离子液体自聚集磁性多壁碳纳米管固相萃取环境水样中的磺胺类药物  

Magnetic Solid Phase Extraction Based on Ionic Liquid Coated Fe_3O_4-Grafted Multi-Walled Carbon Nanotubes for Determination of Sulfonamides in Environmental Water Samples

作　　者：曹小吉[1] 蔡若男[2] 沈凌晓 董云渊 陈林吉 马永萍[1] 叶学敏[1] 刘劲松[3] 莫卫民[1,2] 

机构地区：[1]浙江工业大学分析测试中心,杭州310014 [2]浙江工业大学化学工程学院,杭州310014 [3]浙江省环境监测中心,杭州310012

出　　处：《分析化学》2015年第5期669-674,共6页Chinese Journal of Analytical Chemistry

基　　金：浙江省环保科研计划项目基金(No.2014A011);杭州市环境保护科技项目基金(No.2013HZHB0021);浙江省公益性技术应用研究计划项目基金(No.2014C37077)资助

摘　　要：将1-己基-3-甲基咪唑六氟磷酸([C6MIM][PF6])离子液体自聚集于磁性多壁碳纳米管(Fe3O4@MWCNTs)表面,并将其作为磁性固相吸附剂,建立了同时测定环境水样中磺胺二甲嘧啶、磺胺对甲氧嘧啶、磺胺邻二甲氧嘧啶和磺胺二甲异噁唑4种磺胺类药物的涡旋辅助磁性固相萃取-高效液相色谱法。优化条件为:将20.0 mg[C6MIM][PF6]包覆的Fe3O4@MWCNTs分散于200 m L水样中,涡旋萃取15 min,磁性分离获取磁性吸附剂,3.5 m L 1.0%乙酸铵-甲醇溶液洗脱,洗脱液氮吹至干,300μL甲醇溶解后待下一步高效液相色谱/二极管阵列检测器(HPLC-PDA)分析。4种磺胺类药物在0.375~75.0μg/L范围内与峰面积呈良好的线性关系,其相关系数为0.9985~0.9996,检出限(S/N=3)为0.079~0.099μg/L,3个加标浓度水平的回收率为80.60%~99.99%,日内、日间测定的相对标准偏差分别为1.3%~6.9%和1.2%~2.9%(n=3)。结果表明,本方法简单方便,易于操作,适用于环境水样中痕量磺胺类药物的检测。In combination with high performance liquid chromatography-photodiode array detector （HPLC- PDA）, a vortex-assisted magnetic solid phase extraction method with the 1-hexyl-3-methylimidazolium hexafluorophosphate （ [ C6MIM ] [ PF6 ] ） ionic liquid coated Fe3O4-grafted multi-walled carbon nanotubes （IL- Fe3Q @ MWCNTs ） as the magnetic adsorbent was developed for the determination of four sulfonamides including sulfamethazine, sulfisoxazole, sulfadoxine, and sulfameter in environmental water samples. The optimal conditions for analysis were as follows ： 20.0 mg of IL-Fe3O4 @ MWCNTs was dispersed into 200 mL of water sample under vortex for 15 min. Then, the IL-Fe304@ MWCNTs carrying sulfonamides was separated from the water sample by an external magnetic field. Next, the sulfonamides were eluted from IL-Fe304 @ MWCNTs with 3.5 mL of 1.0% ammonium acetate methanol solution. Finally, the eluent was dried under a mild stream of nitrogen and reconstituted in 300 ~L of methanol for the subsequent HPLC-PDA analysis Under the optimized conditions, an excellent linearity was observed in the range of 0.375-75.0 p^g/L for the four sulfonamides, with the correlation coefficients ranging from 0. 9985 to 0. 9996. The limits of detections （S/N= 3 ） ranged from 0. 079 to 0. 099 lxg/L. The mean recoveries at three spiked levels ranged from 80.60% to 99.99%. The relative standard deviations （RSDs） 6.9% and from 1.2% to 2.9%. （n=3）, respectively. The p of intra-day and inter-day varied from 1.3 % to roposed method was demonstrated to be simple and feasible for the trace analysis of sulfonamides in environmental water samples.

关 键 词：离子液体 磁性多壁碳纳米管 磁性固相萃取 环境水样 磺胺类药物 

分 类 号：X832[环境科学与工程—环境工程] O658.2[理学—分析化学]