A novel, simple, and sensitive Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the quantification of process-related impurities and degradants, as well as the assay of Docetaxel. ...A novel, simple, and sensitive Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the quantification of process-related impurities and degradants, as well as the assay of Docetaxel. The stability-indicating capability of the method was demonstrated through forced degradation studies and a comprehensive mass balance evaluation. Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column (100 × 2.1 mm, 1.7 µm), with gradient elution. The mobile phase A comprised a mixture of water, methanol, and acetonitrile (500:300:200, v/v/v), while mobile phase B was acetonitrile and water (800:200, v/v). The flow rate was set at 0.4 mL/min, with detection at 232 nm using a photodiode array detector. The method exhibited excellent performance, with a tailing factor of 1.10 for Docetaxel. The method was rigorously validated for precision, accuracy, linearity, LOD, LOQ, ruggedness, specificity, and robustness. Forced degradation studies confirmed the method’s suitability for stability analysis. Stability testing on the drug substance was conducted following ICH guidelines.展开更多
The objective of the present research work is to develop a gradient, reversed-phase liquid chromatographic (RP-UPLC) method for the determination of Finasteride in pharmaceutical bulk drugs for assay and its related i...The objective of the present research work is to develop a gradient, reversed-phase liquid chromatographic (RP-UPLC) method for the determination of Finasteride in pharmaceutical bulk drugs for assay and its related impurities. The chromatographic separation was achieved on a Waters ACQUITY UPLC BEH Phenyl Column (150 mm × 2.1 mm, 1.7 μm), The gradient LC method employs solutions A and B as mobile phase. The solution A Contains 2.5 mM ortho phosphoric acid (Buffer) and solution B contains a mixture of acetonitrile and water in the ratio of (90:10 v/v). The flow rate was 0.22 ml/min and the detection wavelength was 210 nm. In the developed UPLC method, the resolution between Finasteride and its potential impurities, namely Imp-1, Imp-2, Imp-3 and Imp-4 was found to be greater than 2.0. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. Considerable degradation was found to occur in alkaline medium and oxidative stress conditions. Degradation product formed during oxidative hydrolysis was found to be Imp-1. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 99.5%. The developed RP-UPLC method was validated with respect to linearity, accuracy, precision and robustness. The limit of quantification of Imp-1, Imp-2, Imp-3 and Imp-4 were 0.06, 0.06, 0.05 and 0.036% (of analyte concentration, i.e. 0.5 mg/ml) with 1μl injection volume. The developed method was found to be linear in the range of 2.5 - 15 μg/mL with correlation coefficient of 0.999 for assay procedures and found to be linear in the range of 0.05 - 3 μg/mL with correlation coefficient of 0.999 for related impurities.展开更多
文摘A novel, simple, and sensitive Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the quantification of process-related impurities and degradants, as well as the assay of Docetaxel. The stability-indicating capability of the method was demonstrated through forced degradation studies and a comprehensive mass balance evaluation. Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column (100 × 2.1 mm, 1.7 µm), with gradient elution. The mobile phase A comprised a mixture of water, methanol, and acetonitrile (500:300:200, v/v/v), while mobile phase B was acetonitrile and water (800:200, v/v). The flow rate was set at 0.4 mL/min, with detection at 232 nm using a photodiode array detector. The method exhibited excellent performance, with a tailing factor of 1.10 for Docetaxel. The method was rigorously validated for precision, accuracy, linearity, LOD, LOQ, ruggedness, specificity, and robustness. Forced degradation studies confirmed the method’s suitability for stability analysis. Stability testing on the drug substance was conducted following ICH guidelines.
文摘The objective of the present research work is to develop a gradient, reversed-phase liquid chromatographic (RP-UPLC) method for the determination of Finasteride in pharmaceutical bulk drugs for assay and its related impurities. The chromatographic separation was achieved on a Waters ACQUITY UPLC BEH Phenyl Column (150 mm × 2.1 mm, 1.7 μm), The gradient LC method employs solutions A and B as mobile phase. The solution A Contains 2.5 mM ortho phosphoric acid (Buffer) and solution B contains a mixture of acetonitrile and water in the ratio of (90:10 v/v). The flow rate was 0.22 ml/min and the detection wavelength was 210 nm. In the developed UPLC method, the resolution between Finasteride and its potential impurities, namely Imp-1, Imp-2, Imp-3 and Imp-4 was found to be greater than 2.0. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. Considerable degradation was found to occur in alkaline medium and oxidative stress conditions. Degradation product formed during oxidative hydrolysis was found to be Imp-1. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 99.5%. The developed RP-UPLC method was validated with respect to linearity, accuracy, precision and robustness. The limit of quantification of Imp-1, Imp-2, Imp-3 and Imp-4 were 0.06, 0.06, 0.05 and 0.036% (of analyte concentration, i.e. 0.5 mg/ml) with 1μl injection volume. The developed method was found to be linear in the range of 2.5 - 15 μg/mL with correlation coefficient of 0.999 for assay procedures and found to be linear in the range of 0.05 - 3 μg/mL with correlation coefficient of 0.999 for related impurities.
