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

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 (100 ng/g (d.w.)) and the matrix effect was less than −20% for most compounds. The limits of detection were between 0.5 and 10 ng/g (d.w.) and the limits of quantification (LOQ) were between 1 and 25 ng/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-181.2 ng/g (d.w.)) and 4-methyl-1-H-benzotriazole (<LOQ-82.3 ng/g (d.w.)). Benzenesulfonamide (n.d.-70.2 ng/g (d.w.)) and toluenesulfonamide (n.d.-83.9 ng/g (d.w.)) were also determined.