Aim and Background:To develop and validate a simple, precise, accurate, and stability indicating a UV-method for estimation of Telmisartan (TELM). UV, HPLC, HPTLC, and many more experiments were carried out by taking single drug and also by combining with other drugs. However, Such type of studies was not reported.Materials and Methods:In both methods, TELM has the absorbance maxima at 296 nm. Method A involves method development and validation and Method B involves forced degradation study. In these methods, methanol was used as a solvent. Linearity was observed in the concentration range of 4–16 μg/ml. Validation experiments were performed to demonstrate system suitability, specificity, precision, linearity, accuracy, robustness, LOD, and LOQ as per International Conference on Harmonization guidelines. Furthermore stability studies of TELM were carried out under acidic, alkali, neutral, oxidation, photolytic, and thermal degradation as per stability indicating assay methods.Results:The results of analysis have been validated, and recovery studies were carried out using a standard addition method by adding specific drug amount (80%, 100%, and 120%) and show recovery studies in the range (99.26–101.26)%.Conclusion:The proposed method can be successfully applied for method development, validation, and stability study of TELM.

Aim:To develop a simple, accurate, sensitive, rapid and precise method for the determination of galantamine hydrobromide in bulk drug and pharmaceutical dosage form.Material and Methods:The method employs wavelength detection and determination of galantamine hydrobromide at excitation wavelength 282 nm and emission wavelength 607 nm in a solution of simple distilled water.Result and Conclusion:The method was found to be linear in the range of 2–14 μg/ml having r2 = 0.9999. The mean accuracy was found to be 98.12% to 99.67%. The intraday and interday precision was found to be 0.18–0.35% and 0.13–0.46%, respectively. The limit of detection was found to be 0.29 μg/ml. The limit of quantification was found to be 0.89 μg/ml. The method was successfully applied for the determination of galantamine hydrobromide in bulk drug as well as pharmaceutical dosage form.

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Background:A new, simple, selective, precise, and stability-indicating high-performance thin-layer chromatographic method has been established for analysis of itraconazole (ITZ) in the bulk drug and in pharmaceutical formulations. Separation was achieved on aluminium plate precoated with silica gel 60F254 using Toluene : Chloroform : Methanol [5 : 5 : 1.5 (v/v)] as mobile phase. Densitometric analysis was performed at 260 nm.Result:Compact bands of ITZ were obtained at Rf 0.52 ± 0.02. Linearity (R2 = 0.9978), limit of detection (180.29 ng/band), limit of quantification (546.34 ng/band), recovery (98–102%), and precision (≤0.51%) were satisfactory. Drug was not degraded under neutral and alkaline hydrolysis, UV and photolytic degradation, under-elevated temperature, and humidity. ITZ is degraded under acidic hydrolysis and oxidative condition; the degraded products were well resolved from individual bulk drug response. Developed method can effectively resolve drug from its excipients in capsule dosage form. The specificity of the method was confirmed by peak purity of resolved peak.Conclusion:The method can be applicable for routine analysis of ITZ in pharmaceutical formulation as stability-indicating. Because the method can effectively separate the drug from its degradation products as well as excipients, it can be used as a stability-indicating method.

Aim and Background:The present manuscript describes simple, sensitive, rapid, accurate, precise and economical spectrophotometric method for the simultaneous determination of telmisartan and metoprolol succinate in combined tablet dosage form.Materials and Methods:The method is based on the absorbance correction equations for analysis of both the drugs using methanol as solvent. Telmisartan has absorbance maxima at 296 nm and metoprolol succinate has absorbance maxima at 223 nm in methanol. The linearity was obtained in the concentration range of 2-16 μg/ ml and 3-24 μg/ml for telmisartan and metoprolol succinate, respectively. The concentrations of the drugs were determined by using absorbance correction method at both the wavelengths. The method was successfully applied to pharmaceutical dosage form because no interference from the tablet excipients was found. The suitability of this method for the quantitative determination of telmisartan and metoprolol succinate was proved by validation. The proposed method was found to be simple and sensitive for the quality control application of telmisartan and metoprolol succinate in pharmaceutical dosage form.Result:The result of analysis has been validated statistically and by recovery studies. Recoveries were found in the range of 98.08-100.55% of telmisartan and 98.41-101.87% of metoprolol succinate.

Background Nitrosamine impurities are potent carcinogens in animals and probable carcinogens in humans. In current scenario, there is a need for effective analytical methods to detect and identify various nitrosamine impurities, and to develop rapid solutions to ensure the safety and quality of the drugs. Objective In present work, liquid chromatographic method was developed for estimation of six nitrosamine impurities in Valsartan. Methods The developed method employed C18 (250 × 4.6 mm, 5 μ) column as a stationary phase, combination of acetonitrile, water (pH 3.2 adjusted with formic acid) and methanol with gradient elution as mobile phase and 228 nm as detection wavelength. Developed method was validated as per ICH Q2(R1) guideline. Method was successfully applied to estimate six nitrosamine impurities in Valsartan API and formulation (tablets). Results Method was able to separate each impurity and Valsartan with resolved and sharp peaks. Results indicated that developed method is linear in selected ranges (coefficient of regressions > 0.9996), precise (RSD < 2%), accurate (recovery in a range of 99.02–100.16%), sensitive (low detection and quantitation limits) and specific for estimation of each impurity in Valsartan. Assay results were found in agreement with the amount of each impurity spiked. Conclusion Developed method can be applied for simultaneous estimation of six nitrosamine impurities in Valsartan raw material, tablets and fixed dose combination at very low level. Highlights Development, validation and application of HPLC method for estimation of six nitrosamine impurities in Valsartan API and formulation samples.

Background and Aim:A fixed dose combination of moxifloxacin hydrochloride and ketorolac tromethamine is used in ratio of 1:1 as eye drops for the treatment of the reduction of post operative inflammatory conditions of the eye. A simple, precise, and accurate High Performance Liquid Chromatographic (HPLC) method was developed and validated for determination of moxifloxacin hydrochloride and ketorolac tromethamine in eye drops. Materials and Methods: Isocratic HPLC separation was achieved on a ACE C 18 column (C 18 (5 μm, 150 mm × 4.6 mm, i.d.)) using the mobile phase 10 mM potassium di-hydrogen phosphate buffer pH 4.6-Acetonitrile (75:25 v/v) at a flow rate of 1.0 mL/min. The detection was performed at 307 nm. Drugs were subjected to acid, alkali and neutral hydrolysis, oxidation and photo degradation. Moreover, the proposed HPLC method was utilized to investigate the pH dependent degradation kinetics of moxifloxacin hydrochloride and ketorolac tromethamine in buffer solutions at different pH values like 2.0, 6.8 and 9.0. Results and Conclusion: The retention time (t R ) of moxifloxacin hydrochloride and ketorolac tromethamine were 3.81±0.01 and 8.82±0.02 min, respectively. The method was linear in the concentration range of 2-20 μg/mL each for moxifloxacin hydrochloride and ketorolac tromethamine with a correlation coefficient of 0.9996 and 0.9999, respectively. The method was validated for linearity, precision, accuracy, robustness, specificity, limit of detection and limit of quantitation. The drugs could be effectively separated from different degradation products and hence the method can be used for stability analysis. Different kinetics parameters like apparent first-order rate constant, half-life and t 90 (time for 90% potency left) were calculated.

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