Abstract
Water-soluble components from sludge and sediments were sampled and analyzed with solid-phase microextraction (SPME) and high-performance liquid chromatography–electrospray ionization–mass spectrometry (HPLC–ESI–MS). The extraction, desorption, and detection conditions were examined with Carbowax-coated SPME fibers for a number of selected carboxylic acids, phthalates, and surfactants. The maximum recoveries of the defined compounds were obtained for extraction times ranging from 1 to 15 h (phthalates and surfactants) with a desorption time of 2 min for a of 80:20 (v/v) methanol–ethanol mixture. The reference compounds were detected in the low-ppb range. The main components of analyzed sludge and sediment samples were identified as phthalates, fatty acids, nonionic surfactants, chlorinated phenols, and carbohydrate derivatives. Additional information for compound identification was obtained using different spray potentials for the mass spectrometric ionization. Switching from positive to negative ionization modes changed the selectivity and sensitivity of detection, thus allowing the detection of substances of different nature. © 1998 John Wiley & Sons, Inc. J Micro Sep 10: 225–234, 1998
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