Jiangsu Wuxi Environmental Monitoring Center, Wuxi, PR China; State Key Laboratory of Food Science and Technology, Jiangsu Key Laboratory of Anaerobic Biotechnology, School of Environmental and Civil Engineering, Jiangnan University, Wuxi, PR China.
Jiangsu Wuxi Environmental Monitoring Center, Wuxi, PR China; State Key Laboratory of Food Science and Technology, Jiangsu Key Laboratory of Anaerobic Biotechnology, School of Environmental and Civil Engineering, Jiangnan University, Wuxi, PR China.
J Chromatogr A. 2022 Aug 16;1677:463304. doi: 10.1016/j.chroma.2022.463304. Epub 2022 Jul 3.
A method was developed for the determination of 33 antibiotics belonging to 4 different antibiotic groups, including sulfonamides (16), fluoroquinolones (12), macrolides (1), and tetracyclines (4) in water samples using on-line solid-phase extraction-ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (on-line SPE-UPLC-MS/MS). The enrichment and analysis conditions were optimized for the determination of trace concentrations (nanogram per liter). Aliquots of the water samples (5 mL) were filtered through a membrane and enriched on an on-line polymeric column with hydrophilic-lipophilic balance (HLB). The analyte was eluted by the mobile phase during on-line SPE and separated on an Acquity BEH130 column, detected by tandem mass spectrometry, and quantified using an external standard method. The optimization of the analytical methods was discussed, which included optimization of pH of the sample, filtration membrane, NaEDTA, chromatographic column, formic acid and aqueous ammonia in mobile phase. The detection limit for all test compounds by this method was in the range of 0.2-1.5 ng/L, with recoveries of 76.6-118%. The precision of the method, as indicated by the relative standard deviation, was 2.4-7.9%. Results of analysis of surface water samples demonstrated the ability of the proposed method to analyze ultra-trace levels of antibiotics, without the need for complex manual pretreatment.
建立了一种同时测定水中 4 类 33 种抗生素（磺胺类 16 种、氟喹诺酮类 12 种、大环内酯类 1 种、四环素类 4 种）的在线固相萃取-超高效液相色谱-电喷雾串联质谱（on-line SPE-UPLC-MS/MS）分析方法。优化了痕量（纳克/升）浓度条件下的富集和分析条件。取 5 mL 水样经膜过滤后，用亲水-亲脂平衡（HLB）在线聚合物柱富集。在线 SPE 过程中用流动相洗脱目标物，在 Acquity BEH130 柱上分离，串联质谱检测，外标法定量。讨论了分析方法的优化，包括样品 pH 值、滤膜、NaEDTA、色谱柱、流动相中甲酸和氨水的优化。该方法对所有测试化合物的检测限在 0.2-1.5 ng/L 范围内，回收率为 76.6-118%。方法的精密度（相对标准偏差）为 2.4-7.9%。对地表水样品的分析结果表明，该方法无需复杂的手动预处理，即可分析超痕量水平的抗生素。
