Validation with Proprietary Compounds

The consequences for the scientific assessment of study validity did induce the European Medicines Evaluation Agency and its Committee for Proprietary Medicinal Products (EMEA/CPMP) to issue a draft guideline to deal with this problem of control sample contamination (CPMP, 2004). In this draft guideline reference is made to the GLP Principles and their requirement of fully, and truthfully, representing all results from a study, and the guideline stresses what is required for a GLP-compliant study report as follows The contamination of control samples with the test compound in toxicology studies shall be reported appropriately within a GLP statement as a deviation or violation. Contamination of controls should also be clearly acknowledged in the study reports and discussed by the Study Director with respect to its impact on the validity ofthe study. ... 

Other examples of cleaning validation have been reported, but identities of the compounds were withheld due to proprietary considerations. " Nevertheless, quantitative determination of residual APIs and intermediates on equipment surfaces were described in detail. The linear dynamic ranges for the compounds investigated were 0.1-1.0 pg/mL for one compound and 1-10 pg/mL for the others. With IMS technology, they were able to evaluate 30 samples in less than 2 h. In another study, analysis required only 0.5 min/sample compared with 15-30 min/sample using the HPLC method. ... 

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