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.
J Chromatogr A. 2015 Feb 27;1383:8-17. doi: 10.1016/j.chroma.2015.01.022. Epub 2015 Jan 15.
A novel and Green analytical methodology for the determination of alkylphenols (4-tert-octylphenol, 4-n-octylphenol, 4-n-nonylphenol, nonylphenol) in sediments was developed and validated. The method was based on pressurized hot water extraction (PHWE) followed by miniaturized membrane assisted solvent extraction (MASE) and liquid chromatography-electrospray ionization tandem mass spectrometry detection (LC-ESI-MS/MS). The extraction conditions were optimized by a Plackett-Burman design in order to minimize the number of assays according to Green principles. Matrix effect was studied and compensated using deuterated labeled standards as surrogate standards for the quantitation of the target compounds. The analytical features of the method were satisfactory: relative recoveries varied between 92 and 103% and repeatability and intermediate precision were <9% for all compounds. Quantitation limits of the method (MQL) ranged from 0.061 (4-n-nonylphenol) to 1.7ngg(-1) dry weight (nonylphenol). Sensitivity, selectivity, automaticity and fastness are the main advantages of the exposed methodology. Reagent consumption, analysis time and waste generation were minimized. The "greenness" of the proposed method was evaluated using an analytical Eco-Scale approach and satisfactory results were obtained. The applicability of the proposed method was demonstrated analysing sediment samples of Galicia coast (NW of Spain) and the ubiquity of alkylphenols in the environment was demonstrated.
开发并验证了一种用于测定沉积物中烷基酚（4-叔辛基酚、4-正辛基酚、4-正壬基酚、壬基酚）的新型绿色分析方法。该方法基于加压热水萃取（PHWE），随后进行小型化膜辅助溶剂萃取（MASE）和液相色谱-电喷雾电离串联质谱检测（LC-ESI-MS/MS）。通过Plackett-Burman设计优化萃取条件，以根据绿色原则减少分析次数。使用氘代标记标准物作为替代标准物研究并补偿基质效应，用于目标化合物的定量。该方法的分析特性令人满意：所有化合物的相对回收率在92%至103%之间，重复性和中间精密度均<9%。该方法的定量限（MQL）范围为0.061（4-正壬基酚）至1.7ng g(-1)干重（壬基酚）。灵敏度、选择性、自动化程度和快速性是所提出方法的主要优点。试剂消耗、分析时间和废物产生均降至最低。使用分析生态尺度方法评估了所提出方法的“绿色度”，并获得了满意的结果。通过分析西班牙西北部加利西亚海岸的沉积物样品，证明了所提出方法的适用性，并证明了烷基酚在环境中的普遍存在。
