ICH guidelines.

The aim of the research study was the development and validation of a simple, rapid, accurate and precise reversed-phase high performance liquid chromatography (RP-HPLC) stability-indicating method for the determination of aceclofenac in bulk and pharmaceutical dosage forms. The RP-HPLC studies was performed on the instrument Jasco HPLC system with Jasco UV 2010 photo diode array detector, ODS C18 RP-column (Intersile 250 mm × 4.6 mm; i.d. 10 μm), Rheodyne injection syringe with 20µL loop volume and windows based chrompass software was used for separation. The isocratic elution was performed using the mobile phase ratio of methanol: water (65:35 v/v) and UV detection wavelength at 263 nm. The overall run time of the analysis was 20 minutes and the flow rate was 1.0 mL/min. The RP-HPLC method developed for analysis of aceclofenac was validated as per the ICH guidelines with respect to specificity, selectivity, linearity, accuracy, precision and robustness. The linearity for developed method was observed in the concentration range of 5-50 μg/mL with the correlation coefficient (r2) of 0.9992. The percentage accuracy of aceclofenac ranged from 99.40 to 100.79%. The relative standard deviation for inter-day precision was lower than 2.0%. The assay of aceclofenac was determined in tablet dosage form was found to be within limits. Aceclofenac was subjected to stress conditions such as neutral, acidic, alkaline, oxidation, and photolysis degradations as per ICH guidelines. The results of degradation studies revealed that the drug degraded a maximum (32.68%) in acidic conditions followed by alkaline conditions (15.05%). The drug was found to be resistant towards neutral, acidic and photolytic degradation conditions.

A new stability indicating RP-HPLC method was described for the assay of olmesartan in market formulations. This developed RP-HPLC method was based on high performance liquid chromatographic (HPLC) separation of olmesartan with the use of a reversed phase HPLC column [Kromasil BDS, C18, 100 x 4.6 mm, 5μ] with mobile phase consisting of .01M KH2PO4 buffer (pH-4.5) and acetonitrile in the ratio of 55:45 %v/v at ambient temperature. The flow rate of the mobile phase was adjusted to 1.0mL/min and the injection volume was 10μL. Detection was performed by photodiode array detector at a wavelength of 257nm and the chromatographic runtime was 8 minutes for the analysis. The reliability and analytical performance of the proposed method, including linearity, range, precision, accuracy, detection and quantitation limits, were statistically validated. The proposed method can be adopted apparently for routine quality control analysis of raw materials, formulations and testing

A novel, convenient, accurate, precise and reproducible reverse phase high performance liquid chromatography was developed and validated for the estimation of Vilazodone in bulk and pharmaceutical tablet dosage form. Objective was achieved under optimized chromatographic conditions on Shimadzu LC-20AT Prominence Liquid Chromatograph with Welchrom C18 isocratic column, (250 mm × 4.6 mm i.d., particle size 5 μm, maintained at ambient temperature), is used as stationary phase. An isocratic mode with mobile phase consisting of Acetonitrile: Water (50:50 v/v), with apparent pH of 3.3, at a flow rate of 1.0 mL/minutes. The effluent was monitored at 240 nm using Shimadzu SPD-20A prominence UV-Vis detector. The retention time of Vilazodone was found to be 4.103 minutes. The linearity range was found to be 1-5 μg/mL with correlation coefficient (R2) is 0.999. Validation parameters such as specificity, linearity, precision, accuracy, and robustness, limit of detection (LOD) and limit of quantitation (LOQ) were evaluated for the method according to the International Conference on Harmonization ICH Q2 (R1) guidelines. The LOD and the LOQ were found to be 0.044 μg/mL and 0.135 μg/mL respectively. Recovery of Vilazodone was found to be in the range of 99.80 % - 99.92 %. The method was validated statistically using the % RSD and the values are found to be within the limits. Therefore this method was conveniently and easily applied for the quantitative determination of Vilazodone in pharmaceutical dosage forms.

A simple, sensitive, accurate and precise high performance thin layer chromatographic method was developed and validated for simultaneous determination of efavirenz (EFA), emtricitabine (EMT) and tenofovir (TEN) in combined tablet formulation and forced degradation studies were performed as per ICH guidelines. Precoated silica gel 60F 254 was used as stationary phase and the mobile phase used was chloroform: methanol (90:10), gives high resolution for each drug. The densitometric evaluation of each drug was carried out at 262 nm. The developed method was simple, accurate and is suitable for analysis of the drugs and degradation products in stability studies of samples.

  Linagliptin frequently associated in pharmaceutical a formulation that reduces blood sugar levels in patients with type 2 diabetes. Their quantification presents several problems. A HPLC method for the determination of these compounds in pharmaceutical formulations, including the separation of impurities and excipients has been developed and validated. The method was simple, selective, linear, precise and accurate. Isocratic elution at a flow rate of 1ml min-1 was employed on a symmetry C18 column at ambient temperature. The mobile phase consisted of Methanol: Water 83:17(v/v) and pH of the mobile phase was adjusted to 4.1 with 0.1% Orthophosphoric Acid . The UV detection wavelength was at 241nm.Linearity was observed in concentration range of 5-30ppm. The retention time for Linagliptin was 5.85min.The method was validated as per the ICH guidelines. The proposed method can be successfully applied for the estimation of Linagliptin in pharmaceutical dosage forms. Key Words: Linagliptin, HPLC Development and Validation, ICH guidelines.