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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(30m×0.25mm×0.25μm);氢火焰离子化检测器;载气为氮气,流速为0.9mL·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6min,以8℃·min-1的速率升至180℃,保持5min;顶空进样,进样体积为1.0mL。结果:三氯甲烷在9.696～242.4μg(r=0.9994)、甲苯在2.875～71.88μg(r=0.9995),乙醇在82.674～2066.84μg(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 the residues of three organic solvents, chloroform, toluene and ethanol in Sophora alopecuroides. Methods: The capillary gas chromatographic column (30m × 0.25mm × 0.25μm) with DB-WAX polyethylene glycol (PEG-20M) capillary gas chromatography equipped with headspace sampler was used. The flame ionization detector was used. The carrier gas was nitrogen and the flow rate was 0.9mL · min-1. The inlet temperature was 220 ℃ and the detector temperature was 250 ℃. The temperature of the column was raised by programmed temperature, the initial temperature was 60 ℃, kept for 6min, 1 at 180 ° C for 5 min; headspace injection, injection volume 1.0 mL. Results: The linear range of chloroform was 9.696 ~ 242.4μg (r = 0.9994), toluene was 2.875 ~ 71.88μg (r = 0.9995) and ethanol was 82.674 ~ 2066.84μg (r = 0.9993) The average recoveries of toluene and ethanol were 95.9% (RSD = 3.8%), 98.4% (RSD = 4.4%) and 97.6% (RSD = 3.8%), respectively. Conclusion: The method is simple, sensitive, reproducible and accurate. It is suitable for the determination of residual organic solvents in Sophora alopecuroides.