Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Sescelades Campus, Marcel·lí Domingo s/n, 43007 Tarragona, Spain.
Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Sescelades Campus, Marcel·lí Domingo s/n, 43007 Tarragona, Spain.
J Chromatogr A. 2014 Apr 25;1339:34-41. doi: 10.1016/j.chroma.2014.02.081. Epub 2014 Mar 5.
A Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction method followed by liquid chromatography-(Orbitrap) high resolution mass spectrometry was developed for the simultaneous determination of five benzotriazole, four benzothiazole and five benzenesulfonamide derivates in sewage sludge. While the method was being developed, several buffers and dispersive solid-phase extraction clean-up (dSPE) sorbents were tested. Citrate buffer and Z-sep+ (zirconium-based sorbent) were the most effective extraction buffer and dSPE clean-up material. The absolute recoveries were higher than 80% for all compounds (100ng/g (d.w.)) and the matrix effect was less than -20% for most compounds. The limits of detection were between 0.5 and 10ng/g (d.w.) and the limits of quantification (LOQ) were between 1 and 25ng/g (d.w.). Repeatability and reproducibility were lower than 15% (%RSD, n=5). Several sludge samples from five sewage treatment plants in Catalonia were analysed and the most abundant compounds were 2-hydroxybenzothiazole (<LOQ-181.2ng/g (d.w.)) and 4-methyl-1-H-benzotriazole (<LOQ-82.3ng/g (d.w.)). Benzenesulfonamide (n.d.-70.2ng/g (d.w.)) and toluenesulfonamide (n.d.-83.9ng/g (d.w.)) were also determined.
建立了一种快速、简便、价廉、有效、耐用和安全（QuEChERS）的提取方法，结合液相色谱-（轨道阱）高分辨质谱法，同时测定污水污泥中的五种苯并三唑、四种苯并噻唑和五种苯磺酰胺衍生物。在方法开发过程中，测试了几种缓冲液和分散固相萃取净化（dSPE）吸附剂。柠檬酸盐缓冲液和 Z-sep+（基于锆的吸附剂）是最有效的提取缓冲液和 dSPE 净化材料。所有化合物（100ng/g（干重））的绝对回收率均高于 80%，大多数化合物的基质效应小于-20%。检测限在 0.5 和 10ng/g（干重）之间，定量限（LOQ）在 1 和 25ng/g（干重）之间。重复性和再现性低于 15%（%RSD，n=5）。对加泰罗尼亚五个污水处理厂的几个污泥样品进行了分析，最丰富的化合物是 2-羟基苯并噻唑（<LOQ-181.2ng/g（干重））和 4-甲基-1-H-苯并三唑（<LOQ-82.3ng/g（干重））。还测定了苯磺酰胺（n.d.-70.2ng/g（干重））和甲苯磺酰胺（n.d.-83.9ng/g（干重））。
