肝中巴比妥类药物硅藻土固相提取法

The Determination of Barbiturates in Liver by Solid——phase Extraction with Celite

目的：建立一种操作极为简单、快速、去除杂质能力强、提取率高的硅藻土提取肝中巴比妥类药物的方法.方法：肝匀浆用6%高氯酸沉淀蛋白,上清液过硅藻土柱,二氯甲烷洗脱药物,洗脱液挥干用0.45mol/L氢氧化钠溶液溶解,将该溶液等分为两份,再分别制成pH10和pH14水溶液,以pH10溶液为参比,测定pH14溶液的紫外二阶导数光谱进行药物检测.结果：该法提取率在102%—93.4%,检出限均低于0.8μg/g,变异系数小于2.2%,线性范围0.5～5.0μg/mL.

OBJECTIVE： A simple and rapid method for the determination of barbiturates in Liver by solid —phase extraction with celite and UV differential derivative spectrophotometry is presented in this paper. METHOD ：The supermant of homogeneous liver deproteined with 6% perchloric acid were added celite column and elution was effected with dichloromethane. The eluate were evaporated to dry. The residue was redissolved with 0.45 mol/L NaOH solution. The solution was obtained pH10 solution and pill4 solution respectively. The 2nd derivative spectrum of pill4 solutions was measurement with pH10 solution as reference solution. RESULTS ： The detection limite of barbiturates in liver was below 0.8 μg/g. The recoveries of barbiturates are between 102% -93.4% and the relative standard deviation of recoveries are less than 2.2%. The linear range of determination is 0.5 - 5.0 μg/g.