Solid-phase microextraction for determination of 3-chloro-4-(dichloromethyl)-5-hydroxy-2[5H]-furanone in water

Abstract

Microextração em fase sólida, usando a derivatização on-line com bis(trimetilsilil)trifluoroacetamida, cromatografia a gás e espectrometria de massas, foi avaliada para a quantificação de 3-cloro-4-(diclorometil)-5-hidróxi-2(5H)-furanona (MX) em amostras de água. Foram usadas fibras de diferentes polaridades empregando a amostragem por imersão e por headspace. Para o sistema de imersão, foram avaliados vários parâmetros que afetam a extração de MX, como pH, salinidade, temperatura e tempo de extração. O método otimizado (fibra de poliacrilato; 20% Na 2 SO 4 ; pH 2,0; 60 min; 20 °C) foi aplicado para águas cloradas proveniente de reservatórios de abastecimento de água-amostras naturais e amostras com adição de MX (50 ng L -1 e 100 ng L Solid-phase microextraction, using on-line bis(trimethylsilyl)trifluoroacetamide derivatisation, gas chromatography, and mass spectrometry, was evaluated in the quantification of 3-chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone (MX) in water samples. Fibres encompassing a wide range of polarities were used with headspace and direct immersion sampling. For the immersion procedure, various parameters affecting MX extraction, including pH, salinity, temperature, and extraction time were evaluated. The optimised method (polyacrylate fibre; 20% Na 2 SO 4 ; pH 2.0; 60 min; 20 °C) was applied for reservoir chlorinated water samples-either natural or spiked with MX (50 ng L -1 and 100 ng L -1 ). The recovery of MX ranged from 44 to 72%. Quantification of MX in water samples was done using external standard and the selected ion monitoring mode. Correlation coefficient (0.98%), relative standard deviation (5%), limit of detection (30 ng L -1 ) and limit of quantification (50 ng L -1 ) were obtained from calibration curve.

Effects of coagulation on the removal of natural organic matter, genotoxicity, and precursors to halogenated furanones

“…The pH dependent cyclization properties of MX analogues can be used advantageously during the detection of halogenated furanones. Onstad et al (2008) used concentration summations of similar analogues to track the formation and removal of halogenated furanones: Rezemini et al (2008) reported the relevance of an acidification step for studies on the health effects of MX, since the pH of gastric fluid is approximately 1.2 and thus the closed MX form is assumed to be predominant in the human body.…”

Environmental Mass Spectrometry: Emerging Contaminants and Current Issues

“…The trifluoroacylated MX was shown to be stable for 30 days in an excess of the derivatization reagent, and this method was used to measure MX in several drinking water samples, where it was detected up to 517 ng/L. Rezemini et al used SPME with online bis(trimethylsilyl)trifluoroacetamide derivatization-GC/MS to measure MX in drinking water (142). The recovery of MX ranged from 44 to 72%, and limits of detection of 30 ng/L were achieved.…”