气相色谱法测定葛根和淫羊藿总黄酮提取物中大孔树脂有机残留物

Determination of Macroporous Resin Organic Residues in Total Flavonoids Extracts of Pueraria lobata and Epimedium grandiflorum by Gas Chromatography

目的:建立葛根和淫羊藿总黄酮提取物中大孔吸附树脂7种有机残留物的含量测定方法。方法:采用气相色谱法,DB-1毛细管柱(柱长为60 m,内径为0.25 mm,膜厚度为1.0μm),柱温为程序升温,起始温度为40℃,再以4℃/min升温至175℃,保持12 min,用氢火焰离子化检测器检测,检测器温度250℃,进样口温度200℃;载气为氮气,流速为0.8 mL/min,分流比为20∶1,顶空进样,顶空瓶平衡温度为90℃,平衡时间为50 min。结果:7种有机溶剂残留物的峰面积与浓度呈良好线性关系,正己烷、苯、甲苯、二甲苯、苯乙烯、二乙烯苯、1,2-二乙基苯的平均回收率分别为101%、90%、87%、85%、84%、76%、79%。结论:该方法测定准确度高、精密度重复性好。

Objective:To establish a method for the determination of 7 kinds of organic residues in the total flavone extracts of radix puerariae and epimedium by macroporous adsorption resin.Method:Gas chromatography was used.DB-1 capillary column(column length:60 m,inner diameter:0.25 mm,membrane thickness:1.0 μm);The column temperature is programmed,the initial temperature is 40 ℃,and then the temperature is increased to 175 ℃ at 4 ℃/min per minute for 12 min The detector temperature is 250 ℃,which is detected by hydrogen flame ionization detector;Injection port temperature 200 ℃;The carrier gas is nitrogen,and the flow rate is 0.8mL/min.The split ratio is 20∶1.For headspace injection,the equilibrium temperature of the headspace bottle is 90 ℃ and the equilibrium time is 50 min.Results:There is a good linear relationship between the peak areas and concentrations of the residues of seven organic solvents.The average recoveries of n-hexane,benzene,toluene,xylene,styrene,divinylbenzene,1,2-diethylbenzene are 101%,90%,87%,85%,84%,76%,79%,respectively.Conclusion:The method has high accuracy and repeatability.