毛细管气相色谱法检查盐酸美普他酚原料药中10种残留溶剂

Determination of 10 Residual Solvents in Meptazinol Hydrochloride by Capillary Gas Chromatography

目的:建立了测定盐酸美普他酚原料药中正己烷、正庚烷、四氢呋喃、乙酸乙酯、甲醇、异丙醇、乙醇、乙腈、甲苯和乙苯10种溶剂残留量的分析方法。方法:采用毛细管气相色谱法,以N,N-二甲基甲酰胺为溶剂,丙酮为内标。色谱柱为DB-WAX,进样口温度为250℃,氢火焰离子化检测器温度为250℃,程序升温。结果:10种残留溶剂在考察的浓度范围内线性关系良好,r为0.9981～0.9999;平均加样回收率为94.7%～106.0%(RSD=1.2%～4.0%)。结论:该方法操作简单、方法灵敏、结果准确,可用于盐酸美普他酚原料药中残留溶剂检查。

OBJECTIVE：To develop the method for simultaneous determination of residual solvents（n-hexane,n-heptane,tetrahydrofuran,ethyl acetate,methanol,isopropanol,ethanol,acetonitrile,toluene and phenylethane） in meptazinol hydrochloride.METHODS：Capillary GC method was adopted.The solvent was dimethylformamide and the internal standard was acetone.The residual solvents were separated on DB-WAX column with FID detector.The injector temperature was 250 ℃,and detector temperature was 250 ℃ with column temperature programming.RESULTS：The good linear relation of 10 kinds of solvents were achieved（r=0.998 1～0.999 9）.The average recoveries were ranged from 94.7%～106.0%（RSD=1.2%～4.0%）.CONCLUSION：The method is simple,sensitive and accurate;it is suitable for the determination of the residual solvents in meptazinol hydrochloride.