Department of Analytical Chemistry, University of A Coruña, Campus da Zapateira, Rúa da Fraga 10, E-15008 A Coruña, Spain.
J Chromatogr A. 2012 Feb 3;1223:1-8. doi: 10.1016/j.chroma.2011.12.011. Epub 2011 Dec 9.
A fast, simple, sensitive and green analytical chemistry method for the simultaneous determination of alkylphenols (4-tert-octylphenol, 4-octylphenol, 4-n-nonylphenol, nonylphenol) and bisphenol A in seawater was developed and validated. The procedure was based on a dispersive liquid-liquid microextraction (DLLME) of a small volume of seawater sample (30 mL) using only 100 μL of 1-octanol, combined with liquid chromatography-electrospray ionization tandem mass spectrometry in negative mode (LC-ESI-MS/MS). The matrix effect was studied and compensated using deuterated labelled standards as surrogate standards for the quantitation of target compounds. The analytical features of the proposed method were satisfactory: repeatability and intermediate precision were <10% and recoveries were around 84-104% for all compounds. Uncertainty assessment of measurement was estimated on the basis of an in-house validation according to EURACHEM/CITAC guide. Quantitation limits of the method (MQL) ranged between 0.005 and 0.03 μg L⁻¹, therefore the levels established in the Directive 2008/105/EC were achieved. The applicability of the proposed method was demonstrated analyzing seawater samples from different sites of A Coruña (Northwest of Spain). The analyses showed the presence of all compounds at levels between 0.035 (bisphenol A) and 0.14 μg L⁻¹ (nonylphenol).
建立并验证了一种快速、简单、灵敏且绿色的分析化学方法，用于同时测定海水中的烷基酚（4-叔辛基苯酚、4-辛基苯酚、4-壬基苯酚、壬基苯酚）和双酚 A。该方法基于分散液液微萃取（DLLME），仅用 100 μL 1-辛醇萃取 30 mL 小体积海水样品，结合液相色谱-电喷雾串联质谱在负离子模式下（LC-ESI-MS/MS）进行分析。采用氘代标记标准品作为内标，研究并补偿了基质效应，用于目标化合物的定量。该方法的分析性能令人满意：所有化合物的重复性和中间精密度均<10%，回收率在 84-104%之间。根据 EURACHEM/CITAC 指南进行内部验证，对测量不确定度进行了评估。该方法的定量限（MQL）在 0.005-0.03 μg L⁻¹ 之间，因此达到了指令 2008/105/EC 规定的水平。该方法应用于测定西班牙西北部拉科鲁尼亚不同地点的海水样品，结果表明所有化合物的浓度在 0.035（双酚 A）至 0.14 μg L⁻¹（壬基苯酚）之间。
