分析型超临界流体萃取的应用研究  

Applications of Supercritical Fluid Extraction of Samples in Analytical Chemistry

作　　者：王清海[1] 陈儒[1] 朱道乾[1] 周良模[1] 

机构地区：[1]中国科学院大连化学物理研究所

出　　处：《色谱》1998年第4期344-346,共3页Chinese Journal of Chromatography

摘　　要：设计安装了一台超临界流体萃取（ＳＦＥ）装置。以二氧化碳为萃取剂，采用带泵头冷冻的往复泵能满足１０μＬ／ｍｉｎ～５ｍＬ／ｍｉｎ流速和２５ＭＰａ工作压力的要求，最高工作压力可达３５ＭＰａ。不锈钢萃取池体积为０．５ｍＬ和１．０ｍＬ两种规格，萃取样品的收集是用溶剂（己烷）吸收的。实验中主要进行了中药蛇床子中有效成分欧前胡素的萃取研究，对影响欧前胡素回收率的重要因素如温度、压力、密度、萃取时间及萃取改性剂等进行了考察。对萃取产物进行了ＨＰＬＣ分析，结果表明，蛇床子中有效成分欧前胡素经４０ｍｉｎＳＦＥ的回收率，可相当于经典溶剂法萃取７２ｈ的结果。A supercritical fluid extraction (SFE) system was assembled and used to extract imperatorine from the Cnidium Monnieri cusson (a traditional Chinese medicine). Carbon dioxide was used as the extraction solvent, The volumes of the extractors were in two sizes,0 5mL and 1 0mL. The pump with the head cooling used in this system is satisfactory. The extraction conditions were: 10μL/min 5mL/min flow rate and 25MPa working pressure. The highest working pressure at a short period was up to 35MPa. The SFE operating factors (temperature, pressure, density, time and the modifiers) affecting the recovery of imperatorine were investigated where the imperatorine was used to evaluate the extraction efficiency of the SFE system. The recovery of imperatorine is somewhat decreased with increasing temperature but increased with raising pressure, as well as with increasing density of carbon dioxide. The recovery of imperatorine may be improved dramatically when the pressure is over 25MPa. Three modifiers, acetic acid, methanol and hexane were tested. The recovery is higher by adding methanol than by adding hexane or acetic acid. SFE product was analyzed by HPLC and compared with that of conventional solvent extraction. The results showed that the recovery of imperatorine by SFE for 40min is probably the same as that by conventional solvent extraction for 72 hours.

关 键 词：超临界流体萃取 二氧化碳 中药 蛇床子 欧前胡素 

分 类 号：O652.62[理学—分析化学] R282.71[理学—化学]