顶空毛细管气相色谱法测定苦参素中丙酮和乙醇残留量

目的: 建立苦参素中丙酮及乙醇残留量的测定方法。 方法: 采用气相色谱法, 用固定液为聚乙二醇(PEG-20M)的毛细管柱, 载气为氮气, 氢火焰离子化检测器(FID), 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65 ℃, 保持6 min, 然后以15 ℃·min, 顶空进样, 进样体积为1 mL。以水为样品的溶剂。 结果: 丙酮在12.78~127.80 μg·mL^-1的浓度范围内线性关系良好(r=0.9933),乙醇在48.90~489.00 μg·mL^-1的浓度范围内线性关系良好(r=0.9926);丙酮、乙醇的平均回收率(n=9)分别为95.3%,97.4%。结论:本方法准确、可靠,灵敏度高,适用于苦参素中丙酮及乙醇残留量的检测。

Objective: To establish a method for the determination of residual volume of acetone and ethanol in oxymatrine. Method: 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 15 ℃·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 1 mL with headspace sampling.The solvent was water. Results: The calibration curve showed a good linearity with the range of 12.78–127.80 μg·mL^-1 for acetone(r=0.9933)and with the range of 48.90–489.00 μg·mL^-1 for ethanol(r=0.9926).The average recoveries(n=9)of acetone and ethanol were 95.3% and 97.4%,respectively. Conclusion: The method is accurate,reliable and sensitive for the determination of the residual volume of acetone and ethanol in oxymatrine.