桑枝总生物碱提取物中离子交换树脂残留物的顶空毛细管GC法测定

Determination of Resin Residue in Mulberry Twig Total Alkaloids Extract by Head-Space Capillary GC

建立了顶空毛细管气相色谱法测定桑枝总生物碱提取物中的7种离子交换树脂残留物。采用DB-624弹性石英毛细管色谱柱,测定正已烷、苯、甲基环已烷、甲苯和二乙烯苯,用DB-WAX色谱柱测定二甲苯和苯乙烯,载气为氮气,FID检测器,程序升温,照标准加入法测定。7种溶剂分离良好,苯在0.2～10μg、其它6种溶剂均在2～100μg范围内线性关系良好。回收率为96.6%～101.7%,RSD均小于10%。

A head-space capillary GC method was established for the determination of resin residues in mulberry twig total alkaloids extract. The DB-624 column was used for the determination of n-hexane, benzene, methylcyclohexane, toluene and divinylbenzene, and the DB-WAX column was used for the determination of xylene and styrene, with nitrogen as the carrier gas, FID detector and temperature programmed control. Standard addition method was used. Seven residual solvents were separated completely. The calibration curve for benzene was linear in the range of 0.2 - 10 μg while those for the others were linear in the range of 2 - 100 μg. The recoveries were 96.6% - 101.7% with RSDs less than 10 %.