Simultaneous microwave-assisted extraction of polycyclic aromatic hydrocarbons, polychlorinated biphenyls, phthalate esters and nonylphenols in sediments.
A new method was developed for the simultaneous extraction of polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), phthalate esters (PEs), nonylphenols (NPs) and nonylphenol mono- and diethoxylates (NP1EOs and NP2EOs, respectively) in sediment samples by means of a closed microwave system. The extractions were carried out at 21 psi and 80% of microwave power and 15 ml of acetone were used as the common extraction solvent. The filtered extract was further fractionated in two groups using Florisil cartridges: PAHs and PCBs were eluted with n-hexane:toluene (4:1) and the PEs, NPs and ethoxylates were eluted with ethyl acetate. All the compounds were analysed by gas chromatography-mass spectrometry (GC-MS). In case of PAHs and PCBs, the developed method was validated by comparison of the results obtained for the certified reference material NIST 1944 with the certified values. In the absence of a reference material for phthalate esters and nonylphenols, one sediment sample was extracted twice under the optimal conditions in order to check than an exhaustive extraction of the analytes occurred. This method is currently used in the study of the distribution of those organic contaminants in the estuaries of the Bay of Biscay (Spain).
Bartolomé
L
L
Kimika Analitikoaren Saila, Euskal Herriko Unibertsitatea, 644 Posta Kutxatila, E-48080 Bilbao, Spain.
Cortazar
E
E
Raposo
J C
JC
Usobiaga
A
A
Zuloaga
O
O
Etxebarria
N
N
Fernández
L A
LA
D000096:Acetone; D005591:Chemical Fractionation / Q000379:methods; D004784:Environmental Monitoring / Q000379:methods; D004785:Environmental Pollutants / Q000302:isolation & purification*; D005026:Ethylene Glycols / Q000302:isolation & purification; D008401:Gas Chromatography-Mass Spectrometry; D019015:Geologic Sediments / Q000737:chemistry*; D008872:Microwaves; D010636:Phenols / Q000302:isolation & purification*; D010795:Phthalic Acids / Q000302:isolation & purification*; D011078:Polychlorinated Biphenyls / Q000302:isolation & purification*; D011084:Polycyclic Aromatic Hydrocarbons / Q000302:isolation & purification*; D015203:Reproducibility of Results; D012997:Solvents; D013030:Spain
D004785:Environmental Pollutants; D005026:Ethylene Glycols; D010636:Phenols; D010795:Phthalic Acids; D011084:Polycyclic Aromatic Hydrocarbons; D012997:Solvents; D000096:Acetone; C021754:terics; C025256:nonylphenol; D011078:Polychlorinated Biphenyls