Determination study of contaminants of emerging concern at trace levels in agricultural soil. A pilot study

Abstract

In this study, we aimed to develop and validate a quick, easy, and robust extraction method for the simultaneous determination of 30 organic contaminants of emerging concern (CECs) including some transformation products in soil samples. Three different extraction methods based on an ultrasonic cylindrical probe (UAE), a pressurized liquid extraction (PLE), and a QuEChERS method were compared. Ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry (LC-MS/MS) was used for identification and quantification of the target analytes. A modified QuEChERS method showed the best results in terms of extractability and accuracy. The extraction procedure developed provided adequate extraction performances (70% of the target analytes were recovered within a 70-99% range), with good repeatability and reproducibility (variations below 20%) and great sensitivity (LOQ < 0.1 ng/g in most cases). No matrix effects were observed for 70% of the compounds. Finally, the analytical methodology was applied in a pilot study where agricultural soil was irrigated with reclaimed water spiked with the contaminants under study. Of the 25 CECs added in irrigation water, a total of 13 pesticides and 5 pharmaceutical products were detected at concentration ranges from 0.1 to 1.2 ng/g (d.w) and from 0.1 to 2.0 ng/g (d.w), respectively.