Current Issue : January - March Volume : 2016 Issue Number : 1 Articles : 9 Articles
A simple, accurate and precise dual wavelength UV spectrophotometric method was developed for simultaneous determination of fluoxetine HCl and olanzapine in combined pharmaceutical dosage forms. The absorbance difference between two points on the mixture spectra is directly proportional to the concentration of the component of interest”. During selection of two wavelengths the interfering component shows same absorbance while the component of interest shows significant difference in absorbance with concentration. The literature review reveals that there is no dual wavelength method was developed for this combination of drugs, hence this method was developed. The wavelengths selected for determination of fluoxetine HCl were 240 nm and 260.24 nm, whereas, the wavelengths selected for determination of olanzapine were 215.29 nm and 228.94 nm. Acetonitrile, methanol and distilled water were taken as the solvents. The Beer's law was obeyed in the concentration range of 4–20 μg/ml for fluoxetine HCl and 1-5 μg/ml for olanzapine. Correlation coefficient was found to be 0.9966 and 0.9908 for fluoxetine HCl and olanzapine, respectively for dual wavelength method. Accuracy of method was found between 98.0-102.0%. The precision (intra-day, inter-day and analyst to analyst) of method was found within limits (%CV<2). LOD was found to be 0.23 μg/ml and 0.125 μg/ml for fluoxetine HCl and olanzapine respectively and LOQ was found to be 0.708 μg/ml and 0.41 μg/ml for fluoxetine HCl and olanzapine respectively. The proposed method was successfully applied to determination of these drugs in laboratory-prepared mixtures and commercial tablets....
Reference standards (RS) are highly characterized substances which are specifically required in pharmacopoeial tests and assays. Quality control testing of human insulin is performed using the methods given in the Indian Pharmacopoeia (IP) monograph which requires the use of human insulin RS. However, there was no RS available to support the IP monograph on human insulin. Therefore, National Institute of Biologicals undertook a collaborative study to establish the first National human insulin RS. The methods selected to qualify the candidate material were those included in the IP monograph on human insulin. The study was defined to calibrate the candidate by liquid chromatography in terms of International primary standard i.e. human insulin Ph. Eur. RS and to assign a unit age. The collaborative study involved four laboratories from India, including one regulatory lab and three laboratories of insulin manufacturers. It was demonstrated that candidate material is appropriate for use as an RS in the context of human insulin according to IP monograph. Direct calibration of candidate human insulin RS was established on 26th August, 2010 with assigned potency value of 27.5 IU per mg on as-is basis and it is intended to be used in identification and assays....
A simple, specific, accurate and stability-indicating high performance liquid chromatographic method for determination of lafutidine, using Hypersil BDS C18 (250 x 4.6 mm, i.d., 5 µm) column and a mobile phase comprising of methanol and 0.05 M ammonium acetate in a ratio of 45:55 (v/v). The retention time of lafutidine was 9.0 min. The linearity was established in the range of 100-600 µg/ml. The percentage recoveries for lafutidine were in the range of 100.4045±0.0392 - 101.5068±0.5846. The drug was subjected to acid, alkaline, photolytic, oxidative, neutral hydrolysis and thermal degradation. The degradation studies indicated, lafutidine was susceptible towards acid, alkaline, photolytic and oxidative hydrolysis and was comparatively stable towards neutral and thermal stress. The degradation products of lafutidine were well resolved from the pure drug with significant differences in their retention time values. The method can be successfully employed for determination of lafutidine in bulk drug and also for characterization of degradation products as it is stability-indicating one....
The present work deals with development and validation of two precise and accurate spectrophotometric methods for the estimation of flunarizine dihydrochloride in bulk and tablet dosage form. Method A is the absorbance maxima method where absorbance maxima of the drug were recorded at 252 nm. Method B is area under the curve in which wavelength range 244-252 nm was selected for estimation of flunarizine dihydrochloride by using co-solvent method (methanol: water 50:50% v/v). Linearity was observed in the concentration range 4-24 µg/ml for both the methods (r2 = 0.999 for method A and r2 = 0.999 for method B). The results of analysis were validated statistically, which confirmed the accuracy and reproducibility of the methods. Both the methods were found to be precise and accurate and can be employed for routine quality control analysis of flunarizine dihydrochloride in bulk as well as in its solid dosage form....
