Determination of pesticides in sewage sludge from an agro-food industry using QuEChERS extraction followed by analysis with liquid chromatography-tandem mass spectrometry.

An analytical method was developed and validated for the determination of ten pesticides in sewage sludge coming from an agro-food industry. The method was based on the application of Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction for solid sewage sludge and SPE extraction for sludge aqueous phase, followed by liquid chromatography (LC) coupled to hybrid quadrupole/linear ion trap mass spectrometry (QqLIT-MS). The QuEChERS method was reported 14 years ago and nowadays is mainly applied to the analysis of pesticides in food. More recent applications have been reported in other matrices as sewage sludge, but the complexity of the matrix makes necessary the optimization of the cleanup step to improve the efficiency of the analysis. With this aim, several dispersive solid-phase extraction cleanup sorbents were tested, choosing C18 + PSA as a d-SPE sorbent. The proposed method was satisfactorily validated for most compounds investigated, showing recoveries higher than 80% in most cases, with the only exception of prochloraz (71%) at low concentration level. Limits of quantification were lower than 40 ng l-1 in the aqueous phase and below 40 ng g-1 in the solid phase for the majority of the analytes. The method was applied to solid sludge and the sludge aqueous phase coming from an agro-food industry which processes fruits and vegetables. Graphical abstract Application of LC/MS/MS advanced analytical techniques for determination of pesticides contained in sewage sludge.

Degradation and monitoring of acetamiprid, thiabendazole and their transformation products in an agro-food industry effluent during solar photo-Fenton treatment in a raceway pond reactor.

In this study, pesticides acetamiprid and thiabendazole and their transformation products (TPs), seven from each pesticide, were successfully monitored during solar photo-Fenton treatment in a real secondary effluent from an agro-food industry spiked with 100µgL(-1) of each pesticide. To this end, a highly sensitive procedure was developed, based on liquid chromatography (LC) coupled to hybrid quadrupole-linear ion trap mass spectrometry (QqLIT-MS). In addition, finding low-cost and operational technology for the application of AOPs would then facilitate their use on a commercial level. Simple and extensive photoreactors such as raceway pond reactors (RPRs) are therefore proposed as an alternative for the application of solar photo-Fenton. Results showed that high degradation could be achieved in a complex water matrix (>99% TBZ and 91% ACTM in 240min) using a 120-L RPR pilot plant as novel technology. The analyses indicated that after the treatment only three TPs from ACTM were still present in the effluent, while the others had been removed. The study showed that the goal of either just removing the parent compounds, or going one step further and removing all the TPs, can significantly change the treatment time, which would affect process costs.