A rapid, specific, sensitive, and precise reverse-phase HPLC method for the quantitative determination of process related and degradation impurities of Apixaban, an anticoagulant drug is described. The developed RP-HP...A rapid, specific, sensitive, and precise reverse-phase HPLC method for the quantitative determination of process related and degradation impurities of Apixaban, an anticoagulant drug is described. The developed RP-HPLC method was successfully applied to the analysis of both Apixaban drug substance and drug product. The chromatographic separation was achieved on a Sigma-Aldrich’s Ascentis Express®C18 (4.6 mm × 100 mm, 2.7 μ) HPLC column with a runtime of 40 min. Mobile phase-A and mobile phase-B were phosphate buffer and acetonitrile respectively. The column oven temperature was set at 35°C and photodiode array detector was set at 225 nm. Nine process related impurities (Imp-1 to Imp-9) have been detected in test sample of Apixaban by using newly developed RP-HPLC method. Forced degradation study was carried out under acidic, alkaline, oxidative, photolytic and thermal conditions to demonstrate the stability-indicating nature of the developed RP-HPLC method. The developed method was validated as per ICH guideline and found to be specific, precise, sensitive and robust.展开更多
A new, specific, rapid and stability indicating reversed phase liquid chro-matographic (RP-LC) method for the determination of process related and degradation related impurities of Apremilast has been developed and va...A new, specific, rapid and stability indicating reversed phase liquid chro-matographic (RP-LC) method for the determination of process related and degradation related impurities of Apremilast has been developed and validated. The degradation study performed in acid, base, oxidative, photolytic, and thermal stressed conditions. Eight process related impurities (Imp-1 to Imp-8) in test sample of Apremilast have been detected by developed RP-LC method. The good chromatographic resolution between the peaks of process related impurities, degradation impurities and Apremilast has been achieved on a Synergi Max-RP 80 A (150 × 4.6 mm ID), 4 μ column. The process and degradation related impurities were characterized by mass spectrometry, 1H NMR and FT-IR spectral data. The method was validated as per ICH guideline and found to be specific, rapid, and stability indicating. The proposed RP-PLC method was successfully applied to the analysis of drug substance samples of Apremilast.展开更多
A rapid, specific, sensitive, and precise reverse-phase UPLC method developed for the quantitative determination of an atypical antipsychotic drug Iloperidone and its eight potential impurities in drug substances and ...A rapid, specific, sensitive, and precise reverse-phase UPLC method developed for the quantitative determination of an atypical antipsychotic drug Iloperidone and its eight potential impurities in drug substances and drug products is described in this report. Chromatographic separation was achieved on a Waters Acquity UPLC®HSS C18 (2.1 mm × 100 mm, 1.8 micron) column thermostated at 35°C with a short runtime of 10 min. Quantification is achieved with photodiode array detection at 225 nm over the concentration range of 0.03 - 0.15 μg/mL. Forced degradation study was carried out under acidic, alkaline, oxidative, photolytic and thermal conditions to demonstrate the stability-indicating capability of the developed UPLC method. Comparison of system performance with conventional high-performance liquid chromatography is made with respect to analysis time, efficiency, and sensitivity. The method is validated according to the ICH guidelines and is applied successfully for the determination of Iloperidone in tablets.展开更多
文摘A rapid, specific, sensitive, and precise reverse-phase HPLC method for the quantitative determination of process related and degradation impurities of Apixaban, an anticoagulant drug is described. The developed RP-HPLC method was successfully applied to the analysis of both Apixaban drug substance and drug product. The chromatographic separation was achieved on a Sigma-Aldrich’s Ascentis Express®C18 (4.6 mm × 100 mm, 2.7 μ) HPLC column with a runtime of 40 min. Mobile phase-A and mobile phase-B were phosphate buffer and acetonitrile respectively. The column oven temperature was set at 35°C and photodiode array detector was set at 225 nm. Nine process related impurities (Imp-1 to Imp-9) have been detected in test sample of Apixaban by using newly developed RP-HPLC method. Forced degradation study was carried out under acidic, alkaline, oxidative, photolytic and thermal conditions to demonstrate the stability-indicating nature of the developed RP-HPLC method. The developed method was validated as per ICH guideline and found to be specific, precise, sensitive and robust.
文摘A new, specific, rapid and stability indicating reversed phase liquid chro-matographic (RP-LC) method for the determination of process related and degradation related impurities of Apremilast has been developed and validated. The degradation study performed in acid, base, oxidative, photolytic, and thermal stressed conditions. Eight process related impurities (Imp-1 to Imp-8) in test sample of Apremilast have been detected by developed RP-LC method. The good chromatographic resolution between the peaks of process related impurities, degradation impurities and Apremilast has been achieved on a Synergi Max-RP 80 A (150 × 4.6 mm ID), 4 μ column. The process and degradation related impurities were characterized by mass spectrometry, 1H NMR and FT-IR spectral data. The method was validated as per ICH guideline and found to be specific, rapid, and stability indicating. The proposed RP-PLC method was successfully applied to the analysis of drug substance samples of Apremilast.
文摘A rapid, specific, sensitive, and precise reverse-phase UPLC method developed for the quantitative determination of an atypical antipsychotic drug Iloperidone and its eight potential impurities in drug substances and drug products is described in this report. Chromatographic separation was achieved on a Waters Acquity UPLC®HSS C18 (2.1 mm × 100 mm, 1.8 micron) column thermostated at 35°C with a short runtime of 10 min. Quantification is achieved with photodiode array detection at 225 nm over the concentration range of 0.03 - 0.15 μg/mL. Forced degradation study was carried out under acidic, alkaline, oxidative, photolytic and thermal conditions to demonstrate the stability-indicating capability of the developed UPLC method. Comparison of system performance with conventional high-performance liquid chromatography is made with respect to analysis time, efficiency, and sensitivity. The method is validated according to the ICH guidelines and is applied successfully for the determination of Iloperidone in tablets.
