scholarly journals Development and Validation of Stability Indicating RP-HPLC Method for the Determination of Metaxalone in Bulk and its Pharmaceutical Formulations

2011 ◽  
Vol 8 (s1) ◽  
pp. S439-S447 ◽  
Author(s):  
Prafulla Kumar Sahu ◽  
M. Mathrusri Annapurna ◽  
Sahoo Dillip Kumar
Keyword(s):  
Dynamic Range ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Standard Curve ◽  
Oxidation Reduction ◽  
Development And Validation

A stability indicating reverse phase HPLC method was developed for the determination of metaxalone, a skeletal muscle relaxant, present in bulk and its pharmaceutical formulations using gliclazide as the internal standard (I.S). A hypersil ODS C18 column (250 × 4.6 mm, packed with 5 micron) in an isocratic mode with mobile phase Acetonitrile: phosphate buffer 3.6 (50:50%v/v) was used at a flow rate of 0.8 mL/ min and effluent was monitored at 225 nm. The assay exhibited a linear dynamic range of 0.6-100 µg/mL. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. The retention times were 5.13 min and 9.08 min for metaxalone and IS respectively. The extraction recovery of metaxalone from pharmaceutical dosage form (tablets) was >97% and the calibration curve was linear (r2= 0.999) over the entire linear range. The method had an accuracy of >98% and LOD and LOQ of 0.2 µg/mL and 0.6 µg/mL respectively. The specificity of the proposed method was performed whereby metaxalone undergoes different stress conditions like oxidation, reduction, photolysis, acid and alkaline hydrolysis.

scholarly journals Development and validation of a novel stability indicating HPLC method for the separation and determination of darolutamide and its impurities in pharmaceutical formulations

2021 ◽  
Vol 104 (4) ◽  
pp. 57-68
Author(s):  
V.G. Kamani ◽  
◽  
M. Sujatha ◽  
G.B. Daddala ◽  
◽  
...  
Keyword(s):  
Ammonium Acetate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Forced Degradation ◽  
Degradation Study ◽  
Stability Indicating ◽  
System Suitability ◽  
Development And Validation ◽  
First Time

This study reports for the first time about a stability indicating RP-HPLC method for analysis of darolutamide and its impurities 1, 2, and 3 in bulk and formulations. The separation was achieved on Phenomenex column with Luna C18 (250 mm × 4.6 mm, 5 μm) as stationary phase, and 50 mM ammonium acetate: methanol solution 15:80 (v/v) at pH 5.2 as mobile phase at 1.0 mL/min flow rate. UV detection was carried at wavelength of 239 nm. In these conditions the retention time of darolutamide and its impurities 1, 2, and 3 was 7.05, 8.90, 4.63 and 5.95 min, respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability, and robustness. Forced degradation study was done through exposure of the analyte to five different stress conditions and the % degradation was small in all degradation condition. The proposed method can separate and estimate the drug and its impurities in pharmaceutical formulations. Hence, the developed method was suitable for the quantification of darolutamide and can separate and analyse impurities 1, 2, and 3

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

A NOVEL STABILITY INDICATING RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF VALSARTAN AND HYDROCHLOROTHIAZIDE IN BULK AND PHARMACEUTICAL FORMULATIONS

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (08) ◽  
pp. 54-61
Author(s):  
B. Venkateswara Rao ◽  
◽  
S. Vidyadhara ◽  
V. Basaveswara Rao
Keyword(s):  
Method Development ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Liquid Chromatography Method ◽  
Hplc Method Development ◽  
Development And Validation

The prime aim of the present investigation was to develop and validate a novel, precise, accurate, specific, rapid and economical stability- indicating isocratic reverse phase liquid chromatography method for the quantitative simultaneous estimation of valsartan and hydrochlorothiazide in bulk and marketed formulations. Estimation of drugs in this combination was achieved with a C18 column [Kromasil 100-5 C18 column, P134 250 × 4.6 mm] kept at ambient temperature, isocratic mode using mobile phase of composition acetonitrile and phosphate buffer (40:60 V/V, pH 4). The flow rate was 0.8 ml/min and the effluents were monitored at 235 nm, using variable wavelength UV detector. The retention time of valsartan and hydrochlorothiazide were 2.65 min and 3.97 min, respectively. Validation of the method was done according to the ICH guidelines for different analytical parameters. The method was found to be linear over a range of 50-250 μg/mL for valsartan and hydrochlorothiazide. The established method was as reproducible with a %RSD value of less than 2 and having robustness and accuracy within the specified limits. Assay of marketed formulation was determined and was 99.04% and 99.8% respectively. The stressed samples were analyzed. The proposed method was found to be specific and stability indicating as no interfering peaks of degradation compounds and excipients were noticed. The proposed method can be successfully employed in the estimation of commercial formulations.

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