RESUMO
A new high performance liquid chromatography [HPLC] method for the quantitative determination of sitagliptin in human plasma was developed and validated for pharmacokinetics study. The plasma was spiked with the internal standard [Salbutamol, IS], extracted with trichloro acetic acid. The extracted analyte was injected into a Symmetry ODS C18 column [250mm×4.5mm, 5m] and the flourometric detector was operated at 267 nm for excitation and 575 nm for emission. The mobile phase consisting of Potassium dihydrogen phosphate buffer pH [4.9]- Acetonitrile Methanol [30:50:20 v/v] at flow rate of 1.0mL/min. The method showed high specificity. Calibration curves of the peak area ratio of each analyte/IS versus sitagliptin concentration were linear in the range of 0.122-31.25 micro g/mL [r>0.989] for plasma and 0.012-25 ug/ml for QC solution[r>0.995]. The lower limit of quantification [LLOQ] was 0.122microg/mL in plasma and 0.012 in QC solution. The intraday and interday coefficient of variation was lower than 10%. The accuracy [relative recovery] at three levels was 100.95%, 101.03% and 97.79% respectively. The extraction recovery was 97.6%, 92.2% and 91.96% at the concentrations of 6.25, 25 and 100microg/mL, respectively. Short term and long term, freeze thaw stability of standard solutions and plasma samples were satisfactory. The optimized HPLC method was validated and proved to be specific, robust and accurate for determination of Sitagliptin in human plasma
RESUMO
In the present study, a series of N-substituted derivatives of 2-phenylethylamine has been synthesized. The reaction of 2-phenylethylamine [1] with benzene sulfonyl chloride [2] yielded N-[2-phenylethyl] benzenesulfonamide [3], which further on treatment with alkyl/acyl halides [4a-i] in the presence of sodium hydride furnished into Nsubstituted sulfonamides [5a-i]. These derivatives were characterized by IR, [1]H-NMR and EI-MS and then screened against acetyl cholinesterase [AChE], butyryl cholinesterase [BChE] and lipoxygenase enzyme [LOX] and were found to be potent inhibitors of butyryl cholinesterase only