Simultaneous determination of 13 solvents in Ruxolitinib Phosphate by headspace injection gas chromatography
A method for the determination of the residual amount of 13 organic solvents in the raw material of Ruxolitinib Phosphate by headspace injection gas chromatography was established,including methanol,ethanol,isopropanol,acetonitrile,dichloromethane,methyl tert butyl ether,ethyl acetate,tetrahydrofuran,isopropyl acetate,n-heptane,1,4-dioxane,toluene,and N,N-dimethylformamide.DB-624 capillary chromatography column was used as separation column,with headspace equilibrium temperature of 100℃,and headspace equilibrium time of 30 min.Hydrogen flame ionization detector was used to determine and quantification was performed using chromatographic peak area external standard method.The linear relationship between the mass concentrations of 13 organic residual solvents and their corresponding chromatographic peak areas was good within a certain concentration range,and the correlation coefficients were all more than 0.995.The method detection limists were 0.02-3.35 μg/mL,and the quantitation limits were 0.07-11.18 μg/mL.The average recoveries for spiked samples were 99.1%-107.4%,and the relative standard deviations of nine measurement results were 4.9%-6.9%.This method exhibits strong specificity and high accuracy,making it suitable for the detection of residual organic solvents in the active pharmaceutical ingredient of ruxolitinib phosphate.
headspace gas chromatographyRuxolitinib Phosphateresidual organic solventsquality control
万方数据
维普
