CAS Key Laboratory of Coastal Environmental Processes and Ecological Remediation, Research Center for Coastal Environmental Engineering and Technology, Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai 264003, China.
School of Pharmacy, Collaborative Innovation Center of Advanced Drug Delivery System and Biotech Drugs in Universities of Shandong, Key Laboratory of Molecular Pharmacology and Drug Evaluation (Yantai University), Ministry of Education, Yantai University, Yantai 264005, China.
Analyst. 2020 Mar 2;145(5):1825-1832. doi: 10.1039/c9an02127b.
A twin enrichment method based on offline dispersive liquid-liquid microextraction (DLLME) coupled with online field-amplified sample injection (FASI) was developed for the simultaneous determination of four sulfonamide (SA) antibiotics, including sulfamethazine (SMZ), sulfamerazine (SMR), sulfadizine (SDZ) and sulfacetamide (SFA), in different environmental waters, followed by capillary electrophoresis (CE). Various parameters that affected the separation performance of CE and the enrichment efficiencies of DLLME and FASI were optimized in detail, and excellent CE separation was attained within 6 min. The DLLME-FASI-CE offered high sensitivity enrichment factors of 206, 166, 185 and 150 for SMZ, SMR, SDZ and SFA, respectively. Highly sensitive detection was realized with low limits of detection (LODs), which ranged from 2.0-23.0, 2.2-26.0 and 4.3-63.0 ng mL-1 in tap water, lake water and seawater, respectively, as well as limits of quantification (LOQs) within 6.0-63.0, 7.4-96.0 and 14.0-201.0 ng mL-1, respectively. Satisfactory recoveries in the range of 91-108% were obtained with the three spiked environmental water samples, and the relative standard deviations were from 1.09-7.45%. The simple effective twin enrichment method provided promising perspective for CE determination of SAs in complicated aqueous matrices, with rapidity, sensitivity, and accuracy.
基于离线分散液相微萃取（DLLME）与在线场放大样品进样（FASI）的双重富集方法，建立了同时测定不同环境水样中四种磺胺类（SA）抗生素磺胺甲噁唑（SMZ）、磺胺间甲氧嘧啶（SMR）、磺胺地嗪（SDZ）和磺胺噻唑（SFA）的方法，该方法结合了毛细管电泳（CE）。详细优化了影响 CE 分离性能和 DLLME 和 FASI 富集效率的各种参数，并在 6 分钟内实现了优异的 CE 分离。DLLME-FASI-CE 分别为 SMZ、SMR、SDZ 和 SFA 提供了 206、166、185 和 150 的高灵敏度富集因子。在自来水中，检测限（LOD）的范围为 2.0-23.0 ng mL-1，在湖水和海水中，检测限（LOD）的范围分别为 2.2-26.0 和 4.3-63.0 ng mL-1，在自来水中，定量限（LOQ）的范围为 6.0-63.0 ng mL-1，在湖水和海水中，定量限（LOQ）的范围分别为 7.4-96.0 和 14.0-201.0 ng mL-1，实现了高灵敏度检测。在三种加标环境水样中，回收率在 91-108%范围内，相对标准偏差（RSD）为 1.09-7.45%。该简单有效的双重富集方法为 CE 测定复杂水基质中的 SA 提供了有前景的方法，具有快速、灵敏和准确的特点。
