流动气体捕集法测定贯叶连翘提取物中大孔树脂残留物

Determination of Macro-porous Resin Residue in Herba Hyperici Perforat Extraction by Flow Gas Capture Method

采用流动气体捕集法 ,通过GC/MS法测定贯叶连翘提取物中大孔树脂残留物 苯、甲苯和二乙烯苯。与萃取、回流和顶空进样三种处理方式比较 ,自制的流动气体捕集装置能够很好地收集待测成分并有效地消除干扰。整体 (流动气体捕集法处理 +含量测定 )检出限和回收率 (苯 :0 .3ng/g ,99.0 % ;甲苯 :0 .8ng/g ,99 5 % ;二乙烯苯 :0 .5ng/g ,99 2 % ) ,与GC/MS法所得结果 (苯 :0 .1ng/g ,99.2 % ;甲苯 :0 .2ng/g ,99.4 % ;二乙烯苯 :0 .1ng/g ,99.2 % )无显著差别 ,说明该法有较低的检出限和良好的回收率。经其他 3种方式处理后 ,检出限变差回收率下降。结果证明流动气体捕集法适于中药提取物中大孔树脂残留物的定量检测。

By using gas chromatogaphy/mass specrometry (GC/MS),the flow gas capture method was studied in the assay of macro-porous resin D101 residue, benzene, toluene and diviylbenzene, in Herba Hyperici Perforat Extract. Comparing with 3 other methods of preparation (extraction, reflux and headspace). It shows that the flow gas capture is the best method due to the low limit of detection (LOD) and high recovery. The total (preparation plus analysis) LOD is 0.3, 0.8 and 0.5 ng/g, the total recovery is 99.0%, 99.5%, 99 2% for benzene, toluene and diviylbenzene respectively, without significant difference from those of other GC/MS determination method (with the LOD 0.1, 0.2, 0.1 ng/g and the recovery 99.2%, 99.4%, 99.2% for benzene, toluene and diviylbenzene, respectively) was observed.