Evaluation of “Toolkit” consisting of handheld and portable analytical devices for detecting active pharmaceutical ingredients in drug products collected during a simultaneous nation-wide mail blitz

• Published in: Journal of pharmaceutical and biomedical analysis Vol. 203; p. 114183
• Main Authors: Lanzarotta, Adam, Kern, Sara, Batson, JaCinta, Falconer, Travis M., Fulcher, Moseley, Gaston, Kirk W., Kimani, Martin M., Lorenz, Lisa, Morales-Garcia, Flavia, Ranieri, Nicola, Skelton, David, Thatcher, Michael D., Toomey, Valerie M., Voelker, Sarah, Witkowski, Mark R.
• Format: Journal Article
• Language: English
• Published: Elsevier B.V 05-09-2021
• Subjects: Drugs; FDA; FT-IR; Handheld; Portable; Raman; Drugs; Portable; FDA; MS; FT-IR; Raman; Handheld
• ISSN: 0731-7085; 1873-264X
• DOI: 10.1016/j.jpba.2021.114183

•Drug products were collected during a nationwide mail blitz.•Products were rapidly examined for APIs using a toolkit consisting of three portable devices.•The toolkit included a handheld Raman, a portable FT-IR and a portable DART-MS spectrometer.•92.0 % and 64.8 % of the APIs were detected using at least one device at least two devices, respectively.•Results may be used to support FDA action and/or prioritize additional lab-based analyses.
A “toolkit” consisting of a handheld Raman spectrometer equipped with a 1064 nm laser, a portable Fourier transform infrared (FT-IR) spectrometer and a portable direct analysis in real-time mass spectrometer (DART-MS) was employed in a laboratory setting to examine 82 representative products collected during a nationwide mail blitz for the presence of APIs. These results were compared to those obtained using laboratory-based methods; 8 of the products were not found to contain APIs and 74 of the products were found to contain a total of 88 APIs (65 of the 88 APIs were unique). The individual performance of each device and combined performance of the three-device toolkit were evaluated with regard to true positives, true negatives, false positives and false negatives. Using this toolkit, 81 (92.0 %) of the APIs were detected by at least one technique and 47 (64.8 %) of the APIs were detected by at least two techniques. Seven false negatives (8.0 %) were encountered and while the toolkit yielded 12 false positives, no false positives were detected by more than one technique. Overall, this study demonstrated that when the toolkit detects an API using two or more devices, the results are as reliable as those generated by a full-service laboratory.