Thu, Apr 20, 2023 | 1:00 PM – 2:00 PM EDT

After the recall of valsartan in 2018 due to the presence of N-nitrosodimethylamine (NDMA), followed by the detection of nitrosamines in other drugs, the FDA released a Guidance for Industry for nitrosamine impurities, which covers conducting risk assessments and confirmatory testing of the finished drug, APIs, and/or raw materials. Since its publication, USP 1469 was also made official, offering a similar review of the information given by the FDA and also specific methodologies for the analysis of these drugs using GC/MS-MS and LC/MS-MS. In conjunction with a risk assessment, it can be advantageous to perform a screening for nitrosamines in the final drug, API, or raw materials. A test scheme is presented, using both GC/MS-MS and LC/MS-MS, for screening up to thirteen nitrosamines. The robustness of this scheme is demonstrated with a case study involving the screening of an over-the-counter tablet drug product. The tablet was selected as the sample for this example due to the inactive ingredients’ potential to pose analytical challenges, and how to overcome them.