Development and Validation of Stability Indicating RP-HPLC Method for Determination of Safinamide Mesylate (original) (raw)
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Eurasian Journal of Analytical Chemistry, 2016
Dabigatran etexilate mesylate is an anticoagulant drug. Dabigatran demonstrated its efficacy for prophylaxis and treatment of thromboembolic event during orthopaedic surgery and curative treatment of hypercoagulability in atrial fibrillation. The present study deals with the development and validation of a stability-indicating high performance thinlayer chromatography (HPTLC) method for the estimation of Dabigatran etexilate mesylate using TLC plates precoated with silica gel 60 F254 as stationary phase and toluene: ethyl acetate: methanol: formic acid (3:4:3:0.2, v/v/v/v) as the mobile phase. The drug was subjected to stress conditions such as hydrolysis, oxidation, photolysis, neutral and dry heat. Degradation products produced as a result of the stress conditions did not interfere with the detection of DEM, therefore the proposed method can be considered stabilityindicating. DEM showed degradation under hydrolytic, oxidative, photolytic and dry heat conditions. DEM (Rf 0.47 ± 0.02) and its degradation products were well resolved. The wavelength selected for quantitation was 314 nm. The method was linear in the concentration range 50-250 ng/spot with a correlation coefficient of 0.9955. The %RSD for repeatability of peak area measurement was found to be 0.62 and %RSD for repeatability of sample application was found to be 0.75. The % RSD of intraday and interday precisions were 0.91-1.5 and 1.21-1.7 respectively. The accuracy (recovery) was found to be in the range of 99.45-100.37 %. The developed method was applied for assay of marketed formulations and the results were found to be good agreement with labelled claim of formulations.
International Journal of Pharmacy and Pharmaceutical Sciences, 2015
Objective: To develop and validate stability indicating HPTLC method for determination of Dolasetron mesylate. Methods: The chromatographic separation was performed on aluminium plates precoated with silica gel 60 F254 Results: The chromatographic condition gave a compact spot for Dolasetron mesylate at Rf value of 0.65±0.03. Stress testing was performed in accordance with international conference on harmonization (ICH) Q1A R2 guidelines. Method was validated as per ICH Q2 R1 guidelines. The calibration curve was found to be linear in the concentration range of 100-800 ng/band for Dolasetron mesylate. The limit of detection and quantification was found to2.24 ng/band and 6.79 ng/band, respectively. using Methanol: Choloroform: Ethyl acetate (7:2:1 v/v/v) as mobile phase followed by densitometric scanning at 280 nm. Conclusion: A new sensitive, simple, and stability indicating high performance thin layer chromatographic (HPTLC) method has been developed and validated for determination of Dolastron mesylate. The proposed method can be used for routine determination of Dolasetron mesylate stability.
International Journal of Advances in Pharmaceutical Research, 2015
In the present study, two analytical methods were developed for the estimation of Mebeveverine Hydrochloride in tablet dosage form. Method A: UV Spectroscopic method, This method is based on dissolving the drug in ethanol (95%) and further dilutions with water and the measurement of absorbance of Mebeverine hydrochloride at 263nm. Beer's law was obeyed in concentration range 20-50mcg/ml with correlation coefficient value 0.996. The % RSD values in the precision studies, for intra and inter-day analysis, analyst-to-analyst variation reveals that the % RSD of assay results were less than 2.0. Method B: HPLC In HPLC method has been developed for the estimation of Mebeverine hydrochloride using Xterra C18 column (150 X 4.6 mm, 5μ), with mobile phase Acetonitrile: Water: TEA in the ratio of 70:25:5 (v/v/v) at flow rate of 1mL/min using UV detection at 260nm. The method was selective and linear between concentration range 10-50μg/mL, with correlation coefficient 0.999. LOD and LOQ values were found to be 0.102μg/ml and 0.311μg/ml respectively. Mobile phase pH 6.0. Run Time was 7.0min. The calculated % recovery was found as 99.80 to 100.53 at three different levels (50,100 and 120%) which confirms the accuracy for the developed method Both method was validated were validated for different validation parameters like Precision, Linearity, Accuracy, LOD, LOQ Ruggedness and Robustness as per ICH Guidelines. The validated methods were successfully applied to the commercially available pharmaceutical dosage forms, yielding very good and reproducible result.
