Folorunsho Omotola, Bogush Anna, Kourtchev Ivan
Centre for Agroecology Water and Resilience (CAWR), Coventry University, Wolston Lane, Ryton on Dunsmore, CV8 3LG, UK.
Anal Methods. 2023 Jan 19;15(3):284-296. doi: 10.1039/d2ay01574a.
In recent years emerging contaminants (ECs) have received significant attention due to their widespread detection in surface waters and concerns that these compounds can cause adverse ecological and/or human health effects. Therefore, accurate methods for determining and quantifying ECs in surface water are essential for estimating their environmental impact. This work describes the development, validation and application of a sensitive multiclass method for simultaneous determination of 22 per and polyfluorinated alkyl substances (PFASs), 3 pharmaceuticals, 15 pesticides, and 2 bisphenols in surface water using on-line solid phase extraction (SPE) coupled with ultra-performance liquid chromatography-high-resolution mass spectrometry (UPLC-HRMS). The method allows simultaneous sample clean-up from interfering matrices and lower limits of detection (LODs) by injecting a large sample volume into the LC system without compromising chromatographic efficiency and resolution. Linearity of response over several orders of magnitude was demonstrated for all tested compounds ( > 0.99), with the LODs ranging from 0.8 and 33.7 pg mL, allowing detection of ECs at trace levels in surface water. The method showed acceptable accuracy and precision (CV, % and RE below 20%) for all tested ECs. It also provided recoveries between 60% and 130% for all tested ECs. The validated method was successfully applied for analysis of surface water samples from three rivers (Cam, Ouse and Thames) in England. Several ECs, including perfluorooctanesulfonic acid (PFOS), perfluorobutanesulfonic acid (PFBS), perfluorohexanoic acid (PFHxA), perfluorohexane sulfonic acid (PFHxS), dimethyl-metatoluamide (DEET) and ibuprofen were observed in analysed surface water above the method's limit of quantitation (LOQ), with concentrations ranging between 3.5 and 460 pg mL.
近年来，新兴污染物（ECs）因其在地表水中的广泛检出以及人们对这些化合物可能导致不利生态和/或人类健康影响的担忧而受到广泛关注。因此，准确测定和量化地表水中新兴污染物的方法对于评估其环境影响至关重要。本研究描述了一种灵敏的多类分析方法的开发、验证及应用，该方法采用在线固相萃取（SPE）与超高效液相色谱 - 高分辨率质谱联用（UPLC - HRMS）同时测定地表水中的22种全氟和多氟烷基物质（PFASs）、3种药物、15种农药和2种双酚。该方法通过向液相色谱系统中注入大量样品，在不影响色谱效率和分辨率的情况下，实现了从干扰基质中同时净化样品并降低检测限（LODs）。所有测试化合物在几个数量级上均呈现出良好的线性响应（>0.99），检测限范围为0.8至33.7 pg/mL，能够检测地表水中痕量水平的新兴污染物。该方法对所有测试的新兴污染物均显示出可接受的准确度和精密度（CV、%和RE均低于20%），所有测试的新兴污染物回收率在60%至130%之间。该经过验证的方法成功应用于分析英格兰三条河流（剑河、乌斯河和泰晤士河）的地表水样品。在分析的地表水中，观察到几种新兴污染物的含量高于该方法的定量限（LOQ），包括全氟辛烷磺酸（PFOS）、全氟丁烷磺酸（PFBS）、全氟己酸（PFHxA）、全氟己烷磺酸（PFHxS）、避蚊胺（DEET）和布洛芬，浓度范围在3.5至460 pg/mL之间。
