顶空毛细管气相色谱法测定泽泻醇提取物中的溶剂及树脂残留物

Determination of Solvent and Resin Residues in Alisol Extract by Head-space Capillary Gas Chromatography

建立了顶空毛细管气相色谱法测定泽泻醇提取物中的8种溶剂和树脂残留物,采用Rtx-5型毛细管色谱柱测定乙酸乙酯和正己烷,用Stabilwax-DB毛细管色谱柱测定苯、甲苯、对二甲苯、邻二甲苯、苯乙烯和二乙烯苯。使用FID检测器,以N2为载气,程序升温。8种溶剂分离良好,乙酸乙酯在24.88∽734.7μg、正己烷在2.05∽20.5μg、苯在0.04∽0.80μg、甲苯在0.05∽0.84μg、对二甲苯在0.03∽0.85μg、邻二甲苯在0.04∽0.87μg、苯乙烯在0.03∽0.91μg、二乙烯苯在0.09∽0.91μg范围内线性关系良好。乙酸乙酯和正己烷的回收率为112.02%和91.65%,RSD小于3.45%;其他6种树脂残留的回收率为85.05%∽96.32%,RSD小于5.20%。

A head-space capillary GC method was established for the determination of ethyl acetate, n-hexane and six kinds of resin residues in alisol extract. A Rtx-5 column was used for the determination of ethyl acetate and n-hexane, while a Stabilwax-DB column was used for the determination of benzene, toluene, p-xylene, o-xylene, styrene, and divinylbenzene. FID detector was used with temperature programmed control using nitrogen as the carrier gas. Eight residual solvents were separated completely. The calibration curves for the above eight compounds were linear in the ranges of 2.05 - 20.5μg, 24.88 - 734.7 μg, 0.04 - 0.80 μg, 0.05 - 0.84 μg, 0.03 - 0.85 μg, 0.04 - 0.87μg, 0.03 - 0.91 μg and 0.09 - 0.91 μg, respectively. The recoveries of ethyl acetate and n-hexane were 112.02 % and 91.65 %, with RSDs less than 3.45 %, while the recoveries of the others were 85.05 % - 96.32 %, with RSDs less than 5.20 %.