N,O,O-donating ligand was prepared from the condensation of benzofuran hydrazone and ortho-vanilln. Metal complex of this ligand is neither air- nor moisture-sensitive. The effects of varying solvents, bases, and ligand/copper ratio on the performance of the coupling reaction were investigated. All reactions are carried out in anhydrous condition.
Malathi S* and Sivakumar T
Journal Title:World Journal of Pharmacy and Pharmaceutical Sciences
This article gives a simple, rapid and accurate High performance thin layer chromatographic method for determination of Sitagliptin and Simvastatin in pharmaceutical formulation. Merck TLC aluminum sheets of silicagel G60 F254 with the thickness of 200 ?m was used to carry out the separation. Ethyl acetate: toluene: methanol (6:2:2 v/v/v), was used as mobile phase. Analysis of the compounds was carried out by densitometry in the absorbance mode at 254 nm. The selected mobile phase gave the well defined peak at the Rf value of 0.6 +0.02 and 0.3+0.02 for sitagliptin and simvastatin respectively. Method was then validated for accuracy, linearity, precision, specificity, limit of
detection (LOD) and limit of quantification (LOQ) as per ICH Guidelines. The linear regression analysis data for the calibration plots showed good linear relationship with the regression coefficient (r2) of 0.9999 and 0.9994 for the sitagliptin and simvastatin respectively, in the concentration range of 2-6 ?g/spot,0.2-0.6 ?g/spot respectively. The limit of detection and limit of quantification were 5, 20 ng /spot, 50,100 ng /spot respectively for sitagliptin and simvastatin. In conclusion, statistical analysis of data showed that the method is precise, selective and reproducible for estimation of both compounds. Hence the developed method can be applied in routine quality control analysis for identification and quantification of siatgliptin and simvastatin in pharmaceutical formulation.