METHOD VALIDATION FOR DETERMINATION OF HEAVY METALS IN PHYTONADIONE EMULSION (I.M) DOSAGE FORMS BY ICP-MS

The analysis of pharma samples by ICP-MS is challenging due to their high carbon content. Because they are organic based and have a variety of compositions, present a special challenge for ICP-MS analysis: the carbon causes polyatomic interferences and can clog interface cone. Using the NexION™ 300 ICP-MS, several pharma compounds (ranging from API’s to finished products) were successfully analyzed as per USP232 limits using a single set of calibration standards and operating conditions, demonstrating a validation process for the simultaneous analysis of 7 elements, arsenic (As), cadmium (Cd), mercury (Hg), lead (Pb), chromium (Cr), copper (Cu) and nickel (Ni), in phytonadione emulsion samples by inductively coupled plasma-mass spectrometry (ICP-MS) after closed-vessel microwave digestion.Phytonadione (vitamin K?) the most essential and widely used therapeutic agent in treatment of prophylaxis of haemorrhagic disease of the newborn is considered. This validation as per USP233 was realized in parallel with the analysis of the different brands of commercially available phytonadione emulsion samples of Several criteria such as linearity, limits of detection (LOD), limits of quantification (LOQ), precision under repeatability conditions and accurate results were evaluated. Results indicate that this method could be used in the laboratory for the routine determination of metal impurities in pharmaceutical preparations with acceptable analytical performance. The technique was applied not only for determination of metallic impurities but also the assay of various trace elements in pharmaceuticals.