Department of Analytical Chemistry, University of Almeria, E-04071, Almeria, Spain.
J Chromatogr A. 2010 Dec 10;1217(50):7817-25. doi: 10.1016/j.chroma.2010.10.011. Epub 2010 Oct 12.
The analysis of a wide range of pesticides in wastewaters (WWs) undergoing different treatments (both modern and conventional) has been studied. The need for optimizing specific extraction methods for each WW effluent based on their physico-chemical characteristics has been considered. A distribution study was performed to establish if the filtration step before extraction is a correct procedure since pesticides can be more prone to be in the aqueous or the solid phase, depending on their hydrophobicity. This evaluation demonstrated that pesticides are distributed between the aqueous phase and the suspended particulate matter (SPM; e.g. pyrethroids are only found in the SPM). The proposed methodologies involved the determination of 39 polar and 139 non-polar pesticides using solid-phase extraction (SPE) and pressurized-liquid extraction (PLE) for the extraction of the aqueous phase and the SPM, respectively. Ultra high pressure liquid chromatography and gas chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS, GC-MS/MS) were used in the determination stage. WW samples from four different technologies were evaluated: membrane bioreactor, extended aeration, maturation pond and anaerobic pond. Validation data for the four effluents studied were generated, obtaining adequate precision values (estimated as % relative standard deviation, RSD) in almost all cases (<25%). The methods showed limits of detection at 0.01-0.20μgL(-1) and limits of quantification from 0.02 to 0.50μgL(-1). The proposed methods were applied to the analysis of real samples collected from an experimental WW treatment plant, detecting non-polar and polar pesticides at concentrations in the range 0.02-1.94μgL(-1) and 0.02-0.33μgL(-1), respectively.
研究了对不同处理（包括现代和传统处理）的废水中（WW）的多种农药进行分析。考虑到需要根据 WW 废水的物理化学特性优化特定的提取方法。进行了分配研究，以确定在提取之前进行过滤步骤是否是正确的程序，因为农药可能更容易处于水相或固相，这取决于它们的疏水性。该评估表明，农药分布在水相和悬浮颗粒物（SPM；例如，拟除虫菊酯仅存在于 SPM 中）之间。所提出的方法涉及使用固相萃取（SPE）和加压液体萃取（PLE）分别提取水相和 SPM 中的 39 种极性和 139 种非极性农药。超高效液相色谱和气相色谱串联质谱（UHPLC-MS/MS、GC-MS/MS）用于测定阶段。评估了来自四种不同技术的 WW 样品：膜生物反应器、扩展曝气、成熟池塘和厌氧池塘。为研究的四种废水生成了验证数据，在几乎所有情况下（<25%）都获得了足够的精密度值（估计为%相对标准偏差，RSD）。该方法的检测限为 0.01-0.20μgL(-1)，定量限为 0.02 至 0.50μgL(-1)。该方法应用于从实验性 WW 处理厂采集的实际样品的分析，检测到非极性和极性农药的浓度范围分别为 0.02-1.94μgL(-1)和 0.02-0.33μgL(-1)。
