薄膜梯度扩散(DGT)-UPLC-MS/MS法测量地下水中26种抗生素

近年来地下水中抗生素污染持续受到关注. 由于抗生素含量一般为痕量级, 对地下水样中抗生素的采样提取检测提出了很高的要求. 利用薄膜梯度扩散法建立了原位富集地下水中抗生素的采样方法, 成功富集了磺胺类、喹诺酮类、四环素类、大环内酯类等抗生素; 同时, 应用超高效液相三重串联质谱法建立了分析地下水中26种典型抗生素的检测方法, 优化了提取条件. 结果表明, 整套采样及测试方法对地下水中抗生素分析具有较好的富集效果和检测灵敏度. 地下水原位富集采样时间20~30 d为宜, 26种抗生素的仪器检出限为0.002~0.074 ng/L, 平均回收率为47.7%~94.6%, 精密度4.45%~10.84%. 薄膜梯度扩散法原位富集采集地下水中抗生素的采样方式操作简单, 结合三重串联四级杆液相色谱能够实现地下水中抗生素的痕量分析.

DETERMINATION OF 26 ANTIBIOTICS IN GROUNDWATER BY DIFFUSIVE GRADIENTS IN THIN FILMS TECHNIQUE COMBINED WITH UPLC-MS/MS

Antibiotic contamination in groundwater has been concerned in recent years. Due to the trace-level concentration of antibiotics, the processes for sampling, extraction and detection are highly required. The diffusive gradients in thin films (DGT) is used to establish the in situ enrichment sampling method of antibiotics in groundwater, and antibiotics such as sulfonamides, quinolones, tetracyclines and macrolides are successfully enriched. Besides, the ultra-high performance liquid chromatogrphy tandem mass spectrometry (UPLC-MS/MS) is applied for the detection method of 26 typical antibiotics in groundwater, with optimized extraction conditions. The results show that the sampling and testing methods have good enrichment effect and detection sensitivity for analysis of antibiotics in groundwater. The appropriate in-situ enrichment sampling time of groundwater is 20-30 d, with instrument detection limit of 0.002-0.074 ng/L, average recovery of 47.7%-94.6% and precision of 4.45%-10.84%. The in situ enrichment sampling method of antibiotics in groundwater through DGT is simple and can be used for trace analysis of antibiotics in groundwater combined with UPLC-MS/MS.