顶空气相色谱法测定三七叶苷中大孔树脂有机溶剂残留物

Headspace gas chromatographic determination of macro-porous resin residua in leaves saponins of Panax notoginseng

目的:建立三七叶苷中8种大孔树脂有机溶剂残留物的检测方法。方法:采用顶空进样毛细管气相色谱法,色谱柱为INNOWAX 毛细管柱(30 m×0.53 mm×1.0 μm);柱温(程序升温):60℃维持16 min,再以每分钟20℃的升温速率升至200℃,维持2 min;进样口温度:240℃;FID 检测器温度:300℃;25%N,N-二甲基乙酰胺为溶解介质,载气为氮气,测定三七叶苷中正己烷、苯、甲苯、对二甲苯、邻二甲苯、苯乙烯、1,2-二乙基苯及二乙烯苯8种大孔树脂有机溶剂残留量。结果:本法线性关系良好,r=0.9996～0.9999,精密度 RSD 均小于6.0%,8种溶剂的平均回收率为77.4%～101.6%,其 RSD 在3.0%～5.0%。结论:该方法操作简便快速,灵敏度高,准确度好,可作为三七叶苷中大孔树脂有机溶剂残留量的测定方法。

Objective： To establish a method for detecting the residua of macro - porous resin in leaves saponins of Panax notoginseng. Methods： Headspaee GC with HP - INNOWAX column （30 m × 0. 53 mm ×1.0 μm） was used to determine residua in leaves saponins of Panax notoginseng;The column temperature programming was initial tem- perature 60 ℃ （ hold 16 min） ,with the increasing rate of 20 ℃ · min^-1to 200℃ （ hold 2 min） ;The injector temperature was 240℃ and FID detector temperature was 300℃ ;Solvent media was 25% N,N - dimethyl - aeetamide （DMA） and the carrier gas was nitrogen. Results ： There was a good linearity in the experimental concentration （ r = 0. 9996 -0. 9999） ,the RSDs of precision were all less than 6. 0%. The average recoveries of the 8 residua were in the range of 77.4% -101.6%, and their RSDs were 3.0% -5.0%. Conclution： The method is simple, accurate and sensitive. It can be used for the determination of macro - porous resin residua in leaves saponins of Panax notoginseng.