scholarly journals Application of Spectrophotometry and High Performance Liquid Chromatography for the Analysis of Bosentan in Pharmaceutical Dosage Form

Author(s):  
SRUTHI A ◽  
UTTAM PRASAD PANIGRAHY

Objective: A rapid, sensitive and specific reverse phase High performance liquid Chromatography (RP-HPLC) method was developed for the estimation of Fimasartan in bulk and pharmaceutical dosage form. Method: The RP-HPLC analysis was performed isocratically on a Primacel C18 column (150 mm × 4.6 mm internal diameter, 5 μm particle size) using mobile phase of composition Acetonitrile and 0.1% orthophosphoric Acid in 80:20, v/v proportions with a flow rate of 0.8 ml/min. Results: The analyte was monitered with UV-detector at 265 nm. In the developed method Fimasartan elutes at a typical retention time of 2.4 min. The proposed method is having linearity in the concentration ranging from 5-30 μg/ml of Fimasartan. Conclusion: : The method was statistically validated and had been applied to analysis of the drug in bulk and pharmaceutical dosage form.


Author(s):  
Rajesh Nawale ◽  
Shankar Pol ◽  
Prashant Puranik ◽  
Anwar Daud ◽  
Vishal Rajkondawar

Objective: The objective of the study was to develop and validate new, simple, and selective reverse-phase–high-performance liquid chromatography (RP-HPLC) method for the quantitative determination of Dabigatran Etexilate (DE) and its impurities in pharmaceutical dosage form as per the International Conference on Harmonization guidelines.Method: Chromatographic analysis was performed on Princeton SPHER-l00 C18 (250 × 4.6 mm, 5 μm) HPLC column, maintained at 50°C column temperatures, 6°C sample tray temperature, and detection monitored at 225 nm. The mobile phase consisted of acetonitrile:phosphate buffer (pH 2.5) (33:67 V/V). The flow rate was maintained at 1.0 ml/min.Results: The system suitability results indicate good performance of the system. Specificity study indicates that there is no interference of placebo and blank. The percentage relative standard deviation (RSD) of six preparations for known and unknown impurity in the sample solution is found below 10%; hence, the method is precise. The calibration curve for DE (unknown impurity), Impurity A was linear from 0.38 to 4.5 μg/ml (correlation coefficients [r2] for unknown Impurity [DE] and Impurity A are 0.996 and 0.999, respectively). The calibration curve for Impurity B and Impurity E was linear from 0.38 to 9.00 μg/ml (r2 for Impurity B and Impurity E are 0.999 and 0.999, respectively); hence, the method is linear. Accuracy for DE (unknown Impurity), Impurity A, Impurity B, and Impurity E are found within 80%–120%; hence, the method is accurate. The percentage RSD for a standard solution is found below 5% up to 24 h, and percentage impurity change in the sample solution is found below 0.1% up to 18 h; hence, standard solution is stable up to 24 h, and sample solution is stable up to 18 h.Conclusion: The developed method is new, simple, adequate, specific, precise, linear, and accurate for the determination of DE and its impurities in pharmaceutical dosage forms.


2012 ◽  
Vol 18 (3) ◽  
pp. 399-405 ◽  
Author(s):  
Bilal Yilmaz ◽  
Yucel Kadioglu ◽  
Kadem Meral ◽  
Yavuz Onganer

In this study, a new and rapid spectrofluorometry and high performance liquid chromatography (HPLC) methods were developed for determination of human growth hormone in pure and pharmaceutical dosage form. The solvent system, wavelength of detection and chromatographic conditions were optimized in order to maximize the sensitivity of both the proposed methods. The linearity was established over the concentration range of 1.25-50?g mL-1 for spectrofluorometry and 10-75?g mL-1 for HPLC method. The intra- and inter-day relative standard deviation (RSD) was less than 8.46 and 5.98% for spectrofluorometry and HPLC, respectively. Limits of quantitation were determined as 0.075 and 7.5?g mL-1 for spectrofluorometry and HPLC, respectively. No interference was found from tablet excipients at the selected assay conditions. The methods were applied for the quality control of commercial growth hormone dosage form to quantify the drug and to check the formulation content uniformity.


2018 ◽  
Vol 2 (2) ◽  
pp. 78-84
Author(s):  
Bhagyashree R. Patil ◽  
O. G. Bhusnure ◽  
B. N. Paul ◽  
A. Y. Ghodke ◽  
Suraj S. Mulaje

A simple, specific, precise and accurate Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method was developed and validated for the estimation of Diltiazem Hydrochloride in bulk and pharmaceutical dosage form. The chromatographic determination was performed on isocratic high performance liquid chromatography system of Agilent model no.1220. The separation was conducted by using column of Zorbax [C8 (5µ, 4.6 mm×250)] with mobile phase consisting of buffer and Acetonitrile in the ratio of (60:40). The mobile phase was delivered at the flow rate of 1.0ml/min. The eluent was monitored at wavelength 240 nm and found a sharp and symmetrical peak with retention time of 4.66min. The method was validated for linearity, accuracy, precision, specificity, robustness. Recovery of Diltiazem Hydrochloride was found to be in the range of 98%-102%. The method was found to be linear over the concentration range 50-150 µg/ml with coefficient correlation r2 = 0.995. After developing method, validation parameters were carried out successfully and obtained results were complied with USP monograph.


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