The main objective of the present study was to enhance the solubility and dissolution rate of poorly water soluble aceclofenac using its solid dispersion with β-cyclodextrin. FTIR and DSC study was carried out to find out any incompatibility. The phase solubility of drug was carried out in 1, 2, 5, and 10% of β-cyclodextrin in distilled water. Kneading method and solvent evaporation method was use to prepared solid dispersion of aceclofenac and β-cyclodextrin. Different evaluation tests like solubility study in different solvents, PXRD and in vitro dissolution study of aceclofenac- β-cyclodextrin inclusion complex were carried out. The overall finding indicated that β-cyclodextrin is a desirable water soluble carrier, that helps in increasing solubility of drug. Due to its structural feature, β-cyclodextrin forms a good inclusion complex that decreases contact angle of drug with water molecules by increasing wetting properties. Hence, it can be concluded that, β-cyclodextrin is better water soluble carrier molecule in terms of its compatibility and increasing solubility behavior of poorly water soluble drug aceclofenac.

Quality by design approach has been used to develop simple, rapid, sensitive gradient RP-HPLC stability indicating method for fosaprepitant dimeglumine and its related impurities. The chromatographic method has been developed by using symmetry shield RP-18 (250 mm × 4.6 mm; 5 μm) column maintained at column temperature of 20 ºC. The mobile phase-A consisted of water and acetonitrile (800:200, v/v), added 2 mL of orthophosphoric acid and 0.17 g of tetrabutylammonium hydrogen sulphate. The mobile phase-B consisted of water and acetonitrile (200:800, v/v), added 2 mL of orthophosphoric acid and 0.17 g of tetrabutylammonium hydrogen sulphate. Gradient program was executed as time (min)/% MP-A: 0/80, 3/80, 12/40, 20/20, 24/20, 25/80, and 30/80. The UV detection was carried out at wavelength 210 nm and 20 μL of sample was injected. Sample cooler was maintained at 5 ºC. Stability of fosaprepitant dimeglumine sample was investigated in different stress condition as acid, base, oxidation, thermal, humidity and photolytic. The method was developed in two phases, screening and optimization. During the screening phase, the most suitable stationary phase, organic modifier, and solvent were identified based on the behaviour of each stationary phase with fosaprepitant dimeglumine and its impurities using each buffer and solvent. Total 18 experiments were performed to find out the best experimental condition. The optimization was done for secondary influential parameters like column temperature, gradient program, using six experiments to examine multifactorial effects of system suitability parameters and generated design space representing the robust region. A verification experiment was performed within the working design space and the model was accurate. Drug showed unstable behaviour under acid, base, oxidation, thermal, and humidity conditions. Apripetant was found as major degradation impurity. The method was validated as per ICH guideline for specificity, limit of detection (LOD), limit of quantitation (LOQ), linearity, accuracy, precision, ruggedness and robustness. Correlation coefficient is about 0.999 for all impurities, recovery is between 90% to 103% at all level. LOD value of each impurity is less than 0.01% w/w. DOE statistically based experimental designs proved to be an important approach in optimizing selectivity-controlling parameters for the organic impurities determination in FD API. The method was found to be specific, linear, accurate, precise and robust. The peak purity test results confirmed that the fosaprepitant dimeglumine peak was homogenous in all stress samples and the mass balance was found to be more than 99%, thus proving the stability indicating power of the method. Present method is found to be suitable for routine analysis in quality control laboratory.

A Simple, rapid, cost effective, stability indicating RP-HPLC method has been developed for separation of Metformin HCl, its related impurities and Acarbose. Validated the method for simultaneous estimation of Metformin (MF) and Acarbose (ACB) in its novel combination of tablet formulation with Metformin 500 mg and Acarbose 50 mg. Metformin HCl is an orally-administered biguanide, anti-hyperglycemic agent, used in the management of non-insulin dependent diabetes mellitus. Acarbose is an oligosaccharide, used orally for the treatment of type 2 diabetes mellitus. The separation was achieved by using isocratic mobile phase consisting of mixture of phosphate buffer : acetonitrile (27:73 v/v), using Hypersil APS- 2 column, (250 x 4.6 mm x 5m) column at flow rate 2.0 mL/min. The detection was carried out at 210 nm with 20 μl of injection volume. The column temperature was maintained at 35 °C. The retention time (RT) of MF, its related impurities and ACB were found to be RT 2.6 min for 1-Cynogaunidine (RC A), 6.0 for Metformin (MF), 8.5 for 1-Methylbigaunidine (RC B), 10.4 for N,N-Dimethyl-1,3,5-triazine-2,4,6-triamine(RC C), and 12.2 min for Acarbose (ACB). The approach was found to be linear with the concentration of 5-25 μg/ml and 2.5- 15μg/ml and correlation coefficient was 0.999 for MF and ACB respectively. The assay of estimated compounds was found to be 99.19% and 99.08% w/v and mean accuracy 100.66%, 101.59% for MF and ACB respectively. The developed method was validated as per ICH guidelines. The degradation products were well resolved from main peak. The validation was performed for various parameters like specificity, linearity, precision, accuracy and robustness studies. The method was found to be capable for simultaneous quantification of Metformin and Acarbose in its combination drug.