Enantiomeric separation and quantification of S-enantiomer of Tedizolid phosphate drug substance.... more Enantiomeric separation and quantification of S-enantiomer of Tedizolid phosphate drug substance. Material and method: A simple and sensitive reversed phase high performance liquid chromatography (RP-HPLC) method is developed by using-cyclodextrin (-CD) as a chiral mobile phase additive. Effect of the pH value of aqueous buffer, concentration of chiral additive, composition of mobile phase, and column temperature on the enantioseparation of Tedizolid phosphate was investigated on the Phenomenex Luna, Phenyl-Hexyl, 250 x 4.6mm, 5μm HPLC column. A satisfactory resolution was achieved at column temperature 20⁰C using a mobile phase consisting of a mixture of aqueous buffer of pH 7.0 of disodium hydrogen phosphate with additive-cyclodextrin, triethylamine and acetonitrile. This analytical method was evaluated by performing method validation as per ICH guideline. Results: The calibration curve was plotted within the concentration range between 0.30 and 2.25 µg mL −1 and the recoveries between 96.9 and 105.3% were obtained, with regression coefficient R 2 is 0.998. The limit of detection (LOD) and limit of quantitation (LOQ) of S-enantiomer of Tedizolid phosphate is 0.10 and 0.30 μg mL −1 Conclusion: The developed method was demonstrated to be accurate, robust and sensitive for the determination of enantiomeric purity of Tedizolid phosphate drug substance.
2,6-Dihydroxy-3-phenyldiazenylpyridine and 6-Amino-2-hydroxy-3-phenyldiazenylpyridine an impurity... more 2,6-Dihydroxy-3-phenyldiazenylpyridine and 6-Amino-2-hydroxy-3-phenyldiazenylpyridine an impurity formed in the process for the genitourinary antiseptic drug Phenazopyridine hydrochloride. Impurities were synthesized; characterized and reverse phase high-pressure liquid chromatography (HPLC) method has been developed and validated for estimation of related substances of Phenazopyridine hydrochloride active pharmaceutical ingredient (API). Efficient chromatographic separation was achieved on a Cosmosil 5μm particles size, 250mm × 4.6mm column. The method was validated for accuracy, precision, specificity, robustness, and detection and quantification limits, in accordance with ICH guidelines. Statistical analysis proved the method was precise, reproducible, selective, specific, and accurate for analysis of Phenazopyridine hydrochloride and its related impurities. HIGHLIGHTS Related substances method is developed for quantification of specified and unspecified impurities of Phenazopy...
Process related impurities associated with the synthesis of Hydralazine hydrochloride active phar... more Process related impurities associated with the synthesis of Hydralazine hydrochloride active pharmaceutical ingredient (API) was detected by high performance liquid chromatography (HPLC). The impurities are synthesized in laboratory and structure elucidation is done by mass spectrometry (MS), nuclear magnetic resonance spectroscopy (NMR) and infra-red spectroscopy (FTIR). Gradient HPLC method is developed for quantitation on Inertsil C18 column and validated for parameters such as specificity, accuracy, precision, linearity, robustness and ruggedness. The LOD and LOQ of all specified impurities are also determined.
Sertraline hydrochloride is an antidepressant of the selective serotonin reuptake inhibitor (SSRI... more Sertraline hydrochloride is an antidepressant of the selective serotonin reuptake inhibitor (SSRI) class, is synthesized for commercial use as a drug substance in highly pure form. During the synthetic process development studies of Sertraline hydrochloride, an impurity was detected in the final product at levels ranging from 0.05% to 0.15% in Gas Chromatography (GC) method and its molecular weight was determined by LC-MS analysis. The impurity was identified as 4-(4-chlorophenyl)-3,4-dihydronaphthalen-1(2H)-ol impurity, synthesized and characterized, the process of its formation was discussed in detail. After qualification of impurity standard, it was used as a reference standard for development of quantification by High Performance Liquid Chromatography (HPLC) method.
Objective: To develop a novel, simple, selective and enantiomeric separation of rivaroxaban by a ... more Objective: To develop a novel, simple, selective and enantiomeric separation of rivaroxaban by a chiral liquid chromatographic method as per ICH guidelines. Methods: An enantioselective reversed phase high performance liquid chromatographic method was developed and validated. The enantiomers of rivaroxaban was resolved on a Chiralcel OD-H (250 mm × 4.6 mm, 5 mm) column using a mobile phase system containing n-hexane –isopropanol (50: 50 v/v/) and column temperature at 35°C. The resolution between the enantiomers was not less than 2.0. The developed method was validated according to ICH guidelines. Results: The calibration curve was found to be linear over the concentration range of 0.075–1.2µg/mL (r 2 Conclusion: A novel, simple, selective and simple, selective and enantiomeric separation of rivaroxaban by a chiral liquid chromatographic method was developed as per ICH guidelines. = 0.9996). The limit of detection and limit of quantification of the (R)-enantiomer were found to be 0....
