论文部分内容阅读
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。
The ionic liquids of 1-hexyl-3-methylimidazolium hexafluorophosphate ([C6MIM] [PF6]) were self-assembled on the surface of magnetic multi-walled carbon nanotubes (Fe3O4 @ MWCNTs) and used as magnetic solid phase adsorbents Simultaneous determination of four sulfonamides, sulfamethazinum, sulfonamidine, sulfamethoxazole and sulfamethazine in environmental water samples by vortex-assisted magnetic solid-phase extraction-high performance liquid chromatography . The optimum conditions were as follows: Fe3O4 @ MWCNTs coated with 20.0 mg [C6MIM] [PF6] were dispersed in 200 m water sample and vortexed for 15 min. Magnetic adsorbent was obtained by magnetic separation. 3.5 m L of 1.0% ammonium acetate-methanol The solution was eluted, the eluent was blown to dryness, and 300 μL of methanol was dissolved for further analysis by High Performance Liquid Chromatography / Diode Array Detector (HPLC-PDA). The four sulfonamides showed a good linear relationship with the peak area in the range of 0.375 ~ 75.0μg / L, the correlation coefficient was 0.9985 ~ 0.9996, the detection limit (S / N = 3) was 0.079 ~ 0.099μg / L, The recoveries of spiked concentration ranged from 80.60% to 99.99%. The relative standard deviations (RSDs) were 1.3% -6.9% and 1.2% -2.9%, respectively (n = 3). The results showed that the method is simple and easy to operate and suitable for the detection of trace sulfonamides in environmental water samples.