固相萃取-液相色谱法测定烟草中蛇床子素残留量

SPE-LC Determination of Residual Amounts of Osthol in Tobaccos

采用固相萃取-液相色谱法测定烟草中蛇床子素的残留量。样品用50%(体积分数)甲醇溶液提取,通过液液萃取和固相萃取净化后,采用快速液相-二极管阵列检测器进行定量检测,并利用四级杆-串联飞行时间质谱进行定性确证。蛇床子素的质量浓度在0.25~50.0mg·L^(-1)范围内与其峰面积呈线性关系,检出限(3S/N)为0.016mg·kg^(-1)。以空白样品为基体进行加标回收试验,回收率在91.5%~95.5%之间,测定值的日内相对标准偏差(n=5)在3.1%~4.3%之间。

SPE-LC was applied to the determination of residual amounts of osthol in tobaccos. The tobacco sample was extracted with 50% （φ） methanol solution, followed by purification with liquid-liquid extraction and solid phase extraction, and quantification with RRLC-DAD and identification with Q-TOE Linear relationship between values of peak area and mass concentration of osthol was kept in the range of 0. 25-50. 0 mg · L- 1, with detection limit （3S/N） of 0. 016 mg · kg -1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 91.5%--5.5%, with intraday RSD＇s （n=5） in the range of 3.1 %- 4.3 % .