CHARACTERIZATION AND VALIDATION OF IMPURITIES RELATED TO PHARMACEUTICAL BULK DRUG (API) BY USING SOME ANALYTICAL TECHNIQUES

Active Pharmaceutical Ingredient (API) of pharmaceutical bulk drug, four impurities were identified and were detected by a newly developed Reverse phase high performance liquid chromatographic (HPLC) method. The R.S.D.’s for SM-I, SM-II, SM- III and SM were found to be 1.48%, 1.71%, 1.67%, 6.37% respectively. These values are within the acceptance criteria of 10%.The limit of quantification values for SM-I, SM-II and SM-III were found to be 0.006 %, 0.006 %, and 0.006 % w.r.t. analyte concentration (500 μg /cm³), respectively. For determining method accuracy, known as unclean LOQ, the specified limit of 80%, 100% and 120% of the SM bulk sample (test preparation) was pointed. For confirming method precision six different test preparations of samples of SM were analyzed. Identified impurities were characterized by LC/MS/MS method. Identified impurities were unknown. Structural determination of such impurities was carried out by LC/MS/MS using electro spray ionization source and an ion trap mass analyzer. Structural identification by using nuclear magnetic resonance (NMR) and infrared (IR) spectroscopy.  The method was validated according to ICH guidelines with respect to Specificity, Precision, Accuracy, Linearity and Robustness.