A simple, specific and accurate reversed phase high performance liquid chromatographic method was developed and validated for the determination of Eperisone HCl. The determination was carried out using a Thermo C18 (250 x 4.6 mm) 5 μm column and a mobile phase of methanol and water in the proportion of (45:55) pH adjusted with 0.05% o-phosphoric acid. Validation parameters were evaluated for the method according to the ICH (Q2R1) guidelines. Linearity was established for Eperisone HCl in the range of 10 to 50 µg/ml, respectively. The limit of detection and limit of quantitation for the method were 0.286 μg/ml and 0.868 μg/ml, respectively. The statistical analysis shows that the method was found to be accurate, reliable, simple and reproducible. The intra- and inter-assay precisions were satisfactory; the values of relative standard deviations did not exceed 2%. The accuracy of the method was proved; the mean recovery of Eperisone HCl was 98.89% to 100.90%. The chromatographic retention time of proposed method was 7.55 min and the mean assay of content was found to be 99.48±0.59%. The proposed method was successfully applied for the quantitative determination of Eperisone HCl in bulk form and could be used for routine analysis with phenomenal accuracy and precisions. The results were validated as per the ICH guidelines. This method can be successfully employed for the quantitative analysis of Eperisone HCl in pure and formulation....
A new, accurate, precise, linear, reproducible and economical spectrophotometric method has been developed and validated for the determination of eletriptan hydrobromide (EH) in bulk drugs and pharmaceutical dosage form. UV Spectrophotometric method is based on measurement of absorption. The absorbance of eletriptan hydrobromide was found to be at 221 and 272 nm maximum wavelengths. Beer-Lambert’s law is obeyed in the concentration range of 2-10 μg/ml and is described by the regression equation y = 0.081x with a regression coefficient (r2) = 0.999. The value of molar absorptivity and Sandell’s sensitivity for EH estimated are 3.098 x 103 L/mol/cm and 0.123 μg/cm2, respectively. Whereas LOD and LOQ were found to be 0.619 and 1.877 μg/ml, respectively. The developed method was validated with respect to linearity, accuracy (recovery), precision, percentage recovery and specificity. The developed method was validated according to ICH guidelines where the developed method was found to be accurate and precise. The proposed method can be successfully applied for the estimation of EH in bulk and pharmaceutical dosage form....
Zolmitriptan (ZMT) is a 5-HT 1B/1D receptor partial agonist which has been approved for use in the acute treatment of migraine. A simple, precise, accurate and economical UV-Spectrophotometric method has been developed for the determination of ZMT in bulk and pharmaceutical dosage form. The absorbance for ZMT was measured at maximum wavelength of 281 nm. The percentage recovery of ZMT in pharmaceutical dosage form was found to be 99.97±0.3969. The developed method was validated with respect to linearity, accuracy (recovery), precision and specificity. Beers law was obeyed in the concentration range of 5-50 μg/ml having line equation y = 0.019x with correlation coefficient of 0.998. Results of the analysis were validated according to the ICH guidelines. The results obtained were statistically evaluated and were found to be accurate and reproducible. The proposed method can be successfully applied for the estimation of ZMT in bulk and pharmaceutical dosage form....
Two UV methods were developed for combined formulation of indapamide and olmesartan medoxomil. First method is simultaneous equation method. In this method the absorbance at 240 nm and 256 nm were used for IND and OLM respectively. Second method is first order derivative spectroscopic method. In second method the absorbance at 225.4 nm (Zero crossing point of IND) and 256.6 nm (Zero crossing point of OLM) were used for estimation of OLM and IND respectively. In both methods linearity was taken in the concentration series of 1-30 μg/ml for IND and 10-70 μg/ml for OLM. The developed methods were validated as per ICH guidelines....
A reliable and sensitive stability indicating HPLC method has been developed and validated for montelukast sodium and desloratadine in its dosage form. A separation of montelukast sodium and desloratadine were achieved on ODS hypersil C18 (250 mm × 4.6 mm, 5 μ) column using a UV detector to monitor elute at 230 nm. The mobile phase consisted of 0.3% triflouroacetic acid with water: acetonitrile (20:80 v/v) and flow rate of 1.0 ml/min. The retention time were found to be 6.12 min and 4.19 min for MON and DES respectively. Rectilinear relationship with good regression coefficients 0.9969 and 0.9998 was found over the concentration ranges of 80-120 μg/ml and 40-60 μg/ml for MON and DES, respectively, with detection limits 11.51 µg/ml for montelukast sodium and 4.06 µg/ml for desloratadine and quantitation limits 34.89 µg/ml for montelukast sodium and 12.32 µg/ml for desloratadine. Inter day precision (%RSD) for MON and DES were 0.383-1.021 and 0.558-0.695 respectively. Accuracy was 99.55-100.20 for MON and 99.56-100.15 for DES. The drugs were subjected to hydrolysis, oxidation, photolysis and thermal degradation. Because the method could effectively separate the drug from its degradation products, it can be used for stability-indicating analysis....
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