The objective of the current study was to develop a validated, specific and stability-indicating reverse phase liquid chromatographic method for the quantitative determination of fluocinonide and its related substance...The objective of the current study was to develop a validated, specific and stability-indicating reverse phase liquid chromatographic method for the quantitative determination of fluocinonide and its related substances. The determination was done for active pharmaceutical ingredient and its pharmaceutical dosage forms in the presence of degradation products, and its process-related impurities. The drug was subjected to stress condi- tions of hydrolysis (acid and base), oxidation, photolysis and thermal degradation per International Confer- ence on Harmonization (ICH) prescribed stress conditions to show the stability- indicating power of the method. Significant degradation was observed during acid, base hydrolysis, and peroxide degradation. The major degradants were identified by LC-MS, FTIR and 1H/13C NMR spectral analysis. The chromatographic conditions were optimized using an impurity-spiked solution and the samples generated from forced degra- dation studies. In the developed HPLC method, the resolution between fluocinonide and its process-related impurities, (namely imp-1, imp-2, imp-3, imp-4, imp-5, imp-6, imp-7 and imp-8) and its degradation products was found to be greater than 2.0.The chromatographic separation was achieved on a C18, 250 mm × 4.6 mm, 5 μm column. The LC method employed a linear gradient elution and the detection wavelength was set at 240 nm. The stress samples were assayed against a qualified reference standard and the mass balance was found to be close to 99.3%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness.展开更多
This research paper describes simple analytical method for determination of Camylofin dihydrochloride and Nimesulide in tablet formulation by Gas chromatography method. Benzoic acid was used as internal standard. Vali...This research paper describes simple analytical method for determination of Camylofin dihydrochloride and Nimesulide in tablet formulation by Gas chromatography method. Benzoic acid was used as internal standard. Validation was carried out in compliance with the International Conference on Harmonization guidelines. The method utilized GC (Agilent Technologies 6890 N Network GC system with FID detector), and RTX-5 capillary column (5% diphenyl-95% dimethyl polysiloxane), 30 m × 0.53 mm, 1.5 μm as stationary phase. Helium was used as the carrier gas at a flow rate of 1.5 mL?min–1. The proposed method was validated for linearity, LOD, LOQ, accuracy, precision, ruggedness and solution stability. It can be conveniently adopted for routine quality control analysis.展开更多
文摘The objective of the current study was to develop a validated, specific and stability-indicating reverse phase liquid chromatographic method for the quantitative determination of fluocinonide and its related substances. The determination was done for active pharmaceutical ingredient and its pharmaceutical dosage forms in the presence of degradation products, and its process-related impurities. The drug was subjected to stress condi- tions of hydrolysis (acid and base), oxidation, photolysis and thermal degradation per International Confer- ence on Harmonization (ICH) prescribed stress conditions to show the stability- indicating power of the method. Significant degradation was observed during acid, base hydrolysis, and peroxide degradation. The major degradants were identified by LC-MS, FTIR and 1H/13C NMR spectral analysis. The chromatographic conditions were optimized using an impurity-spiked solution and the samples generated from forced degra- dation studies. In the developed HPLC method, the resolution between fluocinonide and its process-related impurities, (namely imp-1, imp-2, imp-3, imp-4, imp-5, imp-6, imp-7 and imp-8) and its degradation products was found to be greater than 2.0.The chromatographic separation was achieved on a C18, 250 mm × 4.6 mm, 5 μm column. The LC method employed a linear gradient elution and the detection wavelength was set at 240 nm. The stress samples were assayed against a qualified reference standard and the mass balance was found to be close to 99.3%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness.
文摘This research paper describes simple analytical method for determination of Camylofin dihydrochloride and Nimesulide in tablet formulation by Gas chromatography method. Benzoic acid was used as internal standard. Validation was carried out in compliance with the International Conference on Harmonization guidelines. The method utilized GC (Agilent Technologies 6890 N Network GC system with FID detector), and RTX-5 capillary column (5% diphenyl-95% dimethyl polysiloxane), 30 m × 0.53 mm, 1.5 μm as stationary phase. Helium was used as the carrier gas at a flow rate of 1.5 mL?min–1. The proposed method was validated for linearity, LOD, LOQ, accuracy, precision, ruggedness and solution stability. It can be conveniently adopted for routine quality control analysis.
