顶空气相色谱法测定苦豆子总碱中残留溶剂

目的: 建立苦豆子总碱中三氯甲烷、甲苯、乙醇3种有机溶剂残留量的测定方法。 方法: 使用配置顶空进样器的毛细管气相色谱仪,采用DB-WAX聚乙二醇(PEG－20M))毛细管气相色谱柱(30 m×0.25 mm×0.25 μm);氢火焰离子化检测器;载气为氮气,流速为0.9 mL·min^-1;进样口温度为220 ℃,检测器温度为250 ℃;柱温采用程序升温,初始温度为60 ℃,保持6 min,以8 ℃·min^-1的速率升至180 ℃,保持5 min;顶空进样,进样体积为1.0 mL。 结果: 三氯甲烷在9.696~242.4 μg(r=0.9994)、甲苯在2.875~71.88 μg(r=0.9995),乙醇在82.674~2066.84 μg(r=0.9993)范围内呈良好的线性关系;三氯甲烷、甲苯和乙醇的平均回收率分别为95.9%(RSD=3.8%),98.4%(RSD=4.4%),97.6%(RSD=3.8%)。 结论: 本方法简便、灵敏度高、重复性好,结果准确,适合苦豆子总碱中有机溶剂残留量的测定。

Objective: To establish a method for the determination of residual volume of trichloromethane toluene and ethanol in total alkali of Sophora alopecuroides L. Methods: The residual organic solvents were determined by GC with capillary column(PEG-20M)with FID detector and nitrogen as the carrier gas.The temperature of the injection port was maintaining at 220℃ and that of the detector at 250℃。The initial column temperature was 65℃,maintaining it for 6 min,then raising the temperature to 180℃ at a rate of 8℃·min^-1 and maintaining it at 180℃ for 5 min.The flow rate of N₂ was 0.9 mL·min^-1 and the injection volume was 1mL with headspace sampling.The solvent was water. Results: The calibration curve showed a good linearity with the range of 9.696-242.4 μg·mL^-1 for trichloromethane(r=0.9994),with the range of 2.875-71.88 4 μg·mL^-1 for toluene (r=0.9995)and with the range of 82.674-2066.84 μg·mL^-1 for ethanol(r=0.9993).The average recoveries(n=9)of trichloromethane,toluene and ethanol were 95.9%(RSD=3.8%),98.4%(RSD=4.4%)and 97.6%(RSD=3.8%). Conclusion :The method is accurate,reliable and sensitive for the determination of the residual volume of trichloromethane toluene and ethanol in total alkaloid of Sophora alopecuroides L.