顶空毛细管气相色谱法测定去氧孕烯中有机溶剂残留量

Determination of organic solvent residues in desogestrel by headspace capillary gas chromatography

建立了顶空毛细管气相色谱法测定去氧孕烯中残留有机溶剂的方法。色谱柱为DB-624毛细管柱,柱温为程序升温,以氮气为载气,用氢火焰离子化检测器(FID)检测。在实验条件下,甲醇、乙醇、丙酮、正己烷、醋酸乙酯、四氢呋喃、环己烷回收率分别为98.5%、97.9%、97.3%、98.2%、97.2%、97.7%、98.5%%,精密度分别为1.7%、2.0%、1.5%、3.1%、1.5%、1.7%、2.2%。在去氧孕烯原料中只检测出了乙醇、丙酮。本法可快速、准确测定去氧孕烯中残留溶剂含量。

A method for determining organic solvent residues in desogestrel by headspace capillary gas chroma tography was developed. A DB-624 caillary column was applied with nitrogen as carrier gas and FID for detection. Organic solvent residues were separated under gradient temperature. Under experimental condi- tions, the recoveries of methanol, ethanol, acetone, N-hexane, acetic ether, tetrahydrofuran and hexamethylene were 98.5%, 97.9%, 97.3% 98.2%, 97.2%, 97.7% and 98.5%, respectively, and the precisions were 1.7%, 2.0%, 1.5%, 3.1%, 1.5%, 1.7% and 2.2%, respectively. The experimental results showed that only ethanol and acetone were found in raw desogestrel. The method is rapid and accurate,and can be used to the determination of seven ogranie solvent residues in desogestrel.