Summer 2009 Newsletter
Case Study: Possible Product Recall
A food manufacturer found a broken pill capsule in a can of nuts and needed to know if they had to issue a product recall. In addition to identifying the unknown pill, they were concerned with potential acute and chronic toxicity via oral ingestion. Time was of the essence and Chemir’s scientists were called into action over a holiday weekend.
Analytical Techniques
The combination of data collected from a spectrum of analytical techniques and instrumentation allowed for the identification of the unknown pill.
A visual examination of the unknown pill did not reveal any identifying markers. Portions of the pill sample were prepared for a variety of analyses. Fourier Transform Infrared Spectroscopy (FTIR) revealed the presence of a cellulose derivative and stearic acid. Cellulose and stearic acid deriviatives are often used in pharmaceutical formulations as excipients (inactive substances used as carrier ingredients or stabilizers).
Proton Nuclear Magnetic Resonance Spectroscopy (1H NMR) and Scanning Electron Microscopy with Energy Dispersive X-Ray Analysis (SEM/EDXA) did not allow for a positive identification of any components of the pill. However, the observation of silicon in the SEM/EDXA data suggested a silica-based (SiO2) excipient in the formula.
The contents of the pill determined thus far are very common in pharmaceuticals and could not help identify the active ingredient. Chemir scientists had to delve deeper…
Gas Chromatography with Mass Spectrometry Detection (GC/MS) confirmed the presence of stearic acid. Another broad peak in the chromatogram with a parent ion at m/z 317 was observed. A thorough search of mass spectral databases did not suggest a reasonable identity for this peak.
Finally, our experts were able to identify the unknown material using Liquid Chromatography with Mass Spectrometry Detection (LC/MS). They observed a parent molecular ion. It was sequentially fragmented in the ion-trap MS to provide daughter ions. One of the daughter ions was the same one observed in the previous GC/MS experiment, m/z 317. A thorough search of scientific literature allowed for the identification of the unknown as a specific fluoroquinolone antibiotic.
Outcome
Chemir’s laboratory results were provided to a toxicologist who prepared a toxicology risk assessment outlining any potential hazards of ingesting this medication. The project, from receipt of samples to toxicology report, was complete within 2 days. The quick, yet thorough analysis over a holiday weekend allowed our client to make an informed decision about whether to issue a product recall.
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