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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0.50~20.00、0.10~58.00和25.00~325.00 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。
OBJECTIVE To establish a method for the determination of triethylamine and toluene and ethanol residues in the form of fumarate in quetiapine fumarate by headspace gas chromatography. Methods A method for the headspace sampling of triethylamine released by aqueous solution of N-methylpyrrolidone and aqueous sodium hydroxide was established. The sample was heated on a DB-624 quartz capillary column with programmed temperature rising, hydrogen flame ionization detector, carrier gas For nitrogen, with n-propanol as internal standard, inlet temperature of 200 ° C and detector temperature of 250 ° C. Results Triethylamine, toluene and ethanol were separated well under the selected chromatographic conditions with the limits of quantitation of 0.53, 0.14 and 0.20.20 mg · L-1, respectively. At 0.50 ~ 20.00, 0.10 ~ 58.00 and 25.00 ~ 325.00 mg · L- 1 within the linear relationship was good, the average recovery rates were 99.7%, 105.4% and 98.3%, RSD were less than 10%. Conclusion This method can provide the basis for the quality control of quetiapine fumarate.