Department of Chemistry, University of La Rioja, Logroño, La Rioja, Spain.
J Sep Sci. 2011 Sep;34(18):2513-22. doi: 10.1002/jssc.201100159. Epub 2011 Aug 23.
A new method for determining endocrine disrupter compounds (EDCs) in sewage sludge is described in this paper. EDCs studied were bisphenol A (BPA) and alkylphenols (APs). In order to obtain a fast and simple method, selective pressurised liquid extraction (SPLE) and focused ultrasound solid-liquid extraction (FUSLE) were tested. Best results for SPLE were obtained using Florisil as clean-up sorbent and dichloromethane as extraction solvent, while temperature was the only significant variable. Analyte extraction by SPLE was completed in only one extraction cycle of 1 min at 130 °C. FUSLE was carried out in one step of 20 s at 75% power (0.5 cycles) and with 8 mL of ethyl acetate. Although the optimised FUSLE process was faster, simpler and cheaper, SPLE provided higher recovery values (ranging from 81 to 105%) and therefore SPLE-based method was selected and validated. The SPLE and GC-MS method showed an LOD of 10.7 ng/g for BPA and LODs between 1.2 and 41.6 ng/g for APs. Relative standard deviation values lower than 6% were obtained for all analytes. As a result, an efficient, fast and simple method based on SPLE and GC-MS for the determination of BPA and APs in sewage sludge is proposed.
本文介绍了一种测定污水污泥中内分泌干扰化合物（EDCs）的新方法。研究的 EDCs 为双酚 A（BPA）和烷基酚（APs）。为了获得快速简单的方法，本文测试了选择性加压液体萃取（SPLE）和聚焦超声固液萃取（FUSLE）。使用 Florisil 作为净化吸附剂和二氯甲烷作为萃取溶剂时，SPLE 可获得最佳结果，而温度是唯一显著的变量。SPLE 分析物的提取仅在 130°C 下进行 1 分钟的一个提取循环即可完成。FUSLE 在 75%功率（0.5 个周期）和 8 mL 乙酸乙酯下一步完成 20 s。虽然优化的 FUSLE 过程更快、更简单、更便宜，但 SPLE 提供了更高的回收率（81%至 105%），因此选择并验证了基于 SPLE 的方法。SPLE 和 GC-MS 方法对 BPA 的检出限为 10.7 ng/g，对 APs 的检出限为 1.2 至 41.6 ng/g。所有分析物的相对标准偏差值均低于 6%。因此，提出了一种基于 SPLE 和 GC-MS 测定污水污泥中 BPA 和 APs 的高效、快速、简单的方法。
