Rapid detection of active pharmaceutical ingredients in drug products collected at an international mail facility by a satellite laboratory using a “toolkit” consisting of a handheld Raman spectrometer, portable mass spectrometer and portable FT-IR spectrometer

Abstract

A satellite laboratory “toolkit” consisting of a handheld Raman spectrometer, portable direct analysis in real-time mass spectrometer (DART-MS) and portable Fourier transform infrared (FT-IR) spectrometer was employed to examine 926 pharmaceutical, unknown and dietary supplement products collected at an international mail facility (IMF) for the presence of declared and undeclared active pharmaceutical ingredients (APIs) over the course of 68 working days. The toolkit successfully identified over 650 APIs, including over 200 unique APIs, using two or more devices. The performance of each individual device, and toolkit as a whole, were evaluated on all products and a subset of the products was forwarded to full-service laboratories for confirmatory analysis to determine false positive and false negative rates of the toolkit. The subset consisted of seven negative items (those not found to contain APIs using the toolkit) and 124 positive items (those found to contain at least one API using the toolkit). Overall, no false positives were detected in the negative items and only four false negatives and five false positives were detected in the positive items. Regarding the positive items, 119 of the 124 items were found to contain at least one API using at least two toolkit devices; each of these APIs were confirmed by a full-service laboratory. Furthermore, 90.2% of the APIs found by confirmatory laboratory analysis were detected by at least two toolkit devices. Based on these metrics and the fact that no false positives were detected by more than one device, it was concluded that when the toolkit detects and subsequently verifies/confirms an API using two or more devices, the results are as reliable as those generated by a full-service laboratory.