顶空毛细管气相色谱法测定富马酸喹硫平中残留溶剂

目的 建立富马酸喹硫平中残留溶剂乙醇、甲苯的气相色谱测定方法.方法 采用DB-624弹性石英毛细管柱(30 m×0.53 mm×3.0 μm),载气为氮气,氢火焰离子化检测器,进样口温度为180 ℃,检测器温度为300 ℃.柱温采用程序升温:初始温度为50 ℃,保持5 min,然后以8 ℃/min的速率升至130 ℃,保持5 min;流速为2 mL/min.分流比为1∶60,以80%乙腈为样品的溶剂.结果 使用该方法乙醇、甲苯得到了较好的分离与测定;回收率分别为95.72%和88.59%,相对标准偏差(RSD)分别为2.4%和4.3%;精密度RSD分别为1.1%和4.0%.结论 该方法简便、准确、可靠,可用于药品检验中富马酸喹硫平中残留溶剂的测定.

Determination of residual solvents in quetiapine fumarate by head-space capillary gas chromatography

Objective To establish the determination method of quetiapine fumarate in the residual solvent ethanol and toluene by gas chromatography method. Methods The DB624 flexible quartz capillary column（30 m×0.53 mm × 3.0μm） was adopted with nitrogen as carrier gas,hydrogen flame ionization detector,injection port tern perature of 180 ℃ and detector temperature of 300℃. The temperature programming was used for column temperature： initial temperature of 50℃ ,maintained for 5min,and then rose to 130 ℃ with the rate of 8 ℃/min,maintained for 5min with the flow rate of 2 mL/min. The split ratio was 1 ： 60 with 80% acetonitrile as solvent for samples. Results Ethanol and toluene were better separated and determined by this method. The recovery rates were 95.72% and 88.59% respectively,RSD were 2.4 % and 4.3%, respectively. RSD of precisions 1.1% and 4.0 %, respectively. Conclusion The method is simple,accurate and reliable,which can be used to detect the residual solvents in quetiap ine fumarate.