Artigo Revisado por pares

A quick, easy, cheap, effective, rugged and safe extraction method followed by liquid chromatography-(Orbitrap) high resolution mass spectrometry to determine benzotriazole, benzothiazole and benzenesulfonamide derivates in sewage sludge

2014; Elsevier BV; Volume: 1339; Linguagem: Inglês

10.1016/j.chroma.2014.02.081

ISSN

1873-3778

Autores

Pol Herrero, Francesc Borrull, Eva Pocurull, Rosa María Marcé,

Tópico(s)

Analytical chemistry methods development

Resumo

A Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction method followed by liquid chromatography-(Orbitrap) high resolution mass spectrometry was developed for the simultaneous determination of five benzotriazole, four benzothiazole and five benzenesulfonamide derivates in sewage sludge. While the method was being developed, several buffers and dispersive solid-phase extraction clean-up (dSPE) sorbents were tested. Citrate buffer and Z-sep+ (zirconium-based sorbent) were the most effective extraction buffer and dSPE clean-up material. The absolute recoveries were higher than 80% for all compounds (100ng/g (d.w.)) and the matrix effect was less than -20% for most compounds. The limits of detection were between 0.5 and 10ng/g (d.w.) and the limits of quantification (LOQ) were between 1 and 25ng/g (d.w.). Repeatability and reproducibility were lower than 15% (%RSD, n=5). Several sludge samples from five sewage treatment plants in Catalonia were analysed and the most abundant compounds were 2-hydroxybenzothiazole (<LOQ-181.2ng/g (d.w.)) and 4-methyl-1-H-benzotriazole (<LOQ-82.3ng/g (d.w.)). Benzenesulfonamide (n.d.-70.2ng/g (d.w.)) and toluenesulfonamide (n.d.-83.9ng/g (d.w.)) were also determined.

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