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Fe3O4@SiO2@C14mimBF4磁性固相萃取技术用于水中磺胺类药物分析

Determination of sulfonamides in water by Fe3O4@SiO2@C14mimBF4-based magnetic mixed hemimicelles solid phase extraction method

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【作者】 叶学敏董丹琪邵华曹小吉莫卫民

【Author】 YE Xuemin;DONG Danqi;SHAO Hua;CAO Xiaoji;MO Weimin;Research Center of Analysis and Measurement, Zhejiang University of Technology;College of Chemical Engineering, Zhejiang University of Technology;

【机构】 浙江工业大学分析测试中心浙江工业大学化学工程学院

【摘要】 构建了Fe3O4@SiO2@C14mimBF4磁性混合半胶束固相萃取体系,结合超高效液相色谱法,分析检测了环境水体中的痕量磺胺类药物。考察了C14mimBF4浓度、Fe3O4@SiO2用量、离子强度、超声萃取时间等因素对磺胺药物萃取效果的影响。结果表明,在pH值为10的碱性条件下,10 mL水样中加入5 mg Fe3O4@SiO2和最终质量浓度为300μg/mL的C14mimBF4可以实现4种磺胺类化合物(磺胺噻唑、磺胺甲二唑、磺胺苯甲酰、磺胺氯吡嗪)的快速吸附。结合超高效液相色谱法,所建立的方法检出限为1.21~2.25μg/L,水样加标回收率为70%~100%,可用于环境水体中磺胺类药物的痕量分析。与传统的固相萃取方法相比,该方法具有绿色环保(有机溶剂用量少,磁性材料用量少并可重复利用)、简便快速(磁性分离操作简便、分离速度快,避免繁琐的过柱程序)、分析物易洗脱等优点。

【Abstract】 A magnetic mixed hemimicelles solid phase extraction system based on Fe3O4@SiO2@C14mimBF4 was established for determination of trace sulfonamides in water via ultra performance liquid chromatography(UPLC). Factors affecting the extraction efficiencies of sulfonamides, including concentration of C14mimBF4, amount of Fe3O4@SiO2, ionic strength and extraction time, were explored and optimized. The results showed that when pH value was 10, 5 mg of Fe3O4@SiO2 and 300 μg/mL of C14mimBF4 could rapidly adsorb four kinds of sulfonamides(sulfathiazole, sulfamethizole, sulfabenzamide and sulfaclozine) from 10 mL of water. UPLC analysis showed that detection limits of the established method were in the range of 1.21~2.25 μg/L and recoveries were between 70% and 100%, indicating the method is reliable for trace analysis of sulfonamides in water. Compared with traditional solid phase extraction methods, the reported method here exhibits many advantages, such as environmental friendliness(less consumption of organic solvent and magnetic material and repetitive use of magnetic material), simple and fast operation(convenient magnetic separation) and easy elution of analyte.

【基金】 浙江省公益技术应用研究(分析测试)项目(2017C37008)
  • 【文献出处】 浙江工业大学学报 ,Journal of Zhejiang University of Technology , 编辑部邮箱 ,2020年05期
  • 【分类号】O658.2;O657.72;X832
  • 【被引频次】3
  • 【下载频次】240
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