Simultaneous determination of aliphatic and aromatic amines in water and sediment samples by ion-pair extraction and gas chromatography–mass spectrometry

A gas chromatography–mass spectrometry (GC–MS) method has been proposed for the determination of aliphatic and aromatic amines in a variety of environmental samples including wastewater, river water, sea water and sediment samples. The method includes ion-pair extraction with bis-2-ethylhexylphosphate (BEHPA), derivatisation of compounds with isobutyl chloroformate (IBCF) and their GC–MS analysis. Aliphatic and aromatic amines were isolated from aqueous samples using BEHPA as ion-pair reagent and derivatised with IBCF for their chromatographic analysis. Solid–liquid extraction of aliphatic and aromatic amines in sediment samples were performed in Soxhlet apparatus with acidic MeOH and ion-pair extraction with BEHPA were carried out for the isolation of amines followed by derivatisation with IBCF. Aliphatic and aromatic amines were then analysed with GC–MS in both electron impact (EI) and positive and negative ion chemical ionisation (PNICI) mode as their isobutyloxycarbonyl (isoBOC) derivatives. The obtained recoveries ranged from 81.0 to 98.0% and the precision of this method, as indicated by the relative standard deviations (RSDs) was within the range of 0.5 and 4.3%. The detection limits obtained from calculations by using GC–MS results based on S/N = 3 were within the range from 0.07 to 0.50 ng/l.