CESPU, Instituto de Investigação e Formação Avançada em Ciências e Tecnologias da Saúde, Rua Central de Gandra, 1317, 4585-116 Gandra PRD, Portugal; Universidade Católica Portuguesa, CBQF - Centro de Biotecnologia e Química Fina - Laboratório Associado, Escola Superior de Biotecnologia, Rua Diogo Botelho 1327, 4169-005 Porto, Portugal.
REQUIMTE/LAQV, Instituto Superior de Engenharia do Porto, Instituto Politécnico do Porto, Rua Dr. António Bernardino de Almeida, 431, 4200-072 Porto, Portugal.
Environ Pollut. 2020 Apr;259:113927. doi: 10.1016/j.envpol.2020.113927. Epub 2020 Jan 10.
Antibiotics are the most consumed therapeutic classes worldwide and are released to the environment in their original form as well as potentially active metabolites and/or degradation products. Consequences of the occurrence of these compounds in the environment are primarily related to bacterial resistance development. This work presents a validated analytical method based on solid phase extraction (SPE) using HLB cartridges, followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) for quantification of seven different fluoroquinolone antibiotics, namely ciprofloxacin (CPF), enrofloxacin (ENR), lomefloxacin (LOM), norfloxacin (NOR), ofloxacin (OFL), prulifloxacin (PLF) and moxifloxacin (MOX) and its application to detect the target compounds in influents and effluents of wastewater treatment plants (WWTP). Linearity was established through calibration curves in solvent and matrix match using internal calibration method in the range of 50-1300 ng L and all the fluoroquinolones showed good linear fit (r ≥ 0.991). Accuracy ranged between 80.3 and 92.9%, precision was comprised between 7.2 and 14.6%, and 10.7 and 18.1% for intra- and inter-batch determinations, respectively. Method detection and quantification limits ranged from 6.7 to 59.0 ng L and 22.3-196.6 ng L, respectively. Influents and effluents of fifteen WWTPs of North of Portugal were analyzed. OFL was the fluoroquinolone found at the highest concentration, up to 4587.0 ng L and 987.9 ng L, in influent and effluent, respectively. NOR and PLF were not detected.
抗生素是全球使用最多的治疗药物类别，它们以原始形式以及潜在的活性代谢物和/或降解产物的形式被释放到环境中。这些化合物在环境中出现的后果主要与细菌耐药性的发展有关。本工作提出了一种基于固相萃取（SPE）使用 HLB 小柱的经过验证的分析方法，随后进行液相色谱-串联质谱（LC-MS/MS）分析，以定量七种不同的氟喹诺酮类抗生素，即环丙沙星（CPF）、恩诺沙星（ENR）、洛美沙星（LOM）、诺氟沙星（NOR）、氧氟沙星（OFL）、普鲁沙星（PLF）和莫西沙星（MOX），并将其应用于检测污水处理厂（WWTP）进水和出水的目标化合物。通过在溶剂和基质匹配中使用内部校准法，在 50-1300ng L 的范围内建立校准曲线，所有氟喹诺酮类抗生素均表现出良好的线性拟合（r≥0.991）。准确度在 80.3%至 92.9%之间，精密度在 7.2%至 14.6%之间，批内和批间分别为 10.7%至 18.1%。方法检测限和定量限范围分别为 6.7 至 59.0ng L 和 22.3 至 196.6ng L。对葡萄牙北部的 15 个 WWTP 的进水和出水进行了分析。OFL 是在进水和出水中浓度最高的氟喹诺酮类抗生素，分别高达 4587.0ng L 和 987.9ng L。NOR 和 PLF 未检出。
