顶空-毛细管气相色谱法测定氟马西尼中有机溶剂残留量

Capillary gas chromatography determination with headspace sampling of the residual organic volatile solvents in flumazenil

目的:同时测定氟马西尼中4种有机溶剂残留量。方法:顶空进样程序升温法,检测器为 FID,色谱柱为 HP-5毛细管柱(30.0 m×320μm×0.25μm),溶剂为水。结果:乙醇、氯仿、醋酸、N,N-二甲基甲酰胺线性的相关系数分别为0.9999,0.9996,0.9991,0.9972;平均回收率(n=5)分别为102.3%,91.5%,97.8%,105.4%,RSD 分别为2.4%,3.1%,4.5%,4.2%。结论:方法柱效高、简单、准确、快捷,适用于氟马西尼中有机溶剂残留量测定。

Objective：To determine the residual organic volatile solvents in flumazenil. Method：The samples were injected by headspace sampler while program heating and FID detector were used. The determination was performed on a 5% Pbenyl Methyl Siloxane HP-5 GC column（ （30. 0 m ×320 μm ×0. 25 μm） while water was used as solvent. Results：The regression coefficients of ethanol,chloroform,acetic acid and DMF were 0. 9999,0. 9996,0. 9991 and 0. 9972, respectively. The recoveries （ n = 5 ） were 102. 3% , 91.5%, 97. 8% and 105.4% respectively with RSD 2. 4%, 3.1% ,4. 5% and 4. 2% accordingly. Conclusion：The methodology appeared to be sensitive,simple, accurate and efficient, and can be used for the determination of the residual organic volatile solvents of flumazenil.