspended particles of the active ingredient have a particle size of 6 μm or less; the temperature of the sterile aqueous phase is maintained at a temperature of between 10 and 25° C. and wherein the angles (±0.1°/2Φ) and relative intensities of the peaks (in brackets) of said crystalline beclomethasone dipropionate monohydrate are set out below 8.2 (85); 9.1 (13); 9.5 (12); 11.0 (21); 12.5 (39); 13.0 (13); 13.5 (6); 14.5 (100); 15.5 (20); 15.9 (20); 16.8 (25); 17.4 (16); 18.1 (22); 19.0 (23); 20.5 (11); 20.9 (9); 21.8 (19); 22.2 (14); 22.9 (18); 23.5 (11); 23.8 (18); 24.5 (13); 25.4 (14).