Herrero P, Borrull F, Marcé R M, Pocurull E
Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili Campus Sescelades, Marcel·lí Domingo s/n, 43007 Tarragona, Spain.
Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili Campus Sescelades, Marcel·lí Domingo s/n, 43007 Tarragona, Spain.
J Chromatogr A. 2014 Aug 15;1355:53-60. doi: 10.1016/j.chroma.2014.05.086. Epub 2014 Jun 18.
Benzothiazole, benzotriazole and benzenesulfonamide derivates are well-known aquatic contaminants, although very few studies have been published about their occurrence in sewage sludge samples. In this paper, a pressurised hot water extraction (PHWE) method has been developed for the simultaneous determination of these families of compounds. The compounds were determined by LC-Orbitrap-HRMS and several clean-up strategies such as in-cell PHWE and solid-phase extraction (SPE) were tested to reduce the high matrix effect that occurs when sludge samples are analysed. Absolute recoveries using the whole method were above 80% and the matrix effect was under -20% for most of the compounds studied. Repeatability and reproducibility were usually under 10% (%RSD, 50 and 250ngg(-1) (d.w.), n=5), while LODs and LOQs were between 0.25 and 25ngg(-1) (d.w.) and 0.5 and 50ngg(-1) (d.w.), respectively. The PHWE/SPE/LC-HRMS method developed was used to analyse several sludge samples collected from five sewage treatment plants (STPs) in Catalonia that use different sewage treatments. The most frequently determined compounds were benzotriazole derivates and the most abundant compound found was 2-hydroxybenzothiazole.
苯并噻唑、苯并三唑和苯磺酰胺衍生物是众所周知的水生污染物，尽管关于它们在污水污泥样品中的存在情况的研究很少。本文开发了一种加压热水萃取（PHWE）方法，用于同时测定这些化合物家族。通过液相色谱-轨道阱-高分辨质谱（LC-Orbitrap-HRMS）测定这些化合物，并测试了几种净化策略，如柱内PHWE和固相萃取（SPE），以减少分析污泥样品时出现的高基质效应。使用整个方法的绝对回收率高于80%，对于大多数研究的化合物，基质效应低于-20%。重复性和再现性通常低于10%（相对标准偏差%RSD，50和250ng g(-1)（干重），n=5），而检测限（LOD）和定量限（LOQ）分别在0.25至25ng g(-1)（干重）和0.5至50ng g(-1)（干重）之间。所开发的PHWE/SPE/LC-HRMS方法用于分析从加泰罗尼亚五个使用不同污水处理方法的污水处理厂（STP）采集的几个污泥样品。最常测定的化合物是苯并三唑衍生物，发现的最丰富的化合物是2-羟基苯并噻唑。
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