气相色谱法测定雷莫司琼中有机溶剂的残留量

Determination of Residual Organic Solvents in Ramosetron by GC

目的应用气相色谱顶空进样法同时测定雷莫司琼中丙酮、四氢呋喃、醋酸乙酯、甲醇、二氯甲烷、乙醇、乙腈、氯仿和二氯乙烷等9种有机溶剂的残留量。方法采用HP-INNOWAX(聚乙二醇)石英毛细管柱(30 m×0.32 mm,0.5μm);载气为氮气;检测器为FID。结果测得各溶剂的线性良好(相关系数>0.997 5);丙酮、四氢呋喃、醋酸乙酯、甲醇、二氯甲烷、乙醇、乙腈、氯仿和二氯乙烷平均回收率分别为97.9%,101.9%,96.4%,99.8%,95.7%,99.2%,97.6%,100.5%和94.7%,检测限分别为0.24,0.14,0.23,3.17,0.66,0.23,0.39,2.96,0.05μg.mL-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。

Objective To establish a headspace GC method for the determination of residual organic solvents （ acetone, tetrabydrofuran, ethyl acetate, methanol, dichloromethane, ethanol, aeetonitrile, chloroform and dichloroethane） in ramosetron . Methods A HP INNOWAX capillary column （30 m × 0.32 mm,0.5 μm） was used with nitrogen gas as carrier and FID as detector. Results The calibration curves of the nine solvents were linear （ r 〉 0.997 5 ）. The average recoveries were 97.9%, 101.9% ,96.4% ,99.8% ,95.7% ,99.2% ,97.6%, 100.5% and 94.7% respectively. The detection limits were 0.24,0.14,0.23,3.17,0.66,0.23,0.39,2.96 and 0.05μg·mL^-1 respectively. Conclusion The detection of 9 residual organic solvents with headspace capillary GC is simple and reproducible with accurate and reliable results.