Current Issue : July - September Volume : 2015 Issue Number : 3 Articles : 9 Articles
A simple, accurate and precise dual wavelength spectrophotometric method was developed for simultaneous determination of lamivudine and tenofovir disproxil fumarate in bulk and their combined pharmaceutical dosage form. The principle for dual wavelength method is “the absorbance difference between two points on the mixture spectra is directly proportional to the concentration of the drug component”. Lamivudine shows maximum absorbance at 270 nm and tenofovir disproxil fumarate shows maximum absorbance at 260 nm. In dual wavelength method, two wavelengths were selected for each drug in a way so that the difference in absorbance is zero for another drug. Lamivudine shows equal absorbance at 263.91 and 276.33 nm, where the difference in absorbance was measured for determination of tenofovir disproxil fumarate. Similarly, difference in absorbance at 253.25 and 266.27 nm were measured for determination of lamivudine. 0.1N NaOH was taken as a solvent. Regression analysis of Beer’s plots showed good linearity in concentration range of 10-120 µg/ml for lamivudine and 10-80 µg/ml for tenofovir disproxil fumarate with correlation coefficient 0.999 and 0.997 for LAM and TDF respectively. The mean percent label claim of tablets of lamivudine and tenofovir disproxil fumarate in formulation estimated by the proposed method was found to be 103.57% and 98.46% for LAM and TDF respectively. The developed method was validated according to ICH guidelines and values of accuracy, precision and other statistical parameters were found to be good accordance with the prescribe values. Accuracy of method was found between 95-105% for both the drugs. The precision (intra‐day, inter‐day and repeatability) of method was found within limits for both the drugs. The proposed method was successfully applied for analysis of these drugs in commercial tablets....
To develop a simple, sensitive and accurate HPTLC densitometric method for the quantitative standardization of Glycyrrhizin from in-house herbal nutritive supplement. Quantification of glycyrrhizin was done on an aluminum plates precoated with silica gel F254 plate with mobile phase composed of n-butanol:water: glacial acetic acid (10:4:2 v/v/v). Developed plates were scanned and quantification was done at wavelength of maximum absorption 251 nm. Rf value for glycyrrhizin was found to be 0.40±0.01, under the above mentioned experimental conditions. Method was shown to be linear (r2 > 0.996), repeatable with system precision (< 3.0), method precision (< 2.0) and intermediate precision (< 2.0) and sensitive over the calibration range for glycyrrhizin. Glycyrrhizin was fully recovered in the presence of normal condition in the range of 91.60%-104.99%. Statistical analysis proves that the proposed method is more selective, reproducible and repeatable for the estimation of the Glycyrrhizin from in-house herbal nutritive supplement....
Accurate, specific, precise and robust TLC densitometric method has been developed for simultaneous estimation of\nmetoprolol succinate (METO) and hydrochlorothiazide (HCTZ) in tablet dosage form. The chromatographic separation was\nperformed on precoated silica gel TLC 60 F254 plates using toluene: methanol: ethyl acetate: glacial acetic acid (7:1.5:1:0.5\nv/v/v/v) as mobile phase. This system was found to give compact bands for metoprolol succinate and hydrochlorothiazide (RF\nvalues 0.15 and 0.35 respectively). Densitometric analysis of metoprolol succinate and hydrochlorothiazide were performed at\n230 nm. Regression analysis data for the calibration plots were indicative of good linear relationships between response and\nconcentration over the range 1000-5000 ng/band for metoprolol succinate and 500-2500 ng/band for hydrochlorothiazide. The\nmethod was validated as per ICH guidelines for accuracy, precision, LOD, LOQ and robustness....
The present work deals with development of two rapid, precise and accurate spectrophotometric methods for the estimation of dexchlorpheniramine maleate in bulk and solid dosage form. Method A is absorption maxima method in which λmax was 260 nm. Method B is area under the curve in which wavelength range 248-272 nm was selected for estimation of dexchlorpheniramine maleate. Linearity was observed in the concentration range 10-90 µg/ml for both the methods (r2 = 0.9996 for method A and r2 = 0.9997 for method B). The results of analysis have been validated statistically, which confirm the accuracy and reproducibility of the methods. All the methods were found to be simple, precise and accurate and can be employed for routine quality control analysis of dexchlorpheniramine maleate in bulk as well as in its solid dosage form....
A simple, sensitive and precise RP-UPLC method for estimation of Emtricitabine has been developed and validated for determination of compounds in commercial tablet dosage form. The compounds were well separated isocratically on a ODS column using a mobile phase consisting of buffer (pH 1.9), butanol and methanol in the ratio of 70:25:5 v/v/v 0.3µl/min with PDA detector. Retention time for Emtricitabine was found to be 1.7min. The method was validated in accordance with ICH guidelines The study showed that the reverse phased liquid chromatography is sensitive and selective for detecting Emtricitabine using the single mobile phase....
