顶空毛细管气相色谱法测定硫酸特布他林有机溶剂残留

Determination of Three Residual Solvents in Terbutaline Sulfate by Headspace Capillary Gas Chromatography

目的建立测定硫酸特布他林原料药中3种有机溶剂残留量的气相色谱法。方法采用顶空毛细管气相色谱法,以1%二甲亚砜水溶液为溶剂,DB-624型毛细管柱(30.0 m×320μm,1.8μm),氮气为载气,氢火焰离子化检测器(FID),柱温采用程序升温。结果甲醇、异丙醇与甲苯3种有机溶剂均达到了完全分离,在考察的质量浓度范围内线性关系均良好,最低检测限分别为2.4,2.6,0.8μg/mL,高、中、低3种质量浓度的回收率均大于98%。结论该方法灵敏度、准确度均达到有机溶剂残留量的检测要求,可用于硫酸特布他林中甲醇、异丙醇与甲苯残留的检测和分析。

Objective To establish a headspace capillary gas chromatography method for simultaneously determining the residual organic solvents in terbutaline sulfate. Methods The headspace capillary gas chromatography method was adopted with 1% aqueous solution of DMSO as the solvent. The DB-624 capillary column（ 30. 0 m × 320 μm,1. 8 μm） was adopted with N_2 used as the carrier gas.Temperature programming was used for column temperature by FID detector. Results The 3 residual organic solvents（ methanol,isopropanol,methylbenzene） were completely separated. A good linearity in the experimental concentration was shown. The limit of detection was 2. 4,2. 6 and 0. 8 μg/mL. The average recoveries of 3 kinds of high,medium and low concentrations were all more than 98%.Conclusion The sensitivity and accuracy of this method are up to the requirement for the detection of residual organic solvents,which can be used for the detection and analysis of 3 residual solvents（ methanol,isopropanol and toluene） in terbutaline sulfate.