顶空毛细管气相色谱法测定富马酸喹硫平中残留有机溶剂

目的建立顶空气相色谱法测定富马酸喹硫平中以富马酸盐形式存在的三乙胺以及甲苯和乙醇三种残留溶剂的方法。方法建立一种以N-甲基吡咯烷酮为溶剂、氢氧化钠水溶液释放三乙胺的顶空进样的方法,采用DB-624石英毛细管柱,经程序升温,氢火焰离子化检测器,载气为氮气,以正丙醇为内标,进样口温度为200℃,检测器温度为250℃。结果三乙胺、甲苯、乙醇在选定的色谱条件下分离良好,定量限分别约为0.53、0.14、20.20 mg·L-1;在0.50²0.00、0.1020.00、0.10⁵8.00和25.0058.00和25.00³25.00 mg·L-1内线性关系良好,其平均回收率分别为99.7%、105.4%和98.3%,RSD均小于10%。结论该方法可以为富马酸喹硫平原料的质量控制提供依据。

Determination of the residual solvents in quetiapine fumarate by headspace gas chromatography

Objective To establish a method for simultaneous determination of the residual triethylamine in its fumarate form, toluene and ethanol in quetiapine fumarate by headspace gas chromatography. Method The sample was dissolved in N-methyl pyrrolidone, and then treated with dilute sodium hydroxide solution in GC headspace vial. Temperature programming was used for the DB-624 capillary column, which was adopted with initial temperature 60 ℃, hydrogen flame ionization detector, nitrogen as carrier gas, and n-propanol as internal standard. The injection temperature was 200 ℃ and the detector temperature was 250 ℃. Result The above solvents could be well separated and determined by this method; The limit of quantitation of triethylamine, toluene and ethanol were separately 0.53, 0.14, 20.2 mg•L^-1. The linear range of these solvents were respectively 0.5-20 mg•L^-1and 0.14-58 mg•L^-1, 25-325 mg•L^-1 with good linear relationship, and the average recovery were 99.7%, 105.4%, 98.3% with RSD less than 10%. The robustness validation of varied GC and headspace parameters and their results showed that the resolution of the three solvents and internal standard exceeded 1.5, the tailing factor were no more than 2.0, and the content variation were within 10%. Conclusion The method can be successfully validated for the residual quality control of quetiapine fumarate for its accuracy, reliability and reproducibility.