19
Figure 2: HPIC chromatograms acquired for nitrite standard, test material and spiked sample. Presence of chloride peak may affect accuracy of method and alternative detection would be recommended.
analysis allows manufacturers to understand which products are more susceptible to nitrosamine formation and risk assess accordingly.
Case Study: Detection of counterfeit
pharmaceutical products The presence of fraudulent healthcare products in the open market is a serious concern for manufacturers and regulators alike, jeopardising brand reputation and costing companies millions in lost revenue; most crucially, they pose a serious risk to patient safety. The identifi cation and subsequent analytical investigations play a major role in tracking down and bringing perpetrators to justice. Analytical assessments often work up in complexity, focussing fi rst on any obvious differences in packaging or printing, either visually or using light microscopy. Spectroscopy-based techniques, such as FTIR and Raman, are also used to compare dyes and adhesives present on suspect products with those used on their genuine counterparts. More advanced techniques can also be used to understand microstructure similarity; for example, X-ray tomography can assess the uniformity of tablet coating. In terms of chemical analysis, non-targeted methods of profi ling the product itself should be implemented, allowing conclusions to be drawn regarding similarity of the suspect sample to the genuine, as well as the presence of any potentially harmful compounds. Techniques should be carefully selected to ensure both organic and inorganic components are profi led, for example a combination of energy dispersive X-ray spectroscopy and NMR or FTIR could be employed (Figure 3). On occasions, the chemical difference between a genuine and fraudulent product could be subtle, however it is still possible that a product has been manufactured with lower grade excipient material, meaning the resulting product will not pass high regulatory standards. In these cases, specifi c differences in materials may need to be targeted; for example, the difference in pharmaceutical grade cellulose and a lower quality material can be identifi ed by looking at degree of crystallinity, either using solid state NMR or powder XRD.
H NMR spectra of genuine and suspected fraudulent healthcare product, showing absence of API signals but also differences in excipient profi le.
Figure 3: 1 Conclusion
The identifi cation of impurities and contaminants, whether inherent to the matrix or the result of external factors, are critical in assuring continued patient safety. One technique alone will seldom provide all the necessary information to either fully elucidate, or to allow the necessary risk assessment to be undertaken. The list of analytical techniques in the modern laboratory environment can be extensive, so it is important to consider whether any particular technique will provide suffi cient selectivity or sensitivity, or whether additional sample preparation steps need to be implemented prior to analysis. Finally, when assessing the impact of a contamination or possible fraudulent product, it is necessary to harness non-targeted methodologies to ensure no potentially harmful components to patients are missed.
About the author
Dr Catherine Frankis is a Senior Scientist II at RSSL who works across the Functional Ingredients and Investigative Analysis teams, specializing in ion exchange chromatography and nuclear magnetic resonance spectroscopy. Frankis works on projects covering a wide variety of issues, including contamination, adulteration, and the development and validation of new analytical methods within the food, pharmaceutical, and cosmetic industries. In 2010, Frankis joined RSSL after completing her PhD in the synthesis and characterisation of stereoselective biopolymer initiators at the University of Bath, where she used a variety of analytical characterisation and thermal property techniques.
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