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Screening of fluoroquinolones in environmental waters using disk-based solid-phase extraction combined to microplate fluorimetric determination and LC-MS/MS

机译:基于圆盘的固相萃取结合微孔板荧光测定和LC-MS / MS筛选环境水中的氟喹诺酮类药物

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摘要

Fluoroquinolones are in the order of the day concerning environmental contamination through anthropogenic activities, resulting in increased risk for antibiotic resistance dissemination. In this context, accessible, low-cost analytical methods are required for implementation of comprehensive surveillance and screening schemes. In this work, we propose a down-scaled disk-based solid-phase extraction system from which the eluate can be first screened by miniaturized fluorimetric reading, followed by individual determination of target fluoroquinolones (ciprofloxacin, norfloxacin, and enrofloxacin) by liquid chromatography combined to tandem mass spectrometry. The fluorimetric measurement is based on the intrinsic fluorescence of fluoroquinolones. Disk-based retention was performed after sample acidification (pH 4.0) by mixed-mode cation exchange using polystyrene divinylbenzene sulphonated sorbent. Sample loading was precisely controlled in a dedicated flow system operating at 4.0 mL min(-1). Different eluent compositions were tested, with elution performed by 1.00 mL of methanol-ammonium hydroxide (98:2, v/v), with subsequent reading of eluate in both detectors. Quantification was attained for 2-25 mu g L-1 range, with LOD values at 1 mu g L-1. The proposed approach was successfully applied to estuarine waters from the Douro River, with comparable results to a conventional SPE-LC-MS/MS procedure.
机译:氟喹诺酮类药物涉及人为活动造成的环境污染,因此增加了抗生素耐药性传播的风险。在这种情况下,需要采用低成本的分析方法来实施全面的监视和筛查计划。在这项工作中,我们提出了一种缩小规模的基于磁盘的固相萃取系统,首先可以通过微型荧光读数来筛选洗脱液,然后通过液相色谱法结合测定目标氟喹诺酮类药物(环丙沙星,诺氟沙星和恩诺沙星)。串联质谱。荧光测量基于氟喹诺酮类药物的固有荧光。在样品酸化(pH 4.0)后,使用聚苯乙烯二乙烯基苯磺化吸附剂通过混合模式阳离子交换进行基于圆盘的保留。在运行于4.0 mL min(-1)的专用流动系统中,精确控制了样品的上样量。测试了不同的洗脱液组成,用1.00 mL甲醇-氢氧化铵(98:2,v / v)进行洗脱,随后在两个检测器中读取洗脱液。定量分析范围为2-25μg L-1,LOD值为1μgL-1。所提出的方法已成功地应用于杜罗河的河口水域,其结果与常规SPE-LC-MS / MS方法相当。

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