Development and Validation of Stability-indicating RP-HPLC Method for Estimation of Pranlukast Hydrate in its Laboratory Mixture.

Pranlukast hydrate is an anti-asthmatic drug and used in the treatment of acute asthma. Stability-indicating RP-HPLC method for pranlukast hydrate has been developed and validated. The reverse phase high performance liquid chromatographic method was developed using Shimadzu Column: Kromosil 100 C18 (150 mm × 4.6 mm × 5 µm) and mobile phase Acetonitrile: 0.1% Glacial acetic acid (85: 15% v/v). Eluent was monitored with UV-detector at 262 nm with a flow rate of 0.5 mL/min, temperature maintained at 30°C. Stress testing was carried out in acidic, alkaline, oxidative, photolytic and dry heat degradation conditions. The method was validated as per the International Conference for Harmonization guidelines and includes specificity, accuracy, precision, linearity and limit of quantitation and detection parameters. A relative standard deviation <2% indicates the developed method was precise. The accuracy of the method was represented by recovery studies ranging between 99.41 and 99.72%. In acid, alkaline, oxidative stress conditions, pranlukast hydrate degrades significantly and in photolytic, dry heat, hydrolytic conditions remain stable. This proposed method is suitable for the analysis of pranlukast hydrate in its laboratory mixture.

Simultaneous Estimation of Six Nitrosamine Impurities in Valsartan Using Liquid Chromatographic Method.

BACKGROUND: Nitrosamine impurities are potent carcinogens in animals and probable carcinogens in humans. 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: A liquid chromatographic method was developed for estimation of six nitrosamine impurities in valsartan. METHODS: The developed method employed: a C18 (250 × 4.6 mm, 5 µm) column as a stationary phase; a combination of acetonitrile, water (pH 3.2 adjusted with formic acid), and methanol with gradient elution as mobile phase; and 228 nm as the detection wavelength. The developed method was validated as per International Conference on Harmonization Q2(R1) guidelines. The method was successfully applied to estimate six nitrosamine impurities in valsartan API (active pharmaceutical ingradient) and formulation (tablets). RESULTS: The method was able to separate each impurity and valsartan with resolved and sharp peaks. Results indicated that the 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 in agreement with the spiked amount of each impurity. CONCLUSION: The developed method can be applied for simultaneous estimation of six nitrosamine impurities in valsartan raw material, tablets, and fixed dose combination at very low levels. HIGHLIGHTS: Development, validation, and application of a HPLC method for the estimation of six nitrosamine impurities in valsartan API and formulation samples.