顶空-气相色谱法测定富马酸伊布利特原料药中5种溶剂残留量

Determination of 5 Solvents Residues in Ibutilide Fumarate Active Pharmaceutical Ingredient by Headspace-Gas Chromatography

建立了顶空-气相色谱法测定富马酸伊布利特原料药中5种溶剂残留量的方法。样品用N,N-二甲基甲酰胺(DMF)溶解,采用DB-624毛细管色谱柱进行分离,初始柱温为40℃,用火焰离子化检测器检测。结果表明:二氯甲烷、四氢呋喃、乙酸乙酯、乙醇和丙酮等5种溶剂均能完全分离,并在一定范围内呈线性关系,检出限(3S/N)依次为0.74,0.042,0.056,0.17,0.050 mg·L^(-1)。按标准加入法进行回收试验,测得回收率为102%~105%,测定值的相对标准偏差(n=5)均小于2.0%。

A method was established for determination of 5 solvents residues in ibutilide fumarate active pharmaceutical ingredient(API)by headspace-gas chromatography.The sample was dissolved in N,N-dimethylformamide(DMF)and separated on DB-624 capillary column,with initial column temperature of 40℃.The flame ionization detector was used for detection.The results showed that 5 solvents including dichloromethane,tetrahydrofuran,ethyl acetate,ethanol and acetone,could be completely separated,and linear relationships of 5 solvents were found in definite ranges.The detection limits(3 S/N)were 0.74,0.042,0.056,0.17,0.050 mg·L^(-1) respectively.Tests for recovery were made by standard addition method,giving results in the range of 102%-105%,and RSDs(n=5)of the determined values all less than 2.0%.