Determination of 6 Residual Solvents in Afatinib Dimaleate by HS-GC
Objective:To establish a HS-GC method for simultaneous detection of six residual solvents Including ethanol,butyl acetate,tetrahydrofuran,dichloromethane,methyl cyclohexane,methyl tert butyl ether in Afatinib dimaleate,and determine 6 residual solvents in 7 batches of samples.Methods:Chromatographic Column with 6%cyanopropylbenzene and 94%dimethylsiloxane as the stationary liquid,the initial column temperature is set to 40℃,and lasting for 8 minutes,after raised to 180℃at 10℃/min,after lasting for 8 minutes.The detector temperature is 220℃,the column flow rate is 1.0 mL/min,the Split Ratio is 5:1,the equilibrium temperature of the sample bottle is 80℃and the balance time of the sample bottle is 30 min.Results:Under the selected experimental method,the resolution between the solvent peaks meets the requirements.Ethanol,butyl acetate,tetrahydrofuran,dichloromethane,methyl cyclohexane,methyl tert butyl ether have good linear relationship between the range of 20%～150%of their respective limit concentrations(r≥0.9980),and the average recovery was 91.3%～107.4%,and the quantitative limit is 0.154～3.43 μg/mL.And butyl acetate,tetrahydrofuran,dichloromethane,methyl cyclohexane,methyl tert butyl ether were not detected in many batches of Afatinib dimaleate,and the detection amount of ethanol is between 0.02%and 0.06%,all of which are less than 30%of the limit.Conclusion:The method has the advantages of simple detection,strong specificity,high detection sensitivity,accurate and repeatable.It can be used for the determination of 6 residual solvents in Afatinib dimaleate at the same time.
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