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采用基于快速、简易、廉价、有效、耐用和安全的提取方法和液相色谱-质谱联用技术,快速灵敏地测定废水中新出现的关注污染物。

Application of a fast and sensitive method for the determination of contaminants of emerging concern in wastewater using a quick, easy, cheap, effective, rugged and safe-based extraction and liquid chromatography coupled to mass spectrometry.

机构信息

CIESOL (Solar Energy Research Center), Joint Centre University of Almeria-CIEMAT, Carretera de Sacramento s/n, Almeria 04120, Spain.

CIESOL (Solar Energy Research Center), Joint Centre University of Almeria-CIEMAT, Carretera de Sacramento s/n, Almeria 04120, Spain; Department of Chemistry and Physics, University of Almeria, Carretera de Sacramento s/n, Almeria 04120, Spain.

出版信息

J Chromatogr A. 2021 Sep 13;1653:462396. doi: 10.1016/j.chroma.2021.462396. Epub 2021 Jul 9.

Abstract

The inefficiency of wastewater treatment plants (WWTPs) to remove contaminants of emerging concern (CECs) leads to their continuous release to the environment. Consequently, CECs are present at low concentrations in the treated wastewater (TWW), producing unpredicted and unwanted effects on living organisms as they are discharged into water receiving bodies. This work presents a fast and reliable method for the determination of CECs in TWW based on the innovative application of a QuEChERS (quick, easy, cheap, effective, rugged and safe) method for water extraction and determination by sensitive liquid chromatography coupled to quadrupole-linear ion trap tandem mass spectrometry (LC-QqLIT-MS/MS). The scope of the proposed QuEChERS-based method allows the monitoring of 107 CECs, including pharmaceuticals (58), antibiotics (16) and pesticides (33). The proposed method was successfully validated in urban TWW at two concentration levels (50 and 500 ng L) and it is a feasible alternative to conventional and time-consuming solid-phase extraction (SPE) methodologies. 89% of the CECs presented mean recovery values in the 70-120% range with relative standard deviations (RSDs) always < 20% (intra and inter-day precision), and limits of quantification (LOQs) in the range 5-500 ng L (89% of the compounds showed a LOQ ≤ 50 ng L). The applicability of the method was demonstrated by the analysis of urban TWW samples (7 sampling events). In total, 35 CECs (23 pharmaceuticals, 2 antibiotics and 10 pesticides) were detected in the monitored samples with concentrations ranging from 5 to 677 ng L.

摘要

污水处理厂(WWTP)去除新兴关注污染物(CECs)的效率低下导致它们持续释放到环境中。因此,CECs 在经过处理的废水中(TWW)以低浓度存在,当它们排放到受纳水体中时,会对生物体产生不可预测和不需要的影响。本工作提出了一种快速可靠的方法,用于基于 QuEChERS(快速、简便、廉价、有效、坚固和安全)方法的创新应用,从 TWW 中提取和测定 CECs,通过灵敏的液相色谱与四极线性离子阱串联质谱(LC-QqLIT-MS/MS)。所提出的 QuEChERS 方法的范围允许监测 107 种 CECs,包括药物(58 种)、抗生素(16 种)和农药(33 种)。该方法在两个浓度水平(50 和 500 ng L)下成功验证,是传统和耗时的固相萃取(SPE)方法的可行替代方法。89%的 CECs 表现出 70-120%范围内的平均回收率,相对标准偏差(RSD)始终<20%(日内和日间精密度),定量限(LOQ)在 5-500 ng L 范围内(89%的化合物显示 LOQ≤50 ng L)。该方法通过分析城市 TWW 样品(7 个采样事件)证明了其适用性。在监测的样品中,共检测到 35 种 CECs(23 种药物、2 种抗生素和 10 种农药),浓度范围为 5-677 ng L。

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