J. Slobodnik et al., Determination of microcontaminants in sediments by on-line solid-phase extraction-gas chromatography-mass spectrometry, CHEMOSPHERE, 41(9), 2000, pp. 1469-1478
Two simple and straightforward analytical procedures for the screening of s
ediment samples are reported. They involve extraction with ethyl acetate or
methanol and subsequent analysis by means of gas chromatography-mass spect
rometry (GC-MS) using large-volume injection (LVI) or solid-phase extractio
n (SPE). The latter, which was originally developed for the analysis of aqu
eous samples, can be used without any modification. In general, 10 ml of or
ganic solvent were added to 2 g of sediment, and the mixture was shaken and
allowed to stand overnight. The methanolic extracts were then diluted in w
ater and subjected to preconcentration and analysis using on-line SPE-GCMS.
The ethyl acetate extracts were injected directly into the GC using LVI. B
oth methods were used for the detection and identification of microcontamin
ants during a monitoring study of the river Nitra (Slovak Republic). They i
ncluded polyaromatic hydrocarbons (PAHs), chlorofluorohydrocarbons, alkoxyl
ated and alkylated phenols and benzothiazole derivatives. Semi-quantitative
profiles of the contaminants were constructed and provisionally interprete
d. The results indicate that SPE-GC-MS, and also LVI-GC-MS, have good poten
tial for a rapid screening of sediment samples and the identification of mi
crocontaminants. The analytical procedures pose no problems, and the on-lin
e set-up is user-friendly. (C) 2000 Elsevier Science Ltd. All rights reserv
ed.