CAS Key Laboratory of Coastal Environmental Processes and Ecological Remediation, Shandong Key Laboratory of Coastal Environmental Processes, Research Center for Coastal Environmental Engineering and Technology of Shandong Province, Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai 264003, China.
School of Source and Environment, University of Chinese Academy of Sciences, Beijing 100049, China.
Molecules. 2022 Mar 27;27(7):2160. doi: 10.3390/molecules27072160.
The residues and abuse of antibiotics have seriously endangered ecological balance and human health; meanwhile, antibiotics determination is very difficult because of their low levels and multiple categories in complicated matrices. Appropriate sample pretreatment is usually imperative to enrich (ultra)trace antibiotics and eliminate matrix interference prior to chromatographic analysis. Dispersive liquid-liquid microextraction (DLLME) has become an ideal pretreatment technique owing to its simplicity, effectiveness, low-consumption, etc. In this work, an ultrasonic-assisted DLLME (UA-DLLME) was developed for the simultaneous extraction of seven sulfonamides (SAs) antibiotics in environmental water and seafood samples coupled with HPLC-DAD determination. Several parameters affecting UA-DLLME efficiency were systematically optimized, and consequently the SAs were separated and detected within 14.5 min. The obtained limits of detection (LODs) and limits of quantification (LOQs) ranged from 0.7-7.8 μg/L and 2.4-26.0 μg/L for three water samples (seawater, aquaculture wastewater and lake water) and two seafood samples (pomfrets and shrimps). High recoveries (80.0-116.0%) with low relative standard deviations (0.1-8.1%) were achieved for all the tested samples at three spiked levels. Notably, sulfadimethoxine was found at 24.49 μg/L in one seawater sample. The facile, robust and benign DLLME-HPLC method demonstrated promising perspectives for multiresidue analysis of antibiotics.
抗生素的残留和滥用严重威胁着生态平衡和人类健康；同时，由于抗生素在复杂基质中的浓度低、种类多，其检测非常困难。在色谱分析之前，通常需要适当的样品前处理来富集（超）痕量抗生素并消除基质干扰。分散液液微萃取（DLLME）因其简单、有效、低消耗等优点，已成为一种理想的预处理技术。在这项工作中，开发了一种超声辅助 DLLME（UA-DLLME），用于同时萃取环境水样和海鲜样品中的七种磺胺类（SAs）抗生素，并结合 HPLC-DAD 进行测定。系统优化了影响 UA-DLLME 效率的几个参数，从而在 14.5 分钟内实现了 SAs 的分离和检测。在三种水样（海水、养殖废水和湖水）和两种海鲜样品（鲳鱼和虾）中，获得的检出限（LOD）和定量限（LOQ）范围为 0.7-7.8μg/L 和 2.4-26.0μg/L。所有测试样品在三个加标水平下的回收率均较高（80.0-116.0%），相对标准偏差较低（0.1-8.1%）。值得注意的是，在一份海水中检出磺胺二甲氧嘧啶，浓度为 24.49μg/L。该简便、稳健、良性的 DLLME-HPLC 方法为抗生素多残留分析提供了有前景的思路。
