Validation of 18 Analytical Methods to Support Pulmonary Product Development

22.06.16

Challenge

The client was developing a pMDI drug product with a complex multi-stage manufacturing  process  involving API re-crystallization and particle size reduction steps . Wide-ranging validated analytical methods (physical, solid-state, chromatographic) were required to release AP I at various stages of the manufacturing process and to support research activities.  Agenda 1  was  able to  deliver  all  required tests  from  its  single site  and  to  cGMP  with  rapid  turnaround  of results.

Response

Agenda 1 established and validated a suite of 18 analytical methods, these included particle size, XRPD, BET SSA, SEM, DSC, KF, FTIR, HPLC assay I impurities and GC (residual solvents), TAMC I TYMC and specified organisms, as well as standard compendial monograph tests; these were written into individual analytical methods, each of which was supported by validation I verification reports. The established methods were used to release test material from all stages of the manufacturing process (API raw material to finished product), and to carry out chemical and so lid-state stability and relaxation studies. Crucially, Agenda 1 supported manufacturing process development  by carrying out a range of lab-scale micronization studies with associated  analysis .

Outcome

The client was provided with cGMP validated  methods for  a wide range of  analysis  undertaken within a single-site facility. These methods continue to be used for release testing purposes as the product moves towards commercialization. The client went on to commission a similar project  involving  11  analytical methods for  a different  API .