Determination of Four Kinds of Organic Residual Solvents in Imatinib Mesylate by Capillary Gas Chromatography / 医药导报

ABSTRACT

Objective To establish a method for simultaneous determination of petroleum ether (60-90 ℃),ethyl acetate,ethanol and pyridineas residual organic solvents in imatinib mesylate API. Methods Capillary gas chromatography was adopted.The determination was performed on DB-WAX capillary column with FID detector.The injector temperature was 180 ℃and the temperature of FID was 200 ℃ by temperature programming with nitrogen serving as carrier gas at a flow rate of 5 mL·min-1.The injection volume was 1 μL.With N,N-dimethylformamide(DMF) serving as solvent,four kinds of organic solvent residues in the samples were calculated by external standard method. Results The four kinds of organic solvent were completely separated under the established chromatographic condition.A good linearity was obtained in the concentration ranges of them (r=0.999 8-0.999 9).The sampling precisions (RSDs) were less than 2.0%(n=5).The average recovery rates of ethyl acetate,ethanol and pyridine were 97%-101%and that of petroleum ether was 88.7%(RSD<2.0%,n=5).The limits of detection for them were 0.58,0.42,0.18 and 0.61 ng respectively(S/N=31).The limits of quantification for them were 1.8,2.1,0.5 and 2.5 ng,respectively (S/N=101). Conclusion The method is simple,sensitive,accurate and reliable.