Lara-Martín Pablo A, Gómez-Parra Abelardo, González-Mazo Eduardo
Departamento de Química Física, Facultad de Ciencias del Mar y Ambientales, Universidad de Cádiz, Campus Río San Pedro s/n 11510 Puerto Real, Cádiz, Spain.
J Chromatogr A. 2006 Dec 29;1137(2):188-97. doi: 10.1016/j.chroma.2006.10.009. Epub 2006 Oct 30.
A new methodology capable of performing the simultaneous analysis of the main surfactants--linear alkylbenzene sulfonates (LAS), alkyl ethoxysulfates (AES), alkyl sulfates (AS), nonylphenol polyethoxylates (NPEOs) and alcohol polyethoxylates (AEOs)--and their carboxylated metabolites--sulfophenyl carboxylic acids (SPCs) and alkylphenol ethoxycarboxylates (APECs)--in environmental samples has been developed for the first time. Extraction is carried out by solid-phase extraction (SPE) and pressurized liquid extraction (PLE) from water and sediment, respectively. Identification and quantification of the target compounds is performed using a liquid chromatography-mass spectrometry (LC-MS) system equipped with an electrospray interface (ESI) operating in mixed-mode. Optimization of parameters such as pH, ionic strength, temperature and solvents has been carried out in order to obtain recoveries in the range from 70 to 107% for most homologs, while the limits of detection are 0.05-0.5 ng mL(-1) in water and 1-10 ng g(-1) in sediment. The proposed methodology has been applied for the simultaneous determination of all the target compounds in samples taken from aquatic ecosystems in the SW of Spain. Values for LAS, AS, AES, NPEOs and AEOs are up to 38.7, 3.0, 2.9, 5.0 and 1.2 microg L(-1) in waters, and in the ranges of 1.73-12.80, 0.11-0.24, 0.02-0.59, 1.94-2.70 and 0.64-3.64 mg kg(-1) in sediments, respectively. The highest concentrations of metabolites found in water are 149.6 microg L(-1) of SPCs and 3.9 microg L(-1) of APECs.
首次开发出一种新方法，可对环境样品中的主要表面活性剂——直链烷基苯磺酸盐（LAS）、烷基醚硫酸盐（AES）、烷基硫酸盐（AS）、壬基酚聚乙氧基化物（NPEO）和醇聚乙氧基化物（AEO）——及其羧化代谢物——磺基苯基羧酸（SPC）和烷基酚乙氧基羧酸盐（APEC）进行同步分析。分别通过固相萃取（SPE）和加压液体萃取（PLE）从水和沉积物中进行萃取。使用配备电喷雾接口（ESI）且以混合模式运行的液相色谱 - 质谱（LC - MS）系统对目标化合物进行鉴定和定量。已对pH、离子强度、温度和溶剂等参数进行了优化，以使大多数同系物的回收率在70%至107%范围内，而水中的检测限为0.05 - 0.5 ng mL⁻¹，沉积物中的检测限为1 - 10 ng g⁻¹。所提出的方法已应用于西班牙西南部水生生态系统采集的样品中所有目标化合物的同步测定。水中LAS、AS、AES、NPEO和AEO的值分别高达38.7、3.0、2.9、5.0和1.2 μg L⁻¹，沉积物中的值分别在1.73 - 12.80、0.11 - 0.24、0.02 - 0.59、1.94 - 2.70和0.64 - 3.64 mg kg⁻¹范围内。在水中发现的代谢物的最高浓度为SPC 149.6 μg L⁻¹和APEC 3.9 μg L⁻¹。
