Hollow fiber membrane-protected solid-phase microextraction of triazine herbicides in bovine milk and sewage sludge samples

A porous polypropylene hollow fiber membrane (HFM)-protected solid-phase microextraction (HFM-SPME) procedure in conjunction with gas chromatography/mass spectrometric analysis for use in the determination of triazine herbicides in bovine milk samples is described. A 65-mum polydimethylsiloxane-divinylbenzne (PDMS-DVB) SPME fiber was protected by an EIFM. HFM-SPME experimental parameters such as fiber type, extraction time, extraction temperature and salt concentration were investigated and optimized. The relative standard deviations for the reproducibility of the optimized HFM-SPME method varied from 4.30 to 12.37%. The correlation coefficients of the calibration curves were between 0.9799 and 0.9965 across a concentration range of 0-200 mug l(-1). The method detection limits for triazines in bovine milk were in the range of 0.003-0.013 mug l(-1) and limits of quantification were in the range of 0.006-0.021 mug l(-1). The suitability of HFM-SPME was extended to the analysis of the herbicides in sewage sludge samples. The results demonstrate that HFM-SPME was an efficient pretreatment and enrichment procedure for complex matrices. (C) 2004 Elsevier B.V. All rights reserved.