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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.

Journal of chromatography. A (2014-03-25)
Pol Herrero, Francesc Borrull, Eva Pocurull, Rosa M Marcé
ABSTRACT

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.

MATERIALS
Product Number
Brand
Product Description

Supelco
Supel QuE, Z-Sep+ Bulk, pkg of 20 g
Supelco
Supel QuE, Z-Sep/C18 Tube, centrifuge tube volume 2 mL, pack of 100
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep+ Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep Bulk
Supelco
Supel QuE, Z-Sep+ Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep/C18 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible