顶空气相色谱法测定格隆溴铵中溶剂残留量

Determination of Residual Solvent in Glycopyrronium Bromide by Headspace Gas Chromatography

目的:建立顶空毛细管气相色谱法测定格隆溴铵中7种有机溶剂残留量的方法。方法:采用毛细管气相色谱法。色谱柱为DB-624弹性石英毛细管柱(30 m×0.32 mm,1.8μm);载气为氮气;检测器为FID;进样口和检测器温度均为250℃;柱温为程序升温,初始温度40℃,保持15分钟,以每分钟20℃升温至200℃。顶空进样:平衡温度为80℃,平衡时间为30 min,分流比为10:1,水为溶剂,正丙醇为内标物。结果:被测物在考察的范围内线性关系良好(r≥0.9990),平均回收率为90.7%~102.1%,检测限分别为。结论:本法灵敏度高,简单,易行,结果准确可靠,该法可用于格隆溴铵原料药中有机溶剂残留量的检查。

Objective A method for the determination of the residual amounts of seven organic solvents in glycopyrronium bromide by headspace capillary gas chromatography was established.Method Capillary gas chromatography is used.The chromatographic column is a DB-624 elastic quartz capillary column(30 m×0.32 mm,1.8μm);the carrier gas is nitrogen;the detector is FID;the inlet and detector temperature are both 250℃;the column temperature is the programmed temperature rise,the initial keep the temperature at 40℃for 15 minutes,and increase the temperature to 200℃at 20℃per minute.Headspace sampling:equilibrium temperature is 80℃,equilibrium time is 30 min,split ratio is 10:1,water is solvent,n-propanol is internal standard.Results The measured substances have a good linear relationship(r≥0.9990)within the range examined,with an average recovery rate of 90.7 to 102.1%,and the detection limits are respectively.Conclusion This method is high in sensitivity,simple,easy to implement,and the results are accurate and reliable.This method can be used for the inspection of the residual amount of organic solvents in glycopyrrolate bromide raw materials.