顶空气相色谱法测定盐酸拉贝洛尔中有机溶剂残留量

目的建立顶空气相色谱法测定盐酸拉贝洛尔中有机溶剂残留量。方法采用顶空气相色谱法,色谱柱为聚乙二醇毛细管柱,载气为氮气,流速为4.5mL.min-1。FID检测器,检测器温度为250℃;进样口温度为200℃;程序升温为初始温度40℃,保持5min,以5℃.min-1升至80℃,再以30℃.min-1升至200℃,保持5min。顶空进样,平衡温度为100℃,平衡时间为30min,分流比为1∶1,二甲亚砜为溶剂,外标法测定盐酸拉贝洛尔中丙酮、乙酸乙酯、甲醇、乙醇和异丙醇的残留量。结果在此色谱条件下，几种有机溶剂均能得到良好的分离，空白对照无干扰，峰面积与检测浓度在所考察的范围内具有良好的线性，r=0．999440．9998；平均回收率为96．0％～106．8％，精密度均小于2．oH，丙酮、乙酸乙酯、甲醇、乙醇和异丙醇最低检出限分别为0．091、0．171、0．738、0．534、0．412μg·mL^-1。结论本试验建立的色谱方法灵敏、准确，适合盐酸拉贝洛尔原料中有机溶剂残留量的检测。

Determination of Residual Solvents in Labetalol Hydrochloride by Headspace GC

Objective To establish a method of Head-space capillary gas chromatography for the determination of residual solvents in labetalol hydrochloride.Methods The residual solvents in labetalol hydrochloride were separated by PEG capillary column with an FID detector.The carried gas was nitrogen.The injector temperature and the detector temperature were controlled at 200℃ and 250℃,respectively.The programmed column temperature was set as follows： maintained at 40℃ for 5min and then raised to 80℃ at the rate of 5℃·min-1 and then raised to 200℃ at the rate of 30℃·min-1 followed by holding for 5min.The sample was dissolved in dimethyl sulfoxide.The containers of head-space injector were in equilibrium at 100℃ for 30min,the splitting-ratio was 1∶1.Results The detected solvents were seperated completely.The calibration curve of each solvent showed a good linear relationship（r=0.9994-0.9998） with good precision and accuracy（not more than 2.0%）.The average recovery rate was in the range of 96.0%-106.8%.The LOD of acetone,ethyl acetate,methanol,ethanol and isopropyl alchol were 0.091,0.171,0.738,0.534 and 0.412μg·mL^-1 respectively.Conclusion The established method is accurate and reliable.It can be used for the determination of residual solvents in labetalol hydrochloride.