The core aim of present work was to develop a simple, precise, rapid and reproducible isocratic reverse phase high performance liquid chromatographic (RP-HPLC) method for the estimation of Amisulpride (AMS) in pure and in tablet dosage form. An isocratic RP-HPLC was performed on a Phenomenex C 18 column (250 x 4.6 mm, 5 micron size column, ambient temperature with mobile phase containing phosphate buffer duly adjusted to pH 4.1 with ortho phosphoric acid and acetonitrile in the ratio of 80:20 v/v. The flow rate was 1 mL/min and eluent was monitored at 227 nm. The chromatogram of AMS was found that the retention time is 5.601 min. The proposed method was linear to the concentration verses peak area responses which was found in the range of 2-10 µg/mL with R 2 value of 0.9999. The reproducibility results of AMS were observed to be % 0.039 (% RSD) which speaks that this method can be reproducible for different tablets. The % RSD values were found to be less than 2 within the limit The percentage recoveries of active pharmaceutical ingredient from dosage forms ranged from 99.53 to 99.72 which indicate that the proposed method to be an accurate. The LOD and LOQ were found to be 0.0175 and 0.0577 respectively. The positive results of robustness of this method permits for extensive application for analysis of drugs. The % assay values for Sulpitac and Solian are 99.16±0.21and 99.85±0.11respectively. This method was specific as no interferences were detected at its retention time of peak drug. Therefore this RP-HPLC method is highly convenient, accurate, precise and economical with less retention time and can be used for the routine determination of AMS in pharmaceutical dosage form.
A simple, linear gradient, rapid, precise and stability-indicating RP-UPLC method was developed for the determination of Cloxacillin Sodium in its bulk form and formulation. Ultra performance liquid chromatography, a most promising advancement in a world of chromatography, reduces analysis time, increases reliability through higher resolution, sensitivity and selectivity as well as used as an economic method due to reducing solvent consumption. A chromatographic separation of a drug as well as its degradants was achieved using Waters acquity BEH, 2.1 3 100 mm, 1.7 mm C 18 column with gradient of mobile phase A: phosphate buffer, pH 6.8 and mobile phase B: methanol:acetonitrile (75:25). The drug and degradants were monitored at a detection wavelength of 225 nm with a flow rate of 0.35 mL/min and an injection volume of 10 mL. The temperature of the column and auto sampler compartments was at 308 8 8 8 8C and 258 8 8 8 8C + + + + + 18 8 8 8 8C, respectively. The retention time of the drug was ∼6.9 min. The resolution of the drug and degradant peak was >1.5 in all cases. Force degradation of CLOX SOD was carried under alkaline, acidic, oxidative, thermal, photo degradation conditions and it was analyzed by the proposed method. The drug degrades under alkaline, acidic and oxidative conditions but was stable in temperature and light. A developed method was validated as per ICH guidelines using validation parameters such as precision, linearity and range, limit of quantification, specificity, assay and robustness. Preparation of solutions An accurately weighed 50 mg of CLOX SOD API was transferred into a 100 mL-volumetric flask. First, it was dissolved in 50 mL buffer and sonicated, then diluted up to the mark with buffer to get the concentration of CLOX SOD (500 mg/mL). Concentrations ranging from 0.025 to 75 mg/mL for CLOX SOD were prepared from stock solution and different validation parameters were performed. Validation procedure Validation of the newly developed method was studied in terms of linearity and range, precision, accuracy, robustness, limit of