Enantiomeric separation and quantification of S-enantiomer of Tedizolid phosphate drug substance.... more Enantiomeric separation and quantification of S-enantiomer of Tedizolid phosphate drug substance. Material and method: A simple and sensitive reversed phase high performance liquid chromatography (RP-HPLC) method is developed by using-cyclodextrin (-CD) as a chiral mobile phase additive. Effect of the pH value of aqueous buffer, concentration of chiral additive, composition of mobile phase, and column temperature on the enantioseparation of Tedizolid phosphate was investigated on the Phenomenex Luna, Phenyl-Hexyl, 250 x 4.6mm, 5μm HPLC column. A satisfactory resolution was achieved at column temperature 20⁰C using a mobile phase consisting of a mixture of aqueous buffer of pH 7.0 of disodium hydrogen phosphate with additive-cyclodextrin, triethylamine and acetonitrile. This analytical method was evaluated by performing method validation as per ICH guideline. Results: The calibration curve was plotted within the concentration range between 0.30 and 2.25 µg mL −1 and the recoveries between 96.9 and 105.3% were obtained, with regression coefficient R 2 is 0.998. The limit of detection (LOD) and limit of quantitation (LOQ) of S-enantiomer of Tedizolid phosphate is 0.10 and 0.30 μg mL −1 Conclusion: The developed method was demonstrated to be accurate, robust and sensitive for the determination of enantiomeric purity of Tedizolid phosphate drug substance.
2,6-Dihydroxy-3-phenyldiazenylpyridine and 6-Amino-2-hydroxy-3-phenyldiazenylpyridine an impurity... more 2,6-Dihydroxy-3-phenyldiazenylpyridine and 6-Amino-2-hydroxy-3-phenyldiazenylpyridine an impurity formed in the process for the genitourinary antiseptic drug Phenazopyridine hydrochloride. Impurities were synthesized; characterized and reverse phase high-pressure liquid chromatography (HPLC) method has been developed and validated for estimation of related substances of Phenazopyridine hydrochloride active pharmaceutical ingredient (API). Efficient chromatographic separation was achieved on a Cosmosil 5μm particles size, 250mm × 4.6mm column. The method was validated for accuracy, precision, specificity, robustness, and detection and quantification limits, in accordance with ICH guidelines. Statistical analysis proved the method was precise, reproducible, selective, specific, and accurate for analysis of Phenazopyridine hydrochloride and its related impurities. HIGHLIGHTS Related substances method is developed for quantification of specified and unspecified impurities of Phenazopy...
Process related impurities associated with the synthesis of Hydralazine hydrochloride active phar... more Process related impurities associated with the synthesis of Hydralazine hydrochloride active pharmaceutical ingredient (API) was detected by high performance liquid chromatography (HPLC). The impurities are synthesized in laboratory and structure elucidation is done by mass spectrometry (MS), nuclear magnetic resonance spectroscopy (NMR) and infra-red spectroscopy (FTIR). Gradient HPLC method is developed for quantitation on Inertsil C18 column and validated for parameters such as specificity, accuracy, precision, linearity, robustness and ruggedness. The LOD and LOQ of all specified impurities are also determined.
Sertraline hydrochloride is an antidepressant of the selective serotonin reuptake inhibitor (SSRI... more Sertraline hydrochloride is an antidepressant of the selective serotonin reuptake inhibitor (SSRI) class, is synthesized for commercial use as a drug substance in highly pure form. During the synthetic process development studies of Sertraline hydrochloride, an impurity was detected in the final product at levels ranging from 0.05% to 0.15% in Gas Chromatography (GC) method and its molecular weight was determined by LC-MS analysis. The impurity was identified as 4-(4-chlorophenyl)-3,4-dihydronaphthalen-1(2H)-ol impurity, synthesized and characterized, the process of its formation was discussed in detail. After qualification of impurity standard, it was used as a reference standard for development of quantification by High Performance Liquid Chromatography (HPLC) method.
Objective: To develop a novel, simple, selective and enantiomeric separation of rivaroxaban by a ... more Objective: To develop a novel, simple, selective and enantiomeric separation of rivaroxaban by a chiral liquid chromatographic method as per ICH guidelines. Methods: An enantioselective reversed phase high performance liquid chromatographic method was developed and validated. The enantiomers of rivaroxaban was resolved on a Chiralcel OD-H (250 mm × 4.6 mm, 5 mm) column using a mobile phase system containing n-hexane –isopropanol (50: 50 v/v/) and column temperature at 35°C. The resolution between the enantiomers was not less than 2.0. The developed method was validated according to ICH guidelines. Results: The calibration curve was found to be linear over the concentration range of 0.075–1.2µg/mL (r 2 Conclusion: A novel, simple, selective and simple, selective and enantiomeric separation of rivaroxaban by a chiral liquid chromatographic method was developed as per ICH guidelines. = 0.9996). The limit of detection and limit of quantification of the (R)-enantiomer were found to be 0....
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