Food and Environmental Safety Research Group, Department of Medicine Preventive, Faculty of Pharmacy, University of Valencia, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, Valencia, Spain.
Food and Environmental Safety Research Group, Department of Medicine Preventive, Faculty of Pharmacy, University of Valencia, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, Valencia, Spain.
J Chromatogr A. 2015 Jan 23;1378:19-31. doi: 10.1016/j.chroma.2014.11.079. Epub 2014 Dec 18.
Pressurized liquid extraction (PLE) and Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction methods were optimized for the simultaneous determination of 50 pesticides in sediment, soils and sewage sludge. For QuEChERS development, several buffers and dispersive solid-phase extraction clean-up (dSPE) sorbents were tested. In the PLE method, several parameters affecting the extraction efficiency, such as organic solvent, amount of sample, cell size, temperature, pressure, static time, number of cycles and % of flush, as well as sorbent used for the on-line clean up, were also evaluated. PLE and QuEChERS were assessed and compared in obtained recoveries (33-89% versus 25-120%), number of pesticides for which recoveries are in the range of 80-100% (up to 13 versus up to 35) and cost of the approach. QuEChERS procedure was faster, cheaper and easier to perform. Recoveries were around 80% (at 50ngg(-1) d.w.) and the matrix effect was less than -20% using matrix-matched standard calibration curve for most of the analytes. The limits of quantification were between 0.1 and 10ngg(-1) (d.w.) except for alachlor and acetochlor. Repeatability and reproducibility were lower than 28% (%RSD, n=5). Soil, sediment and sludge samples, taken from the Túria River Basin, were analyzed by QuEChERS to determine pesticides. Chlorpyrifos (up to 65.3ngg(-1) d.w.) was the most frequent and at higher concentrations. Thiabendazole, imazalil, diazinon, pyriproxyfen, hexythiazox, carbofuran, isoproturon, terbuthylazine and terbumeton were also found in some samples.
加压液体萃取(PLE)和快速、简便、廉价、有效、坚固和安全(QuEChERS)萃取方法被优化用于同时测定沉积物、土壤和污水污泥中的 50 种农药。对于 QuEChERS 的开发,测试了几种缓冲液和分散固相萃取净化(dSPE)吸附剂。在 PLE 方法中,还评估了影响萃取效率的几个参数,如有机溶剂、样品量、细胞大小、温度、压力、静态时间、循环次数和冲洗百分比,以及用于在线净化的吸附剂。评估并比较了 PLE 和 QuEChERS 的回收率(33-89%对 25-120%)、回收率在 80-100%范围内的农药数量(多达 13 种对多达 35 种)和方法成本。QuEChERS 方法更快、更便宜且更易于执行。在大多数分析物中,使用基质匹配标准校准曲线,回收率约为 80%(在 50ngg(-1) d.w.),基质效应小于-20%。除了甲草胺和乙草胺外,定量限在 0.1 和 10ngg(-1)(d.w.)之间。重复性和再现性低于 28%(%RSD,n=5)。从图里亚河流域采集的土壤、沉积物和污泥样品用 QuEChERS 进行分析以确定农药。氯吡硫磷(高达 65.3ngg(-1) d.w.)是最常见的,浓度也更高。噻菌灵、咪唑菌酮、二嗪磷、吡虫丙醚、己唑醇、克百威、异丙隆、特丁津和特丁硫磷也在一些样品中被发现。