磁性ODS微粒的制备及其对污水中激素的富集应用

Preparation of Magnetic Octadecylsilyl Microparticles and Their Application for the Extraction of Hormones in Sewage

以甲苯为分散体系，以十八烷基三甲氧基硅烷为Fe3O4磁性粒子表面修饰剂，通过硅烷化法制备了分散性良好、表面带有—（CH2）17CH3活性官能团、平均几何粒径7．5μm、比表面积26．7m^2／g的磁性十八烷基（ODS）微粒。该磁粒经活化后可吸附疏水性的物质，用甲醇将所吸附的物质洗脱下来进行检测分析，即可以应用于环境中痕量疏水性物质的检测。该文将所制备的磁性ODS微粒应用于污水中雌性激素的提取富集，平均提取效率为23．0％～91．6％。处理后的样品用扫集胶束电动色谱技术（Sweeping MEKC）进行检测。应用该法成功地检测了污水中的痕量雌酮和雌三醇，其质量浓度分别为（5．60±0．08）μg/L和（5．24±0．06）μg/L。研究结果表明，将磁粒提取富集技术与扫集胶束电动色谱技术相结合可以提高污水中痕量物质的检测灵敏度，并减少样品基体中其它物质的干扰。

Magnetic octadecylsilyl （ODS） microparticles were prepared by the silanization method using octadecyl trimethoxysilane as the surface modification reagent for magnetic Fe3O4 particles in toluene medium. Well dispersed ODS microparticles with an average diameter of 7.5 μm and a specific area of 26.7 m^2/g and with a functional group （-（ CH2 ） 17CH3 ） on their surface were obtained. The activated mieroparticles were liable to adsorb hydrophobie substances which could then be eluted easily by methanol and be detected. A method was thus developed for the determination of estrogens - pollutant in environmental water using magnetic ODS mieroparticles to extract trace amount of estrogens and sweeping micellar electrokinetic chromatography for detection. The average extraction efficiencies of estrogens were in the range of 23.0% - 91.6% . The method was successfully applied to the determination of trace amount of estrone and estriol in sewage and their content was （ 5.60 ± 0. 08） μg/L（estrone） , （5.24 ±0. 06） μg/L（estriol） , respectively. The proposed method is sensitive and can eliminate the interferents from the sample matrix.