顶空气相色谱法测定盐酸雷莫司琼中有机溶剂残留量

目的：应用顶空气相色谱法同时测定雷莫司琼中甲醇、丙酮、乙腈、氯仿、乙醇、醋酸乙酯、二氯甲烷、四氢呋喃和1，2-二氯乙烷等9种有机溶剂的残留量。方法：采用顶空毛细管气相色谱法测定，水为溶剂，色谱柱为DB-624毛细管柱（0．53mm×30m，3μm）；载气为氮气；检测器为FID；程序升温，初始温度为30℃，维持10min后，以10℃·min^-1升温至80℃，再以40℃·min^-1井温至200℃。结果：测得各溶剂的线性良好（相关系数〉0．9975）；平均回收率91．2％～102．3％，检测限为0．08～3．0mg·L^-1。结论：采用顶空毛细管气相色谱法同时对雷莫司琼中9种残留溶剂进行检测，操作简便，重现性好，结果准确可靠。

Determination of Residual Solvents in Ramosetron Hydrochloride by Headspace Gas Chromatography

Objective ：To establish a headspace GC method for determination of residual organic solvents （ acetone, tetrahydrofuran, ethyl acetate, methanol, dichloromethane, ethanol, acetonitrile, chloroform and dichloroethane ） in ramosetron hydrochloride. Methods：Headspace gas chromatography was adopted using a DB-624 capillary column （0. 53 mm× 30 m, 3 μm） with nitrogen as cartier gas and FID as detector. The initial column temperature was set at 30 ℃, maintained for 10min and then raised（ 10 ℃ · min^-1 ） to 80 ℃ and then raised （40℃ · min^-1） to 200 ℃. Results：The calibration curves of the nine solvents were linear （r 〉 0. 997 5 ）. The average recoveries were 91.2% - 102. 3 % . The detection limits were 0.08 -3.0 mg· L^-1. Conclusion：The detection of 9 residual organic solvents with headspace capillary GC is simple and reproducible with accurate and reliable results.