Montemurro Nicola, Orfanioti Anastasia, Manasfi Rayana, Thomaidis Nikolaos S, Pérez Sandra
ENFOCHEM, IDAEA-CSIC, c/Jordi Girona 18-26, 08034 Barcelona (Spain).
Laboratory of Analytical Chemistry, Department of Chemistry, National and Kapodistrian University of Athens, Panepistimiopolis Zographou, 15771 Athens, Greece.
J Chromatogr A. 2020 Nov 8;1631:461566. doi: 10.1016/j.chroma.2020.461566. Epub 2020 Sep 19.
Screening of a large number of chemicals of emerging concern is highly desirable for the control of crops irrigated with reclaimed water since it is considered an alternative water source of great value. This study describes a high resolution mass spectrometry approach for developing methods for quantification in lettuce leaves of 48 different wastewater-borne pollutants (including analgesics and anti-inflammatories, anti-hypertensives, antifungal agents, lipid regulators, psychiatric drugs and stimulants, β-blockers, antibiotics, antimycotics, and sweeteners) frequently found in water resources. In this respect, a simple and fast QuEChERS-based method for the determination of contaminants in lettuce has been developed. During extraction, the use of formic acid was adopted to further improve the results of some problematic compounds (e.g., fenofibrate, furosemide, metronidazole, oxcarbazepine, sulfanilamide). High resolution multiple reaction monitoring (MRM) and SWATH acquisition were compared in term of accuracy, repeatability, sensitivity, linearity and matrix effect. Both methods provided similar recoveries between 80 and 120% in lettuce leaves, although sulfanilamide, ciprofloxacin, and sulfamethazine presenting values of 26.8, 27.8, and 28.4% in MRM and 25, 33.9, and 35% in SWATH, respectively. The effectiveness of a two-step cleanup on analyte recovery was also assessed and matrix effects were also taken into consideration during the method validation. The developed method allows the simultaneous quantitative analysis of 48 compounds (drug residues and metabolites) in lettuce leaves irrigated with treated wastewater for human consumption. Application of the present method to lettuce crops growth in controlled conditions showed the presence of 14 out 48 studied compounds with similar concentrations in both acquisition modes ranging from 3.3 and 1.3 ng g for climbazole (for MRM and SWATH, respectively) to 33.2 and 17.7 ng g for sulfamethazine. Drug residues such as carbamazepine (6.0 and 8.5 ng g ), and its metabolite carbamazepine epoxide (18.1 and 16.5 ng g ), frequently found in wastewater effluents, were also detected.
由于再生水被视为一种极具价值的替代水源，因此对大量新出现的关注化学品进行筛查对于控制用再生水灌溉的作物至关重要。本研究描述了一种高分辨率质谱方法，用于开发在生菜叶中定量48种不同的废水传播污染物（包括镇痛药和抗炎药、抗高血压药、抗真菌剂、脂质调节剂、精神药物和兴奋剂、β受体阻滞剂、抗生素、抗霉菌剂和甜味剂）的方法，这些污染物在水资源中经常被发现。在这方面，已开发出一种基于QuEChERS的简单快速的生菜中污染物测定方法。在提取过程中，采用甲酸来进一步改善一些有问题化合物（如非诺贝特、呋塞米、甲硝唑、奥卡西平、磺胺）的检测结果。在准确性、重复性、灵敏度、线性和基质效应方面对高分辨率多反应监测（MRM）和SWATH采集进行了比较。两种方法在生菜叶中的回收率相似，在80%至120%之间，不过磺胺、环丙沙星和磺胺二甲嘧啶在MRM中的回收率分别为26.8%、27.8%和28.4%，在SWATH中的回收率分别为25%、33.9%和35%。还评估了两步净化对分析物回收率的有效性，并且在方法验证过程中也考虑了基质效应。所开发的方法允许对用处理后供人类消费的废水灌溉的生菜叶中的48种化合物（药物残留和代谢物）进行同时定量分析。将本方法应用于在受控条件下生长的生菜作物，结果表明在48种研究化合物中有14种存在，两种采集模式下的浓度相似，从克霉唑的3.3和1.3 ng/g（分别对应MRM和SWATH）到磺胺二甲嘧啶的33.2和17.7 ng/g。还检测到了废水中经常发现的药物残留，如卡马西平（6.0和8.5 ng/g）及其代谢物卡马西平环氧化物（18.1和16.5 ng/g）。
