Novel Analytical Method using Acquity QDa Mass Detector Coupled with LC-PDA for Impurity Profiling of Amlodipine Besylate and Olmesartan Medoxomil in Fixed Dose Tablets Formulation

Abstract

A novel impurity profiling technique for Amlodipine Besylate (ADB) and Olmesartan Medoxomil (OSM) in fixed dose combined tablets has been proposed by HPLC with Acquity Quadrupole Dalton analyser (QDa) mass detector coupled to photodiode array (PDA) detector. This online coupling technique has significant advantage over conventional HPLC techniques that mass and spectral characteristics can be evaluated simultaneously in a single run. The chromatographic separation was achieved on ACE C18 (250 x 4.6mm id, 5µ particle size) column with gradient mode using mobile phase composition of ammonium formate buffer, methanol and acetonitrile. Finalized flow rate was 1.0 mL/min with quantification of 237 nm. Moreover, identification of potential degradation product in stability condition samples was carried out by online coupling of PDA/QDa mass detection. This QDa mass spectrum reveals protonated molecular ion peak [M+H] + at m/z 875.5 for degradation product. This major degradation product was further characterized using MS/MS 2 integrated analytical tools. The method was validated systematically in terms of specificity, precision, linearity, accuracy, limit of detection (LOD), limit of quantification (LOQ) and robustness as per International conference on harmonization (ICH) general guidelines. This proposed study can provide a creative idea and effective method for routine analysis of ADB/OSM in tablet formulation in quality control department where impurity profiling as well as identification of unknown impurities can be evaluated simultaneously.

Impurity Profiling Impurity Profiling of Thiamine Hydrochloride Injection by Rp-HPLC and Characterization of Degradation Product by Lc-MS/MS/Qtof

“…The fragmentation profile was established on positive electrospray ionization (+ve ESI) mode with the following parameters; hexapole RF, capillary voltage 3000 v, cone voltage 25 v, source temperature at 120 °C, desolvation temperature 375 °C, ion energy 1.0 v and the collision energy was set to 8 v. For the MS/MS operation, argon was used as a collision gas with energy 25 v and mass spectra was acquired over an m/z range of 100-1000 range. The MS settings refer to a previous study [56]. The separation was performed on mass compatible HPLC method using Zorbax SB-Aq, 150 mm × 4.6 mm id, 5 µm particle size column (Agilent Corporation, USA) with mobile phase consists of 0.02 mol formate buffer with 0.1% formic acid and acetonitrile/0.02 mol formate buffer with 0.1% formic acid as solution A and B respectively.…”

LC–MS/MS and in silico analysis of pharmaceutical impurities in a combination drug for hypertension

“…Several methods have been reported to simultaneously determine HCT, AML, and OML in combined dosage form by HPLC [19][20] and UPLC [21]. Additionally, we evaluated the related substances for each combination of HCT, AML, and OLM [1,22].…”