Extraction and determination of the Mitins sulcofuron and flucofuron from environmental river water

Abstract

Flucofuron and sulcofuron, both examples of Mitins, were employed as the active ingredients in mothproofing formulations for the protection of textile fabrics by the dyeing industry. Monitoring of their presence in components of the river ecosystem is a regulatory requirement so precise extraction techniques, combined with sensitive detection systems, are required to obtain valid data concerning the levels of target pollutants present. This study continued the development of liquid chromatography combined with negative-ion electrospray ionization tandem mass spectrometry (LC–ESI-MS–MS) operated in the multiple reaction monitoring mode for the determination of these analytes in complex matrices. The paper describes the development of liquid–liquid extraction (LLE) and solid-phase extraction (SPE) techniques for the determination of the analytes in environmental river water. The methods employed an internal standard, trichlorocarbanilide (TCC), to check the extraction efficiencies but not to correct environmental data. The extraction efficiencies obtained with LLE were 73.2 ± 6.7, 112.4 ± 8.6 and 96.4 ± 14.3% (n = 5) compared with 74.3 ± 8.4, 115.9 ± 3.1 and 112.7 ± 4.5% (n = 4) employing SPE for sulcofuron, flucofuron and TCC (100 ng l^–1 matrix fortification level), respectively. The SPE results are consistent with those obtained for LLE, although the precision of the SPE method was better than that of the LLE method. These methods were then successfully applied to samples obtained from a contaminated ecosystem.