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目的建立水飞蓟素中3种有机溶剂残留量的顶空气相色谱测定方法。方法以HP-5弹性石英毛细管柱(30m×0.53mm,i.d,5.0μm),载气为氮气,采用氢火焰离子化检测器,进样口温度为180℃,检测器温度为250℃,柱温采用程序升温(40℃,保持6min,以15℃/min升至180℃,保持3min),流速为1.7mL/min,分流比为1∶10,采用甲醇作为内标物质,分别配制对照溶液及样品溶液,以二甲基亚砜为溶剂,采取顶空进样(85℃预热20min),进样体积为1.0mL。结果乙醇、丙酮、乙酸乙酯在各自对应的浓度范围内,其峰面积与浓度呈良好的线性关系,加样回收率(n=5)分别为98.30%(RSD=0.82%)、97.62%(RSD=1.1%)、96.89%(RSD=1.4%),精密度良好。结论本文所建立的气相色谱条件可同时测定水飞蓟素中的乙醇、丙酮、乙酸乙酯的含量,方法简单可靠。
Objective To establish a method for the determination of three organic solvents in silymarin by headspace gas chromatography. Methods HP-5 elastic quartz capillary column (30m × 0.53mm, id, 5.0μm) was used. The carrier gas was nitrogen. The flame ionization detector was used. The inlet temperature was 180 ℃ and the detector temperature was 250 ℃. Temperature was programmed temperature (40 ℃, hold 6min, 15 ℃ / min rose to 180 ℃, hold 3min), flow rate of 1.7mL / min, split ratio 1:10, the use of methanol as the internal standard substance, respectively, the preparation of the control solution And the sample solution to dimethyl sulfoxide as solvent, take a headspace injection (85 ℃ preheated 20min), the injection volume of 1.0mL. Results The peak area and concentration of ethanol, acetone and ethyl acetate showed a good linear relationship with the recoveries (n = 5) of 98.30% (RSD = 0.82%) and 97.62% (n = RSD = 1.1%), 96.89% (RSD = 1.4%) with good precision. Conclusion The gas chromatography conditions established in this paper can simultaneously determine the contents of ethanol, acetone and ethyl acetate in silymarin. The method is simple and reliable.