Abstract

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF ESTIMATION OF RESIDUAL SOLVENTS IN ESMOLOL HYDROCHLORIDE API BY HEAD SPACE GAS CHROMATOGRAPHY

S. Mouleeswaran*, P. D. Gokulan and K. L. Senthil Kumar

ABSTRACT

The developed Head Space Gas Chromatography (GC-HS) method forthe analysis of Development and Validation of Estimation of ResidualSolvents in Esmolol Hydrochloride API is Precise and feasible. Theseparation was carried out on the DB-624 Column, (length- 60m x InnerDiameter-0.53 mm), Film Thickness-3.0 μm; using Nitrogen as CarrierGas, Hydrogen as Flammable gas and Zero air as Oxidizing agent withFlow rate 3.5 mL/min, Detector temperature-250oC, Injection mode-Split and Ratio-1:1, Linear velocity-24.4 cm/sec, Flow control mode-Pressure, Total flow- 10.0 mL/min, Run time-30 minutes. All Solventsare separated well with the acceptance Criteria limit of Resolution. Theretention time of Methanol is about 6.5Min, Acetone is about 9.2Min,Isopropyl Alcohol is about 9.5, Dichloromethane is about 10.3Min,Ethyl Acetate is about 13.4Min, n-Heptane is about 15.9Min,1,4,Dioxane (Internal standard) is about 17.6Min, Methyl isobutylKetone is about 19.0Min, Pyridine is about 19.4Min. System suitability parameter were meetsthe acceptance criteria and %Relative standard deviation was within the limit. TheCorrelation coefficient of Linearity for individual solvent, obtained from three replicateinjection are not less than 0.998. And all the solvent Recoveries are within the limit of 80% to120%. The method was validated as per International Council for Harmonization (ICH) norms and the method is also cost effective. The proposed method is useful for rapid analysisof estimation of residual solvents in Esmolol Hydrochloride API.

Keywords: Head Space Gas Chromatography (GC-HS), Residual Solvents (Methanol, Acetone, Isopropyl Alcohol, Dichloromethane, Ethyl Acetate, n-Heptane, 1, 4 Dioxane, Methyl isobutyl Ketone, Pyridine), Esmolol Hydrochloride API.