Shi Zhihong, Zhu Xiaomin, Zhang Hongyi
College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China.
J Pharm Biomed Anal. 2007 Aug 15;44(4):867-73. doi: 10.1016/j.jpba.2007.03.035. Epub 2007 Apr 6.
In this paper, a micelle-mediated extraction and cloud point preconcentration method was developed for the determination of less hydrophobic compounds aesculin and aesculetin in Cortex fraxini by HPLC. Non-ionic surfactant oligoethylene glycol monoalkyl ether (Genapol X-080) was employed as the extraction solvent. Various experimental conditions were investigated to optimize the extraction process. Under optimum conditions, i.e. 5% Genapol X-080 (w/v), pH 1.0, liquid/solid ratio of 400:1 (ml/g), ultrasonic-assisted extraction for 30 min, the extraction yield reached the highest value. For the preconcentration of aesculin and aesculetin by cloud point extraction (CPE), the solution was incubated in a thermostatic water bath at 55 degrees C for 30 min, and 20% NaCl (w/v) was added to the solution to facilitate the phase separation and increase the preconcentration factor during the CPE process. Compared with methanol, which was used in Chinese Pharmacopoeia (2005 edition) for the extraction of C. fraxini, the extraction efficiency of 5% Genapol X-080 reached higher value.
本文建立了一种胶束介导萃取和浊点预富集方法,用于高效液相色谱法测定秦皮中疏水性较弱的化合物七叶苷和七叶内酯。采用非离子表面活性剂低聚乙二醇单烷基醚(Genapol X - 080)作为萃取溶剂。研究了各种实验条件以优化萃取过程。在最佳条件下,即5% Genapol X - 080(w/v)、pH 1.0、液固比400:1(ml/g)、超声辅助萃取30 min时,萃取率达到最高值。对于通过浊点萃取(CPE)对七叶苷和七叶内酯进行预富集,将溶液在55℃的恒温水浴中孵育30 min,并向溶液中加入20% NaCl(w/v)以促进相分离并提高CPE过程中的预富集因子。与《中国药典》(2005年版)中用于秦皮萃取的甲醇相比,5% Genapol X - 080的萃取效率更高。