The development of analytical procedures using ICP-OES and ICP-MS for the analysis of trace metals in pharmaceutical formulations

摘要

New regulations regarding elemental impurities in pharmaceuticals will be implemented in January 2018 and the guidelines include the use of inductively coupled plasma optical emission spectroscopy (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). In this work, a method using each instrument was developed for the analysis of arsenic (As), cadmium (Cd), mercury (Hg), lead (Pb), cobalt (Co), nickel (Ni) and vanadium (V) and validated to meet the international conference of harmonisation (ICH Q3D) guidelines. Liquid and solid samples were prepared using microwave assisted acid digestion method that was developed using reverse aqua regia. The results obtained from the validation showed good linearity (R2>0.995) with low limits of detections (LODs) and limits of quantifications (LOQs). The percentage recoveries for both the standard reference material (SRM) and the spiked samples were between 95-105% with relative standard deviation (RSD) of less than 5. Cold symptoms relief products were purchased and analysed. Levels of Pb and Cd in certain products were found to exceed the permitted daily exposure limit (PDE) when the maximum dose was taken.