title: Fast extraction of polychlorinated dibenzo-p-dioxin and polychlorinated dibenzofuran in sewage sludge and soil samples.
abstract: The current environmental legislations recommend monitoring chemical contaminants such as polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans before the use of sewage sludge on the agricultural land. In this study, a solid-liquid extraction with low-temperature purification (SLE-LTP) was optimized and validated to determine 2,3,7,8-tetrachlorodibenzo-p-dioxin and 2,3,7,8-tetrachlorodibenzofuran in sewage sludge and soil samples. The analyses were performed by gas chromatography-mass spectrometry operating in the selective ion mode (GC-MS-SIM). Acetonitrile:ethyl acetate 6.5:1.5 (v/v) was the best extraction phase, and the recoveries percentages were close to 100%. The linearity was demonstrated in the range of 1.25-25 µg L-1of 1.25-20 µg L-1for sewage sludge and soil, respectively. Matrix effect was proved for the two compounds and in the two matrices studied. Extraction percentages were between 78 and 109% and relative standard deviations ≤ 19%. The proposed method is faster than methods described in the literature because showed a few steps. The quantification limits (LOQ) in sewage sludge were 6.4 and 32 ng TEQ kg-1for 2,3,7,8-TCDF and 2,3,7,8-TCDD, respectively. In soil, LOQs were 0.8 and 8.0 ng TEQ kg-1for 2,3,7,8-TCDF and 2,3,7,8-TCDD, respectively. These values are lower than the maximum residue limits established by European Legislation. The method was applied to 22 agricultural soil samples from different Brazilian cities and 2,3,7,8-TCDF was detected in one of these samples.
authors.affiliation: a Institute of Agricultural Sciences, Federal University of Minas Gerais , Montes Claros , Brazil.
authors.forename: Valéria F
authors.initials: VF
authors.lastname: Andrade
authors.affiliation: a Institute of Agricultural Sciences, Federal University of Minas Gerais , Montes Claros , Brazil.
authors.forename: Alisson F S
authors.initials: AF
authors.lastname: Durães
authors.affiliation: a Institute of Agricultural Sciences, Federal University of Minas Gerais , Montes Claros , Brazil.
authors.forename: Douglas L
authors.initials: DL
authors.lastname: Cassimiro
authors.affiliation: a Institute of Agricultural Sciences, Federal University of Minas Gerais , Montes Claros , Brazil.
authors.forename: Gevany P
authors.initials: GP
authors.lastname: de Pinho
authors.affiliation: a Institute of Agricultural Sciences, Federal University of Minas Gerais , Montes Claros , Brazil.
authors.forename: Flaviano O
authors.initials: FO
authors.lastname: Silvério
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D000383:Agriculture; D001572:Benzofurans / Q000302:isolation & purification; D001938:Brazil; D005591:Chemical Fractionation / Q000379:methods*; D002947:Cities; D000072338:Dibenzofurans, Polychlorinated / Q000302:isolation & purification*; D004784:Environmental Monitoring / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D057230:Limit of Detection; D000072317:Polychlorinated Dibenzodioxins / Q000302:isolation & purification*; D012722:Sewage / Q000737:chemistry*; D012989:Soil Pollutants / Q000302:isolation & purification
chemical_list: D000097:Acetonitriles; D001572:Benzofurans; D000072338:Dibenzofurans, Polychlorinated; D000072317:Polychlorinated Dibenzodioxins; D012722:Sewage; D012989:Soil Pollutants; C014211:2,3,7,8-tetrachlorodibenzofuran; C032159:acetonitrile
keywords: Biosolids; SLE-LTP; dioxins and furans