Abstract

β-Cyclodextrin modified magnetic microspheres were synthesized and used as an effective adsorbent for the solid-phase extraction of three phenols from water samples. Scanning electron microscopy and Fourier transform infrared spectrometry were used to characterize the adsorbents. The major parameters affecting the extraction and desorption efficiencies, such as adsorbent dosage, extraction time, pH, ionic strength, and eluent type were systematically optimized. Under these conditions, three phenols in water samples were extracted and determined by high performance liquid chromatography (HPLC) with diode array detection (DAD). Limits of detection (LODs) of 0.04–0.34 ng mL⁻¹ and limits of quantification (LOQs) from 0.13 to 1.14 ng mL⁻¹ were achieved with good repeatability (relative standard deviation <7.5%). The developed method was applied for the determination of 2,4-dichlorophenol, 2,4-dinitrophenol and bisphenol A in spiked Yangtze River water, and the recoveries were from 81.0% to 94.9%. The results demonstrated that the combination of magnetic solid-phase extraction (MSPE) with HPLC-DAD is suitable for the determination of trace phenolics in environmental water.

摘要

合成了β-环糊精修饰的磁性微球，并将其用作有效吸附剂，用于固相萃取水样中的三种酚类物质。扫描电子显微镜和傅里叶变换红外光谱用于表征吸附剂。系统优化了影响萃取和解吸效率的主要参数，如吸附剂用量、萃取时间、pH、离子强度和洗脱液类型。在这些条件下，水样中的三种酚类物质通过高效液相色谱 (HPLC) 和二极管阵列检测 (DAD) 进行萃取和测定。检测限 (LOD) 为 0.04–0.34 ng mL ^-1，定量限 (LOQ) 为 0.13 至 1.14 ng mL ^-1实现了良好的重复性（相对标准偏差 <7.5%）。建立的方法用于测定加标长江水中2,4-二氯苯酚、2,4-二硝基苯酚和双酚A，回收率为81.0%~94.9%。结果表明，磁固相萃取（MSPE）与HPLC-DAD相结合适用于环境水中痕量酚类物质的测定。