摘要
采用顶空进样毛细管气相色谱法,色谱柱为HP-INNOWAX毛细管柱(30m×0.32mm×0.5μm);柱温(程序升温):60℃维持16min,再以每分钟20℃的升温速率升至200℃,维持2min;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,测定三七总皂苷中正己烷、苯、甲苯、对二甲苯、邻二甲苯、苯乙烯、1,2-二乙基苯7种大孔树脂有机溶剂残留量.结果本法线性关系良好,r=0.9957～0.9999,精密度RSDs均小于7.0%,7种溶剂的平均回收率为95.59%～101.34%,其RSDs在1.10～1.91%.该方法操作简便快速,灵敏度高,准确度好,可作为三七总皂苷中大孔树脂有机溶剂残留量的测定方法.
Headspace -GC with HP-INNOWAX column （30m×0.32mm×0.5μm） was used to determine residua in Panax notoginseng saponions; The column temperature programming was initial temperature 60℃ （hold 16min）, with the increasing rate of 20℃ min^-1 to 200℃ （hold 2 min） ;The injector temperature was 240℃ and FID detector temperature was 300℃ ;Solvent media was 25% N,N - dimethyl - acetamide （DMA） and the carrier gas was nitrogen. There was a good linearity in the experimental concentration （ r = 0. 9957 - 0. 9999 ）, the RSDs of precision were all less than 7.0%. The average recoveries of the 7 residua were in the range of 95.59% 101.34% ,and their RSDs were 1.10 -1.91% . The method is simple,accurate and sensitive. It can be used for the determination of macro-porous resin residua in Panax notoginseng saponions.
出处
《商丘师范学院学报》
CAS
2009年第6期71-73,共3页
Journal of Shangqiu Normal University
基金
云南省应用基础研究项目(2007C258M)
国家科技支撑计划项目(2006BA114B03-2)
关键词
大孔树脂残留物
三七总皂苷
顶空气相色谱法
macro--porous resin residues
headspace GC
Panax notoginseng saponions
