顶空气相色谱法同时测定硫酸特布他林中10种有机溶剂残留量

Simultaneous determination of 10 residual organic solvents in terbutaline sulfate by headspace gas chromatography

目的建立硫酸特布他林中甲醇、乙醇、丙酮、甲基叔丁基醚、乙酸乙酯、四氢呋喃、苯、乙酸、甲苯和氯化苄共10种有机溶剂残留量的测定方法。方法采用顶空气相色谱法,色谱柱为DB-624UI毛细管柱(30 m×0.32 mm,1.80μm),柱温采用程序升温;进样口温度为200℃;检测器为氢火焰离子化检测器,检测器温度为250℃,溶剂为体积分数为70%二甲基甲酰胺。结果 10种溶剂完全分离;在考察的质量浓度范围内线性关系良好,相关系数r>0.999 4,平均回收率为95.7%~102.4%。结论建立的顶空气相色谱法可用于硫酸特布他林中残留溶剂的测定。

Objective To develop a headspace GC method for the determination of residual organic solvents such as methanol, ethanol, acetone, methyl tert-butyl ether, ethyl acetate, tetrahydrofuran, benzene, acetic acid,toluene, benzyl chloride in terbutaline sulfate. Methods Separation was performed on a DB-624UI capillary column （ 30 m×0.32 mm,1.80μm） using temperature programming. The inlet temperature was 200 ℃; FID was used as detector with a temperature of 250 ℃; the sample was dissolved in dimethylformamide- water mixture （ V： V = 7： 3 ）. Results Ten residual solvents were separated completely. It was appeared to present a good linearity within the experimental concentration and all correlation coefficients were no less than 0. 999 4. The average recoveries were in the range of 95.7% - 102.4%. Conclusions The established method can be used for the determination of the residual solvents in terbutaline sulfate.