Quality by design (QbD) refers to the achievement of certain predictable quality with desired and predetermined specifications. The primary objective of this study was to implement QbD approach to develop and validate a HPLC method that could separate gatifloxacin in the bulk and formulated forms with in-depth understanding of the method and build in the quality during the method development to ensure optimum method performance and its application to study in vitro interaction of gatifloxacin with cations like Calcium, Aluminum and Iron. The method was developed using princetonspher-100 CN Column (150 cm x 4.6 mm i.d., 5m) column with mobile phase consisting of a mixture of phosphate buffer of pH 2.5 and acetonitrile (85:15%v/v). The method fulfilled validation criteria and was shown to be sensitive, with limits of detection (LOD) and quantitation (LOQ) of 0.015 and 0.046 μg/mL, respectively. The calibration graph was linear in the range of 10–50 μg/mL. In vitro interaction study shown that Calcium Sandoz-250 and Calcium Sandoz woman (525 mg of calcium carbonate) decreases dissolution of gatifloxacin tablet by 7.78% and 28.73%, respectively. Iron supplement (Autrin) and aluminum + magnesium containing product decreases dissolution of gatifloxacin tablet by 14.91% and 14.91%, respectively. The method was sound as per ICH guidelines and it can be applied for interactions of cations with gatifloxacin....
A sensitive, accurate, precise and reproducible high performance liquid chromatographic (HPLC) method was developed and validated for the analysis of triamterene and hydrochlorothiazide combination in tablet dosage form. Chromatographic separation was achieved under isocratic condition on a Thermo Hypersil BDS, C18 column (250 mm x 4.6 mm, 5 μm) utilizing a mobile phase of acetonitrile:sodium dihydrogen phosphate buffer of pH 5.5 in the ratio of 20:80 (v/v) at a flow rate of 1 ml/min with UV detection at 325 nm. The retention time of hydrochlorothiazide and triamterene was 5.1 and 9.8 min respectively. The developed method has followed linearity in the range of 7.5-37.5 μg/ml for triamterene and 5-25μg/ml for hydrochlorothiazide. The value of correlation coefficient was 0.998 and 0.998 respectively. Satisfactory values of percent relative standard deviation for the intra-day and inter-day precision indicated that method was precise. Results of the recovery studies (95% to 105%) showed accuracy of the method. LOD and LOQ were calculated as 0.137 μg/ml and 0.416 μg/ml for triamterene and 0.105 μg/ml and 0.318 μg/ml for hydrochlorothiazide respectively. The developed method can be used for routine estimation of triamterene and hydrochlorothiazide in tablet dosage forms....
A sensitive, accurate and precise method was developed and validated for the simultaneous estimation of doxylamine succinate and pyridoxine hydrochloride in its combined dosage form. The developed RP-HPLC method had shown adequate separation for doxylamine succinate and pyridoxine hydrochloride from its degradation products. The separation was achieved by using a C18 column (150 х 4.6 mm i.d.) with mobile phase composition of phosphate buffer pH 4.0 and acetonitrile (70:30) %v/v at a flow rate of 1 ml/min, with detection wavelength of 260 nm. The retention time for pyridoxine hydrochloride and doxylamine succinate were 2.400±0.5 min and 4.256±0.5 min. with linearity range 10-50 μg/ml. Proposed method was validated as per ICH guidelines for linearity, accuracy, precision, specificity and LOD and LOQ and found to be useful for estimation of doxylamine succinate and pyridoxine hydrochloride in its tablet dosage form....
A simple precise and accurate stability indicating RP-HPLC method has been developed for estimation of metolazone in pharmaceutical dosage form. A stability indicating assay accurately measures the active ingredients, without interference from degradation product. Stability study and degradation kinetics are an integral part of the quality control of the drug or medicinal product on an industrial level. Forced degradation of drug substance and drug product according to the ICH guideline was studied. In RP-HPLC method methanol:water (80:20% v/v) was used as a mobile phase. The Hiber 100-5 C18 column, 250 mm L × 4.6 mm in size was used as a stationary phase for separation of drug with other degraded product. The flow rate was 0.8 ml/ min, detection wavelength was 236 nm. The linearity was observed in range of 3 µg/ml -7 µg/ml. The peak purity was found to be more than 0.990 the assay of the drug was found in acceptance range. The degradation product peak was well resolved from the pure drug peak with significant difference in their retention time, so that developed method could be used for routine analysis and stability studies....
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