顶空-GC法检测灯盏花素中大孔树脂残留物的量

Determination of macro-porous resin residua in Breviscapin by headspace-GC

目的：建立灯盏花素中7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HP-INNOWAX毛细管柱（30 m×0.32 mm×0.5μm）;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℃;2%的碳酸钠-25%二甲亚砜溶液为溶解介质,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=0.9938-0.9999,精密度RSDs均小于7.0%,7种溶剂的平均回收率为93.34%~98.39%,其RSDs在0.99-5.10%。结论：该方法操作简便快速,灵敏度高,准确度好,可作为灯盏花素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 7 types of Breviscapins. Methods： Headspace-GC with HP-INNOWAX column （30 m× 0.32 minx 0.5 μm） was used to determine residua in Breviscapin; the column temperature programming was initial temperature 60℃ （kept for 16 rains）, with the increasing rate of 20 ℃/min to 200℃ （kept for 2 mins） ; the injector temperature was 240℃ and FID detector temperature was 300℃ ;solvent media was 2 % sodium carbonate --25% dimethyl sulfoxide （DMSO） and the carrier gas was nitrogen. Results： There was a good linearity in the experimental concentration （r=0. 9938 -0. 9999 ）, the RSDs of precision were all less than 7.0%. The average recoveries of the 7 residua were in the range of 93.34%-98.39%, and their RSDs were 0.99 -5.10%. Conclusion： The method is simple, accurate and sensitive. It can be used for the determination of macro-porous resin residua in Breviscapin.