Validation and application of a multiresidue method based on liquid chromatography-tandem mass spectrometry for evaluating the plant uptake of 74 microcontaminants in crops irrigated with treated municipal wastewater.


J Chromatogr A. 2018 Jan 26;1534:10-21. doi: 10.1016/j.chroma.2017.12.037. Epub 2017 Dec 15.

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.

Martínez-Piernas AB, Polo-López MI, Fernández-Ibáñez P, Agüera A.

Author information
1 CIESOL, Joint Centre University of Almería-CIEMAT, Almería, Spain.
2 Plataforma Solar de Almería-CIEMAT, Carretera Senés Km 4, 04200, Tabernas, Almería, Spain.
3 Nanotechnology and Integrated BioEngineering Centre, School of Engineering, University of Ulster, Newtownabbey, Northern Ireland, United Kingdom.
4 CIESOL, Joint Centre University of Almería-CIEMAT, Almería, Spain. Electronic address: This email address is being protected from spambots. You need JavaScript enabled to view it..

Contaminants of emerging concern; Liquid chromatography–mass spectrometry; Plant uptake; QuEChERS; Wastewater irrigation

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