Milling process for the production of finely milled medicinal substances

Abstract

The present invention is a method of milling materials to form a fine powder with a median particle size below 10 micrometer which is suitable for inhalation and which has substantially no amorphous content generated during milling. The method is particularly suitable for milling materials which are soft. The method comprises milling the material in a fluid energy mill at reduced temperature using helium, or helium mixed with another gas, as milling fluid. Temperatures of −30° C. or less are used.

1 . A method for producing a fine, highly crystalline material product, the method comprising fluid energy milling a crystalline material using a milling fluid comprising helium, wherein the temperature of the milling fluid is between −30° C. and −120° C.  
     
     
         2 . The method according to  claim 1 , wherein the milling fluid consists of helium.  
     
     
         3 . (canceled)  
     
     
         4 . The method according to  claim 1 , wherein the temperature of the milling fluid is between −50° C. and −70° C.  
     
     
         5 . The method according to  claim 1 , wherein the crystalline material comprises a medicament powder.  
     
     
         6 . (canceled)  
     
     
         7 . The method according to  claim 1 , wherein the product has an amorphous content of less than 5%.  
     
     
         8 . The method according to  claim 7 , wherein the product has an amorphous content of less than 2%.  
     
     
         9 . The method according to  claim 8 , wherein the product has an amorphous content of less than 1%.  
     
     
         10 . The method according to  claim 1 , wherein the product comprises a medicament powder in a form suitable for inhalation.  
     
     
         11 . The method according to  claim 10 , wherein the product has a median particle size of less than 10 microns.  
     
     
         12 . A crystalline material containing substantially no amorphous content and having a median particle size of less than 2 microns.  
     
     
         13 . The crystalline material according to  claim 12 , having a median particle size of about 1 micron.  
     
     
         14 . (canceled)  
     
     
         15 . The crystalline material produced by a method according to  claim 1 .  
     
     
         16 . The crystalline material according to  claim 15  containing substantially no amorphous content and having a median particle size of less than 2 microns.