La FDA a adressé une mise en demeure à un fabricant de principe actif pour des manquements répétés à "l'intégrité des données" chromatographiques :
1. Failure to maintain complete and accurate laboratory test data generated in the course of establishing compliance of your APIs to established specifications and standards.
a. There was no written explanation for deletion events observed on audit trails for your standalone HPLC units. Your standard operating procedures (SOPs) did not include instructions for the retention of electronic raw data. In response to this letter, provide your procedures describing requirements to maintain complete data.
b. Your laboratory test data did not include records of the integration parameters used for any HPLC analyses.
c. There was incomplete raw data to support the test method validation/verification activities for the test methods used for your APIs. Your response should include new test method validation/verification data for the (b)(4) residual solvents testing that was requested during the inspection.
d. Our investigators identified the practice of performing trial injections for HPLC analyses prior to running the release and stability tests that are then reported. There was no justification for the practice of the trial preparations and injections.
Your response indicates that the practice has been stopped. Provide a comprehensive retrospective review and address any trial sample injections performed. Also provide an action plan that details how you plan to implement reliable laboratory controls to prevent the misuse or misidentification of test sample injections.
e. Our investigators identified calibration and media preparation records that were not authentic in that the persons that signed each record as having performed the activity were not at work on the day the work was accomplished.
Audit and identify the extent of this activity in your laboratory and manufacturing operations and provide an update to your investigation into this matter.
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