Methanol.

A simple, rapid, accurate and precise high performance thin-layer chromatography (HPTLC) method was developed and validated for simultaneous estimation of alogliptin and metformin active pharmaceutical ingredients and fixed dose combination. Alogliptin and metformin densitograms were developed on silica gel 60 F254 HPTLC plates with chloroform: methanol: 0.5 % ammonium sulphate (4:4:2 %v/v) as mobile phase. Densitometric quantification was performed at 254 nm. For Alogliptin and Metformin Rf values were found as 0.66 and 0.44, respectively. The linearity curves of Alogliptin and Metformin were obtained in the concentration range of 100-500 ng/spot and 4000-20000 ng/spot by area with correlation co-efficient of 0.998 and 0.995 for Alogliptin and Metformin, respectively. Limit of detection was found to be 2 ng and 40 ng/spot for Alogliptin and Metformin, respectively; lowest possible quantity to be quantified by the proposed method was found to be 6 ng and 130 ng per spot for Alogliptin and Metformin, respectively. The method was validated for precision, accuracy, specificity and robustness. The developed method was validated and found to be selective, specific and suitable for application in pharmaceutical analysis of these drugs in bulk and fixed dose combination.

The present manuscript describes sensitive, rapid, accurate, and precise spectrophotometric method for simultaneous estimation of allopurinol and aceclofenac in pharmaceutical dosage form. Simultaneous equation method used at 250nm & 273nm as λmax of allopurinol and aceclofenac respectively in 0.1N HCl. Both the drugs follow beer-lamber’s law on the concentration range 2-12µg/ml and 2-24µg/ml respectively for allopurinol & aceclofenac. The mean percentage recovery is 100.01% and 99.4% for allopurinol and aceclofenac respectively by simultaneous equation. The method has been validated as per ICH guidelines. The proposed method effectively applied to bulk drug and pharmaceutical formulation. The accuracy and reproducibility are close to 100% with acceptance range of %R.S.D. The method was successfully applied to pharmaceutical dosage form because no interference was found from excipient. 

A simple, rapid and accurate high performance liquid chromatography method is described for determination of rupatadine fumarate from its active pharmaceutical ingredients. The separation of drug was achieved on Inertsil ODS-3 C18 (250 X 4.6 mm) 5µ column. The mobile phase was a mixture of acetonitrile and methanol (80:20 v/v) : buffer of pH  4.5 [70:30 % v/v]. The buffer of pH 4.5 was prepared from 0.01 M ammonium acetate and pH was adjusted with dilute acetic acid. The detection was carried out at wavelength 250 nm. The mixture of water: acetonitrile (30:70 % v/v) was used as a diluent. The method was validated for system suitability, linearity, accuracy, precision, robustness, stability of sample solution. The method has been successfully used to analyze rupatadine fumarate from pharmaceutical formulation.