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

摘要: 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%。

Abstract: 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 (3S/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%.