Reuse of treated wastewater for agricultural purposes can mitigate water stress in some regions where the lack of water is an extended problem. However, the environmental long-term consequences of this practice are still unknown. It is demonstrated that using reclaimed water for irrigation lead to accumulation and translocation of some microcontaminants (MCs) in soil and crops. However, so far, only a small group of contaminants has been investigated. This study aims to develop and validate a simple and efficient multiresidue method based on QuEChERs (Quick, Easy, Cheap, Effective and Rugged) extraction coupled to liquid chromatography tandem mass spectrometry (LC-MS/MS). The novelty of the study relays in the large number of MCs analyzed (74), some of them not previously investigated, in three commodities (lettuce, radish and strawberry). Optimized conditions yielded good results for the three commodities under study. Up to 84% of the compounds were recovered within a 70-120% range, with good repeatability (relative standard deviations below 20% in most cases). Method detection (MDLs) and quantification limits (MQLs) ranged from 0.01 to 2 ng/g. The proposed method was successfully applied to assess the potential uptake of MCs by lettuce and radish crops irrigated with wastewater under controlled conditions for 3 and 1.5 months, respectively. 12 compounds were detected in the crops with concentrations ranging from 0.03 to 57.6 ng/g. N-Formyl-4-aminoantipyrine (4FAA) was the most concentrated compound. The application of this method demonstrated for the first time the accumulation of 5 contaminants of emerging concern (CECs) not previously reported: 4FAA, N-Acetyl-4-aminoantipyrine (4AAA), hydrochlorothiazide, mepivacaine and venlafaxine.

Water scarcity is a problem worldwide, affecting specially countries with desert/semi-desert areas and low/irregular rainfall. In this context, reuse of reclaimed wastewater (RWW) for agricultural irrigation is undoubtedly a key strategy to reduce fresh water consumption. It is well-known that current wastewater treatments do not effectively remove organic microcontaminants (OMCs), and research in water analysis of OMCs is extensive. However, the focus on agricultural soils irrigated with RWW as potential recipients of OMCs and potential sources of OMCs to crops is still in their beginnings. This study aims to apply a target and a suspect approach for the multi-residue monitoring of OMCs in agricultural soils and a soilless subtract, both irrigated with RWW for more than ten years. The study involved, firstly, the development and validation of an extraction method for target analysis of 73 OMCs using a QuEChERS-based method and liquid chromatography coupled to quadrupole-linear ion trap mass spectrometry (LC-QqLIT-MS/MS); and secondly, the application of a suspect workflow for the screening of a list of 1300 potential contaminants using LC coupled to quadrupole-time-of-flight MS (LC-QTOF-MS). The results demonstrated the occurrence of 11 OMCs in the agricultural soil samples and 26 in the soilless subtract (0.1-100 ng g, dry weight, d.w.). The suspect analysis leaded to the confirmation of 28 OMCs analytes from the list of candidates. The subsequent combination of both strategies (suspect and target) revealed the presence of 11 new OMCs which were not previously reported. Furthermore, this study presents the first application of a OMCs suspect screening to agricultural soils irrigated with RWW for a long period. These results highlight the importance of monitoring soils with RWW-based irrigation and the application of wide-scope approaches for environmental analysis.

The sunlight/H2O2 process has recently been considered as a sustainable alternative option compared to other solar driven advanced oxidation processes (AOPs) in advanced treatment of municipal wastewater (WW) to be reused for crop irrigation. Accordingly, in this study sunlight/H2O2 was used as disinfection/oxidation treatment for urban WW treatment plant effluent in a compound parabolic collector photoreactor to assess subsequent cross-contamination of lettuce and soil by contaminants of emerging concern (CECs) (determined by QuEChERS extraction and LC-QqLIT-MS/MS analysis) and antibiotic resistant (AR) bacteria after irrigation with treated WW. Three CECs (carbamazepine (CBZ), flumequine (FLU), and thiabendazole (TBZ) at 100 μg L(-1)) and two AR bacterial strains (E. coli and E. faecalis, at 10(5) CFU mL(-1)) were spiked in real WW. A detection limit (DL) of 2 CFU mL(-1) was reached after 120 min of solar exposure for AR E. coli, while AR E. faecalis was more resistant to the disinfection process (240 min to reach DL). CBZ and TBZ were poorly removed after 90 min (12% and 50%, respectively) compared to FLU (94%). Lettuce was irrigated with treated WW for 5 weeks. CBZ and TBZ were accumulated in soil up to 472 ng g(-1) and 256 ng g(-1) and up-taken by lettuce up to 109 and 18 ng g(-1), respectively, when 90 min treated WW was used for irrigation; whereas no bacteria contamination was observed when the bacterial density in treated WW was below the DL. A proper treatment time (>90 min) should be guaranteed in order to avoid the transfer of pathogens from disinfected WW to irrigated crops and soil.

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