(565a) Residence Time Distribution and Segregation Studies Trough Real Time Measurements By Near Infrared Spectroscopy
AIChE Annual Meeting
2017 Annual Meeting
Pharmaceutical Discovery, Development and Manufacturing Forum
PAT for Process Understanding, Reduced Testing, and Elucidation of Fundamental Phenomena in Drug Product/Substance Development
Wednesday, November 1, 2017 - 12:35pm to 12:55pm
RTD characterization was performed through in-line measurements by near infrared (NIR) spectroscopy of changes in composition adding a pulse of tracer into the system. Each material used was analyzed by using a continuous blending setup consisting in one feeder connected to a GEA continuous blender through a hopper. At the blender outlet, a chute was connected with a lateral window to control the level of powder with a rotary valve. Perpendicular to the powder flow, a near infrared probe with the light source was connected for spectral acquisition in diffuse reflectance mode. The reflected light is transferred to the interferometer for processing through fiber optic. Six experiments for each material has been performed at tow flow rates and 3 impeller speeds (revolution per minute (RPM)). A second feeder was necessary in cases where low density exceeds the gear capacity of a single feeder setup. Results of in-line RTD measurements demonstrated the selectivity of calibration models and low limit of detection required for analysis of tracers providing critical information for blender characterization.
Segregation studies were conducted for five formulations in continuous blending. For each configuration in blender RPM, samples were collected for further analysis in an ASTM D 6940-04 segregation tester. Near infrared prediction of ten samples collected for each experiment were performed by using 1-Dimentional sampling approach. Calibration models for each formulation were prepared and implemented. Results indicates that each blender configuration has a different impact in the segregation behavior of the API concentration and the NIR method provided a fast and reliable results.
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