气相色谱法测定候选新药SM934原料中有机溶剂残留量

Determination of residual organic solvents in SM934 by gas chromatography

目的建立气相色谱法测定候选新药SM934中6种残留有机溶剂的含量。方法采用毛细管气相色谱法,使用DM-5石英毛细管柱(30 m×0.25 mm,0.25μm),采取程序升温,分离测定甲醇、乙醇、二氯甲烷、乙酸乙酯、石油醚和N,N-二甲基甲酰胺的残留量。结果 6种有机溶剂完全分离,线性范围为13.0～250.0 mg.L-1,精密度良好,加样回收率在97%～105%之间(RSD<4%)。结论本法灵敏、准确、可靠,适用于候选新药SM934质量控制中有机溶剂残留量的检测。

AIM To establish a capillary gas chromatography method for the determination of residual organic solvents in SM934.METHODS A capillary gas chromatography with DM-5 capillary column（30 m × 0.25 mm,0.25 μm） was used to determine the residues of methanol,ethanol,dichloromethane,ethyl acetate,petroleum ether and N,N-dimethylformamide.RESULTS The six organic solvents were separated completely.The linear range was 13.0-250.0 mg.L-1.The average recovery rate was in the range of 97%-105%（RSD 4%）.CONCLUSION This method is accurate,sensitive and reliable for the determination of residual organic solvents in quality control of SM934.