毛细管气相色谱法测定辛伐他汀中5种有机溶剂残留量

Determination of organic residual solvents in simvastatin by gas chromatography

目的 采用气相色谱法测定辛伐他汀原料药中甲醇、醋酸乙酯、环己烷、甲苯及四氢呋喃 5种有机溶剂的含量。方法 使用毛细管色谱柱 ,以 6 %氰丙基苯基 94%二甲基聚硅氧烷 (DB 62 4 )为固定相 ,以二甲基甲酰胺为溶剂 ,正戊烷为内标 ,FID检测器 ,柱温 1 1 0℃ ,气化室及进样口温度均为 2 50℃。结果 5种有机溶剂实现基线分离且线性关系良好 ,加样回收率均得到满意结果。结论 经实验方法学验证 ,该方法灵敏、准确 。

OBJECTIVE: A gas chromatography method was established to determine the contents of methanol, ethyl acetate, cyclohexane, toluene and tetrahydrofuran, the residual organic volatile solvents, in simvastatin raw material. METHODS: After dissolved in dimethylformamide, 1μl sample solution was injected on to a DB-624 capillary column with column temperature at 110°C and detected by FID detector. The five organic volatile solvents and the internal standard n-pentane were separated thoroughly. RESULTS: The liner range and the recoveries for five organic solvents were satisfied. Three batches of samples were analysed. CONCLUSION: The method was proved to be accurate, sensitive and reliable. It is quite suitable to be used in the analysis of the organic volatile solvents in bulk pharmaceuticals.