IMDEA-Water (Madrid Institute for Advanced Studies-Water), Parque Cientifico de la Universidad de Alcala, Alcalá de Henares, Madrid, Spain.
Anal Bioanal Chem. 2012 Oct;404(6-7):1993-2006. doi: 10.1007/s00216-012-6251-9. Epub 2012 Aug 1.
A new analytical method using stir-bar-sorptive extraction (SBSE) followed by liquid desorption (LD) and gas chromatography with triple-quadrupole mass spectrometric detection (GC-QqQ-MS-MS) has been used for quantitative determination of 25 chlorinated endocrine-disrupting compounds (EDCs) in river water and wastewater. The experimental conditions affecting the SBSE-LD performance were studied and are discussed in detail. Results from systematic assay revealed that a 100-mL water sample, stir bars coated with 47 μL PDMS, an extraction time of 14 h (at 900 rpm), 5 % MeOH as modifier and 10 % NaCl resulted in the best analytical recovery of all the target compounds studied. Use of 1:1 ACN-MeOH as back-extraction solvent and two successive sonication steps, each for 5 min, resulted in the best performance for monitoring EDCs in water matrices. The method detection limits for most of the target compounds were very good- ≤ 2 ng L(-1) and ≤10 ng L(-1) for river water and wastewater effluents respectively. Experimental recovery for all the compounds was >70 %, with the exception of simazine for which recovery from the matrix was 65 %. Signal enhancement observed for a few of the compounds in wastewater effluents was managed by use of matrix-matched standards and different injection liners. The method was successfully used for analysis of river water samples from Henares River (Spain) and wastewater effluent samples from wastewater-treatment plants (WWTP). Eleven of the 25 compounds studied were detected in both river water and wastewater effluents. Terbutylazine and methoxychlor were detected in almost all the river water and effluent samples; amounts varied between 37-58.5 ng L(-1) and 15.2-46.8 ng L(-1), respectively. This method was shown enable reliable, effective, and sensitive monitoring of chlorinated EDCs at nanogram levels in surface water and wastewater effluent.
一种新的分析方法，使用搅拌棒吸附萃取（SBSE），然后进行液体解吸（LD）和气相色谱三重四极杆质谱联用（GC-QqQ-MS-MS），已用于定量测定河水中和废水中的 25 种氯化内分泌干扰化合物（EDCs）。研究了影响 SBSE-LD 性能的实验条件，并进行了详细讨论。系统测定结果表明，对于所有研究的目标化合物，100mL 水样、涂有 47μL PDMS 的搅拌棒、14h 的萃取时间（在 900rpm 下）、5%甲醇作为改性剂和 10%NaCl，可获得最佳的分析回收率。使用 1:1 ACN-MeOH 作为反萃取溶剂，并进行两次连续超声处理，每次 5min，可获得水基质中 EDCs 的最佳监测性能。大多数目标化合物的方法检测限都非常好-分别为≤2ngL(-1)和≤10ngL(-1)，适用于河水和废水。所有化合物的实验回收率均>70%，除西玛津外，其对基质的回收率为 65%。一些化合物在废水处理厂废水中的信号增强通过使用基质匹配标准和不同的进样衬管来管理。该方法成功地用于分析来自 Henares 河（西班牙）的河水样品和来自废水处理厂（WWTP）的废水样品。在所研究的 25 种化合物中，有 11 种在河水和废水处理厂废水中都有检出。特丁基嗪和甲氧氯普遍存在于几乎所有的河水和废水处理厂废水中；含量分别在 37-58.5ngL(-1)和 15.2-46.8ngL(-1)之间变化。该方法能够可靠、有效、灵敏地监测地表水和废水处理厂废水中纳克级的氯化 EDCs。
