Department of Analytical Chemistry, University of A Coruña, Campus da Zapateira, Rúa da Fraga 10, E-15008 A Coruña, Spain.
J Chromatogr A. 2012 Dec 28;1270:80-7. doi: 10.1016/j.chroma.2012.11.014.
A novel and green analytical methodology for the determination of alkylphenols (4-tert-octylphenol, 4-n-octylphenol, 4-n-nonylphenol, nonylphenol technical mixture) and bisphenol A in bivalve mollusc samples 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). 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 80 and 107% and repeatability and intermediate precision were <20% 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 0.34 (4-n-octylphenol) and 3.6 ng g(−1) dry weight (nonylphenol). The main advantages of the method are sensitivity, selectivity, automaticity, low volumes of solvents required and low sample analysis time (according with the principles of Green Chemistry). The method was applied to the analysis of mussel samples of Galicia coast (NW of Spain). Nonylphenol and 4-tert-octylphenol were measured in all samples at concentrations between 9.3 and 372 ng g(−1) dw. As an approach, the human daily intake of these compounds was estimated and no risk for human health was found.
建立并验证了一种用于测定双壳贝类样品中烷基酚（4-叔辛基苯酚、4-正辛基苯酚、4-正壬基苯酚、壬基酚工业混合物）和双酚 A 的新型绿色分析方法。该方法基于选择性加压液体萃取（SPLE），同时进行细胞内净化，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。采用标准添加曲线进行定量，以校正基质效应。该方法的分析性能令人满意：所有化合物的相对回收率在 80%至 107%之间，重复性和中间精密度均<20%。根据 EURACHEM/CITAC 指南，基于内部验证对测量不确定度进行了评估。方法的定量限（MQL）范围为 0.34（4-正辛基苯酚）至 3.6ng/g 干重（壬基酚）。该方法的主要优点是灵敏度高、选择性好、自动化程度高、所需溶剂体积小、样品分析时间短（符合绿色化学原则）。该方法应用于西班牙西北部加利西亚海岸的贻贝样品分析。在所分析的所有贻贝样品中，均检测到了壬基酚和 4-叔辛基苯酚，浓度范围在 9.3 至 372ng/g 干重之间。作为一种方法，对这些化合物的人体日摄入量进行了估计，未发现对人体健康有风险。
