HS-GC Method Development and Validation for the Estimation of Class-2 Residual Solvents in Ivabradine

Abstract

A simple, rapid, accurate method for simultaneous estimation of residual solvents like Dichloromethane, Tetrahydrofuran, Toluene and Xylene in Ivabradine was performed by Head space - Gas chromatography. The residual solvents were separated using a 30 m long DB-624 column with an inner diameter of 0.53 mm and a film thickness of 3.0 m, with a flow rate of 1.2 ml/min and a run period of 12 minutes, using Nitrogen as the carrier gas and Dimethyl Sulphoxide as the solvent. All the head space parameters were maintained to achieve a good separation by maintaining temperature of 95°C -105°C and suitable pressure. Analytical method was also developed by performing various trails by changing various parameters such as chromatographic conditions and head space parameters and an optimized chromatogram was obtained by showing high resolution and accurate peaks. Validation process was carried by using ICH guidelines. All parameters were carried by procedures and results were within limits as per guidelines. Validation parameters such as linearity, precision, accuracy, ruggedness, robustness, LOD, LOQ, Specificity and system suitability were performed and the proposed was said to be more precise, specific, rapid and accurate. The percentage recoveries and peak response of dichloromethane, tetrahydrofuran, toluene and xylene were with range of 90-110% and NMT 15.