顶空气相色谱法测定硫酸羟基氯喹中的残留溶剂

Determination of residual organic solvents in hydroxychloroquine sulfate by headspace gas chromatography

目的:采用顶空气相色谱法测定硫酸羟基氯喹中残留有机溶剂甲醇、乙醇、丙酮、正己烷、环己烷、甲苯、二氯甲烷的含量。方法:氢火焰离子化检测器(FID),以10%N-N二甲基甲酰胺水溶液为溶剂,采用PE毛细管柱30m×0.25mm×1.8μm,初始温度40℃,保持4min,以10℃.min-1的升温速度升至180℃,保持1min;检测室温度:250℃;汽化室温度:200℃,柱流量(N2):0.5mL.min-1,分流比10∶1,实现了各组分的基线分离。结果:样品中各有机溶剂残留量均符合要求。结论:经方法学试验验证,该方法灵敏、准确、可靠,适用于硫酸羟基氯喹有机溶剂残留量的测定。

To establish the determination method of hydroxychloroquine sulfate in the residual solvents methanol,ethanol,acetone, n-hexane, cyclo-hexane, toluene, dichloromethane by headspace gas chromatography method. Methods： The PE Elite 17 capillary column（30m × 0.25mm× 1.8υm）was adopted with nitrogen as carrier gas, hydrogen flame ionization detector, injection port temperature of 200~℃C and detector temperature of 250℃. The temperature program- ming was used for column temperature： initial temperature of 40℃ , maintained for 4 min, and then rose to 180℃ with the rate of 10℃ · min^-1 ,maintained for 1 min with the flow rate of 0. 5mL· min^-1. The split ratio was 10： 1. Under the above conditions, various components were separated completely. Conclusion： The method is simple, accurate and reliable, which can be used to detect the residual solvents in hydroxychloroquine sulfate.