Salgueiro-González N, Turnes-Carou I, Muniategui-Lorenzo S, López-Mahía P, Prada-Rodríguez D
Grupo Química Analítica Aplicada (QANAP), Instituto Universitario de Medio Ambiente (IUMA), Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus de A Coruña, E-15071 A Coruña, Spain.
Grupo Química Analítica Aplicada (QANAP), Instituto Universitario de Medio Ambiente (IUMA), Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus de A Coruña, E-15071 A Coruña, Spain.
Anal Chim Acta. 2014 Dec 10;852:112-20. doi: 10.1016/j.aca.2014.09.041. Epub 2014 Sep 28.
A less time-, solvent- and sorbent-consuming analytical methodology for the determination of bisphenol A and alkylphenols (4-tert-octylphenol, 4-octylphenol, 4-n-nonylphenol, nonylphenol) in marine sediment was developed and validated. The method was based on selective pressurized liquid extraction (SPLE) with a simultaneous in cell clean up combined with liquid chromatography-electrospray ionization tandem mass spectrometry in negative mode (LC-ESI-MS/MS). The SPLE extraction conditions were optimized by a Plackett-Burman design followed by a central composite design. Quantitation was performed by standard addition curves in order to correct matrix effects. The analytical features of the method were satisfactory: relative recoveries varied between 94 and 100% and repeatability and intermediate precision were <6% 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 0.17 (4-n-nonylphenol) and 4.01 ng g(-1) dry weight (nonylphenol). Sensitivity, selectivity, automaticity and fastness are the main advantages of this green methodology. As an application, marine sediment samples from Galicia coast (NW of Spain) were analysed. Nonylphenol and 4-tert-octylphenol were measured in all samples at concentrations between 20.1 and 1409 ng g(-1) dry weight, respectively. Sediment toxicity was estimated and no risk to aquatic biota was found.
开发并验证了一种测定海洋沉积物中双酚A和烷基酚（4-叔辛基酚、4-辛基酚、4-正壬基酚、壬基酚）的分析方法，该方法耗时更短、溶剂和吸附剂消耗更少。该方法基于选择性加压液体萃取（SPLE），同时在萃取池中进行净化，并结合负离子模式的液相色谱-电喷雾电离串联质谱（LC-ESI-MS/MS）。通过Plackett-Burman设计优化SPLE萃取条件，随后进行中心复合设计。采用标准加入曲线进行定量，以校正基质效应。该方法的分析特性令人满意：所有化合物的相对回收率在94%至100%之间，重复性和中间精密度均<6%。根据EURACHEM/CITAC指南，基于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0.17（4-正壬基酚）至4.01 ng g⁻¹干重（壬基酚）之间。灵敏度、选择性、自动化程度和快速性是这种绿色方法的主要优点。作为应用实例，分析了来自西班牙西北部加利西亚海岸的海洋沉积物样品。所有样品中壬基酚和4-叔辛基酚的测量浓度分别在20.1至1409 ng g⁻¹干重之间。评估了沉积物毒性，未发现对水生生物群的风险。
