顶空气相色谱法测定盐酸青藤碱中三氯甲烷的残留量

目的：建立毛细管色谱法测定盐酸青藤碱中三氯甲烷的残留量。方法：采用DB-624毛细管色谱柱（30 m×0.32 mm，涂层厚1.8 μm），载气为氮气，进样口温度为200 ℃，柱温为65 ℃，检测器温度为230 ℃，FID为检测器，顶空进样法，水为溶剂，平衡温度70 ℃，平衡时间45min。结果：三氯甲烷在0.1845～18.45 μg·mL^-1范围内呈良好的线性关系（r ＝0.9995）；平均回收率为98.2％，RSD为2.2％（n=6）；最低检出限为36.9 ng·mL^-1。结论：该方法灵敏、简单、准确，可用于测定盐酸青藤碱中三氯甲烷的残留量。

Objective:A headspace GC method was established for determination of residual chloroform in sinomenone hydrochloride.Method:Using a DB-624 column with 30 m long and 0.32 mm in internal diameter(diameter 1.8 μm),with nitrogen as carrier gas and FID as detector. The injector temperature was 200 ℃,the column temperature was 65 ℃ and the detector temperature was 230 ℃.Water was used as solvent ,and samples had been equilibrated at 70 ℃ for 45 minutes.Results:The calibration curves of chloroform showed good linearity in the range of 0.1845-18.45 μg·mL^-1 (r=0.9995);The average recovery was 98.2% with RSD 2.2%(n=6); The detection limit was 36.9 ng·mL^-1.Conclusion:The method is accurate sensitive,simple and reliable,it is suitable for measurement of residual chloroform in the sinomenone hydrochloride.