Characterization of Impurities in Acarbose Hydrate by using LCMS/MS and NMR

An accurate and lively LC-MS/MS and NMR analytical methods have been developed for the recognition and characterization of key impurities in Acarbose. Acarbose is a diabetic medication used to treat Diabetes mellitus Type II and prediabetes in certain countries. Three unknown impurities were detected in Acarbose hydrate bulk drug substance using RP-HPLC method at RT 17.65 min, 18.4 min and 25.85 min. Such impurities have been separated by HPLC and are further characterized by the use of techniques LC-MS / MS and NMR. The C18 reverse phase column and Methanol and Ammonium Type analysis (80:20) have been conducted for the purpose of analysis. With an injection volume of 10 μL, the flow rate was maintained at 0,5mL / min. With binary gradient program, the separations were achieved and the column was kept at ambient temperature. The MS conditions adopted for this analysis with a scan range of m/z = 50 to 500 with a dwell time of 3 seconds. NMR was carried out using DMSO as solvent. Based on spectral data, the impurities have been characterized as IMP B, IMP D and IMP E.