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).
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).
Department of Analytical Chemistry, University of A Coruña, Campus da Zapateira, Rúa da Fraga 10, E-15008 A Coruña, Spain.
N
N
Salgueiro-González
E
E
Concha-Graña
I
I
Turnes-Carou
S
S
Muniategui-Lorenzo
P
P
López-Mahía
D
D
Prada-Rodríguez
D001559:Benzhydryl Compounds; D004968:Estrogens, Non-Steroidal / Q000032:analysis / Q000302:isolation & purification; D059627:Liquid Phase Microextraction / Q000379:methods*; D010636:Phenols / Q000032:analysis* / Q000302:isolation & purification; D015203:Reproducibility of Results; D012623:Seawater / Q000032:analysis*; D012680:Sensitivity and Specificity; D013030:Spain; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification; D000098826:Bisphenol A Compounds
D001559:Benzhydryl Compounds; D004968:Estrogens, Non-Steroidal; D010636:Phenols; D014874:Water Pollutants, Chemical; C025256:nonylphenol; C080417:4-octylphenol; C041594:4-nonylphenol; C105260:4-tert-octylphenol; C006780:bisphenol A; D000098826:Bisphenol A Compounds