Determination of alkylphenols and bisphenol A in seawater samples by dispersive liquid–liquid microextraction and liquid chromatography tandem mass spectrometry for compliance with environmental quality standards (Directive 2008/105/EC)

• Published in: Journal of Chromatography A Vol. 1223; pp. 1 - 8
• Main Authors: Salgueiro-González, N., Concha-Graña, E., Turnes-Carou, I., Muniategui-Lorenzo, S., López-Mahía, P., Prada-Rodríguez, D.
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 03.02.2012
• Subjects: Alkylphenols; Benzhydryl Compounds; Bisphenol A; Dispersive liquid–liquid microextraction; Estrogens, Non-Steroidal - analysis; Estrogens, Non-Steroidal - isolation & purification; LC–ESI-MS/MS; Liquid Phase Microextraction - methods; Phenols - analysis; Phenols - isolation & purification; Reproducibility of Results; Seawater; Seawater - analysis; Sensitivity and Specificity; Spain; Spectrometry, Mass, Electrospray Ionization - methods; Tandem Mass Spectrometry - methods; Water Pollutants, Chemical - analysis; Water Pollutants, Chemical - isolation & purification; Bisphenol A; Alkylphenols; Dispersive liquid–liquid microextraction; LC–ESI-MS/MS; Seawater
• DOI: 10.1016/j.chroma.2011.12.011
• ISSN: 0021-9673

► Fast, simple and sensitive method for APs and BPA determination in seawater. ► DLLME of 30 mL of sample with only 100 μL of 1-octanol (Green Chemistry principles). ► Ultratrace determination with lower sample volumes than literature. ► Compliance of the Directive 2008/105/EC. 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).