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Extraction of natural estrogens in environmental waters by dispersive multiwalled carbon nanotube-based agitation-assisted adsorption and ultrasound-assisted desorption

机译:基于分散多壁碳纳米管的搅拌辅助吸附和超声辅助解吸提取环境水中的天然雌激素

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摘要

A dispersive multiwalled carbon nanotube (MWCNT) based agitation-assisted adsorption and ultrasound-assisted desorption method has been developed for extracting natural estrogenic steroids in environmental waters prior to high performance liquid chromatography-diode array detection (HPLC-DAD) analysis. With the aid of agitation, the trace estrogens in bulk aqueous solution were adsorbed onto milligrams of dispersive MWCNTs: After filtration, the estrogens enriched on MWCNT nanoparticles were quickly desorbed into milliliters of organic solvent in an ultrasonic bath. Finally, the analytes in the organic solvent were directly determined by HPLC-DAD. The stability examination of estrogens under the tested ultrasonic irradiation was performed and the results indicated that the estrogens were stable during the extraction process. Several parameters that could influence the extraction efficiency, such as type and volume of desorption solvent, consumed amount of MWCNTs, pH and ionic strength of sample solution, agitation-assisted adsorption and ultrasound-assisted desorption time, were examined. Under the optimized conditions, the recoveries for three analytes in spiked samples were over 82%. The detection limits were 0.076 ng mL~(-1) for estrone, 0.049 ng mL~(-1) for 17p-estradiol, and 0.057 ng mL~(-1) for estriol, respectively, while the relative standard deviations were less than 9% (at the 20 ng mL~(-1) estrogen level for 10 runs).
机译:已经开发了一种基于分散多壁碳纳米管(MWCNT)的搅拌辅助吸附和超声辅助解吸方法,用于在高效液相色谱-二极管阵列检测(HPLC-DAD)分析之前提取环境水中的天然雌激素类固醇。借助搅拌,将散装水溶液中的痕量雌激素吸附到毫克分散的MWCNT上:过滤后,富集在MWCNT纳米颗粒上的雌激素在超声浴中迅速解吸到毫升有机溶剂中。最后,通过HPLC-DAD直接测定有机溶剂中的分析物。进行了超声波辐射下雌激素的稳定性检查,结果表明在提取过程中雌激素是稳定的。研究了影响萃取效率的几个参数,如脱附溶剂的类型和体积,多壁碳纳米管的消耗量,样品溶液的pH和离子强度,搅拌辅助吸附和超声辅助脱附时间。在优化的条件下,加标样品中三种分析物的回收率均超过82%。雌酮的检出限分别为0.076 ng mL〜(-1),17p-雌二醇的检出限为0.049 ng mL〜(-1),雌三醇的检出限分别为0.057 ng mL〜(-1),相对标准偏差小于9%(在20 ng mL〜(-1)的雌激素水平下运行10次)。

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