A liquid chromatography tandem mass spectrometry (LC-MS/MS) based method was developed for the simultaneous monitoring plasma levels of Sitagliptin (STG) and Pioglitazone (PIO) for applicability to pharmacokinetic studies. The method was based on HPLC separation on the reversed phase Phenomenex Synergy C 18 column (30 mm length, 4.6 mm internal diameter, and 4.0 μm particle size) at a temperature of 40˚C using a binary gradient mobile phase consisting of methanol and 2 mM ammonium acetate buffer pH adjusted to 4.5 with acetic acid, at a flow rate of 1 mL·min −1. Tolbutamide was used as an internal standard. Detection of analytes was achieved with LC-MS/MS system in Multiple Reaction Monitoring (MRM) mode. The method was validated over concentration range of 10.98 -2091.77 ng·mL −1 for SIT and 8.25 -1571.63 ng·mL −1 for PIO and lower limit of quantification was 10.98 ng·mL −1 and 8.25 ng·mL −1 for STG and PIO respectively. Recoveries from spiked controls were within acceptance criteria for all the analytes and internal standard at all QC levels. Within batch and between batch accuracy for STG was found within 96.9% -100.3% and for PIO was found within 100.0% -104.3%. Within batch and between batch precision for STG was less than 3.1% CV (coefficient of variation) and for PIO was less than 5.3% CV at all concentrations levels. This method was successfully applied to monitor pharmacokinetics profile of both STG and PIO on simultaneous oral administration to rats. This method can be applicable for pharmacokinetic drug-drug interaction studies.
Objective: To develop and validated a new stability indicating reverse phase high performance liquid chromatography (RP-HPLC) method for analysis of naftopidil (NAF), both as a bulk drug and in formulation. Method: The separation was achieved using a C18 GRACE column (250 mm × 4.6 mm i.d., 5 μm particle size) and gradient mobile phase system consisting of (A) 10 mM of ammonium acetate buffer pH adjusted to 4.0 with glacial acetic acid and (B) acetonitrile. The fl ow rate was 1.0 mL/ min with UV detection at 284 nm. NAF was subjected to stress conditions like hydrolysis (acid, alkali and neutral degradation), oxidation, photolytic and thermal decomposition. The linearity of the proposed method was investigated in the range of 10-150 μg/mL. Application of design of experiments for the robustness study method was carried out, where in fi ve factors was selected: pH of mobile phase, fl ow rate, strength of the buffer and column temperature. These factors were examined using JMP@ (SAS Institute) software. Result: The analytical method for NAF was developed and validated at the linearity range of 10-150 μg/mL. The LOD and LOQ were 0.6 and 2.04, respectively and accuracy of analysis was 100.5-101.1%. Conclusion: A robuststabilityindicating HPLC assay method was developed using DOE, for the quantitation of NAF in its bulk and tablet dosage forms
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