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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1.8μm),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0.1845～18.45μg·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: To establish a method for the determination of chloroform in sinomenine hydrochloride by capillary chromatography. Methods: The DB-624 capillary column (30 m × 0.32 mm, 1.8 μm coating thickness) was used. The carrier gas was nitrogen. The inlet temperature was 200 ℃, the column temperature was 65 ℃, the detector temperature was 230 ℃. The FID For the detector, headspace sampling method, water as the solvent, the equilibrium temperature of 70 ℃, the balance of time 45min. Results: The linear range of chloroform was 0.1845 ~ 18.45μg · mL-1 (r = 0.9995). The average recovery was 98.2% and the RSD was 2.2% (n = 6). The lowest detection limit was 36.9 ng · mL-1. Conclusion: The method is sensitive, simple and accurate and can be used to determine the residual amount of trichloromethane in sinomenine hydrochloride.