ICH guidelines

Iloperidone is a novel antipsychotic drug widely used to treat schizophrenia. Objective of this investigation was to develop a validated stability indicating high performance thin layer chromatographic method for the quantification of iloperidone in bulk and pharmaceutical dosage form. Aluminium backed TLC plates precoated with silica gel 60F-254 was employed as the stationary phase and n-propanol: chloroform (5:5 v/v) as the mobile phase. Densitometric analysis was performed at 275 nm in the reflectance mode. Compact spots of iloperidone with Rf value 0.36 were observed. Validation of the method as per ICH guidelines produced satisfactory results of linearity (r2>0.999), limit of detection (5.349 ng/spot), limit of quantification (16.2099 ng/spot), precision (< 2%), and accuracy (99.66 ±0.341 to 100.34±0.292%). Degradation products were found to be well separated from the pure drug with significantly different Rf values suggesting a stability indicating analysis method for the estimation of iloperidone in pharmaceutical preparations and as bulk drug. The proposed method is selective, sensitive, precise, and accurate. It is also simple, economic and time saving as compared to reported HPLC methods. 

A novel, precise and selective high performance liquid chromatographic method was developed for the estimation of paliperidone using paracetamol as the internal standard. Separation was achieved on a LiChrospher® RP-18 HPLC column (5 μ particle size and 25 cm × 4.6 mm internal diameter) using 10 mM ammonium acetate: methanol in the ratio of 10:90 (v/v) as the mobile phase, at flow rate of 0.7 ml/min and the eluate was monitored at 277 nm. The method was validated in compliance with ICH guidelines. The correlation coefficient of the calibration graph was 0.99946±0.00037 over the concentration range 1 to 5 µg mL-1. The limit of detection and limit of quantification were 0.569 µg mL-1 and 1 µg mL-1, respectively. Overall percentage recovery of paliperidone ranged between 98.92±0.595 to 100.30±0.693. Relative standard deviations for intra- and inter-day precision studies were