Li Haixia, Jiang Ye, Liu Yan
Department of Analysis, Hebei Medical University, No. 361 Zhongshan East Road, Shijiazhuang City, PR China.
J Chromatogr Sci. 2011 Oct;49(9):676-82. doi: 10.1093/chrsci/49.9.676.
This paper presents a novel and simple cleanup procedure based on hollow fiber liquid-phase microextraction (HF-LPME) for the determination of trace estradiol in environmental. Estradiol was extracted from a 140-mL water sample (the donor phase) into the pores of the hollow fiber wall organic solvent, then into the organic solvent (the acceptor phase) in the lumen of the hollow fiber. Afterwards, the hollow fiber was eluted with methanol to capture estradiol from the acceptor phase. Different experimental parameters, including the organic phase type and its volume, compositions of the donor phases, ionic strength, stirring rate, temperature, and the extraction times were controlled and optimized based on the response of the HPLC instrument. Under the optimized experimental conditions, the proposed method was found to be linear in the concentration of 1-1000 ng/mL for estradiol, and the limit of detection was 0.1 ng/mL. Furthermore, the method provided a good enrichment factor of 300, and repeatability (relative standard deviation = 5.5). Finally, the proposed method was applied for the analysis of real environmental samples.
本文提出了一种基于中空纤维液相微萃取（HF-LPME）的新型简便净化方法，用于测定环境中的痕量雌二醇。雌二醇从140 mL水样（供体相）中被萃取到中空纤维壁有机溶剂的孔隙中，然后进入中空纤维内腔的有机溶剂（受体相）。之后，用甲醇洗脱中空纤维以从受体相中捕获雌二醇。基于高效液相色谱仪的响应，对包括有机相类型及其体积、供体相组成、离子强度、搅拌速率、温度和萃取次数在内的不同实验参数进行了控制和优化。在优化的实验条件下，该方法对雌二醇的浓度在1 - 1000 ng/mL范围内呈线性，检测限为0.1 ng/mL。此外，该方法具有300的良好富集因子和重复性（相对标准偏差 = 5.5）。最后，该方法被应用于实际环境样品的分析。
