毛细管气相色谱法检测葛根素衍生物中的残留溶剂

Determination of residual solvents in the derivative of puerarin by capillary gas chromatography

目的:建立葛根素衍生物中二氯甲烷、丙酮、乙酸乙酯、吡啶4种有机溶剂残留量的检测方法。方法:采用气相色谱法,色谱柱为 HP-5(交联5%苯甲基聚硅氧烷)毛细管柱(30m×0.53mm×0.23μm),载气为氮气。检测器温度:250℃;进样口温度:280℃;程序升温:初始温度为36℃,保持0.5min,以每分钟3℃升至70℃,保持1min(延迟时间3min,保持250℃)。分流进样,分流比为1:100,柱前压为37.5kPa。结果:被测物均得到很好的分离,峰面积与浓度呈现良好的线性关系,精密度良好。结论:本方法简单、快捷,且灵敏度高,可用于葛根素衍生物中的残留溶剂检测。

Objective：To establish a method for determination of residual dichloromethane, acetone, ethyl acetate and pyridine simultaneously in derivative of puerarin（4ac）. Methods：The residual solvents in 4ac were separated by HP -5（5% phenyl methyl siloxane） capillary column（30 m×0. 53 mm×0. 23 μm） with an FID detector. The carrier gas was nitrogen. The programmed column temperature was set as follows：maintained at 36 ℃ for 0. 5 min and then raised to 70 ℃ at the rate of 3 ℃ · min^-1 followed by holding for 1 min （ maintained at 250℃ for 3 min of the delay time）. This was followed by split injection ,where the splitting- ratio was 1：100 and the column pressure was 37. 5 kPa. Result-The solvents detected were separated completely. The calibration curve of each solvent showed a good linear relationship with good precision and accuracy. Conclusion：The method is simple, rapid with good sensitivity. It is suitable for the measurement of residual solvents in derivative of puerarin.