Environmental Laboratory


31


Figure 2. Absolute recoveries for each target analyte (n=4) after performing QuEChERS-SPE or FUSLE-SPE extraction.


For this purpose, the effectiveness of two extraction techniques (i.e., focused ultrasound solid-liquid extraction (FUSLE) and QuEChERS was evaluated and the clean-up step using solid phase extraction (SPE) was also thoroughly studied (Figure 2).


The method was successfully validated at 10 μg·kg-1 and 50 μg·kg-1


(0.45 to 7.50 μg·kg-1 (27.1 ± 1.4 µg·kg-1 , 25 μg·kg-1 showing adequate trueness (70-130 %) and


repeatability (RSD<30 %), with few exceptions. Procedural limits of quantifi cation (LOQPRO


) were determined for soil:compost ) and manure (0.31 to 5.53 μg·kg-1


. Sulfamethazine (7.9 ± 0.8 µg·kg-1 ) and trimethoprim (4.9 ± 0.5 µg·kg-1 ) samples.


Pefl oxacin could not be validated at the lowest level since LOQPRO ≥ 10 μg·kg-1


), danofl oxacin ) were


detected in soil samples; and tetracycline (56.8 ± 2.8 µg·kg-1 ),


among other AMs, in the plants grown on the surface of the studied soil samples. Similarly, SAs, TCs and fl uoroquinolones (FQs) were detected in sheep manure in a range of (1.7± 0.3) - (93.3± 6.8) µg·kg-1


REFERENCES


Hang, L., Zhao, Y., Liu, C., Yu, Y., He, Y., Xu, J., & Lu, Z. (2021). Determine Multiple Classes of Veterinary Antibiotics in Soil: Comparing Dispersive and Solid-Phase Extraction for Sample Cleanup. Chromatographia, 84(9), 833-844. https://doi. org/10.1007/s10337-021-04064-5 Jadeja, N. B., & Worrich, A. (2022). From gut to mud: Dissemination of antimicrobial resistance between animal and agricultural niches. Environmental Microbiology, 24(8), 3290-3306. https://doi. org/10.1111/1462-2920.15927


Kang, D. H., Gupta, S., Rosen, C., Fritz, V., Singh, A., Chander, Y., Murray, H., & Rohwer, C. (2013). Antibiotic Uptake by Vegetable Crops from Manure-Applied Soils. Journal of Agricultural and Food Chemistry, 61(42), 9992-10001.


. Soil and manure samples were also analysed


through UHPLC coupled to a high-resolution mass-spectrometer (UHPLC-qOrbitrap) in order to extent the multitarget method to suspect screening of more than 22,281 suspects. A specifi c transformation product (TP) of sulfamethazine (formyl- sulfamethazine) (Figure 3) was annotated at 2a level in manure samples, among others.


https://doi.org/10.1021/jf404045m Vergara-Luis, I., Báez-Millán, J. C., Baciero, I., González-Gaya, B., Olivares, M., Zuloaga, O., & Prieto, A. (2023). Comparison of conventional and dispersive solid phase extraction clean-up approaches for the simultaneous analysis of tetracyclines and sulfonamides in a variety of fresh vegetables. Talanta, 254, 124192. https://doi.org/10.1016/j.talanta.2022.124192


Vergara-Luis, I., Bocayá, N., Irazola-Duñabeitia, M., Zuloaga, O., Lacuesta, M., Olivares, M., & Prieto, A. (2023). Multitarget and suspect screening of antimicrobials in soil and manure by means of QuEChERS — liquid chromatography tandem mass spectrometry. Analytical and Bioanalytical Chemistry, 415, 6291-6310.


Author Contact Details I. Vergara-Luisa,b*


I. Vergara-Luis, chemist and pre-doctoral researcher in environmental contamination and toxicology in the IBeA (Ikerkuntza eta Berrikuntza Analitikoa) research group at the University of the Basque Country.


https://doi.org/10.1007/s00216-023-04905-2


Zalewska, M., Błażejewska, A., Czapko, A., & Popowska, M. (2021). Antibiotics and Antibiotic


Resistance Genes in Animal Manure – Consequences of Its Application in Agriculture. Frontiers in Microbiology, 12, 610656. https://doi.org/10.3389/fmicb.2021.610656


, N. Bocayáa


, J.C. Baez Millána


, M. Irazola-Duñabeitiaa,b Figure 3. Chemical structure of the identifi ed TP, formyl-sulfamethazine.


This work contributes to the efforts that have been made in the last decade to develop analytical methods that allow multitarget analysis of a wide variety of AMs, including TPs, in complex environmental matrices, which is a complex task due to the diverse physicochemical properties of the AMs. Furthermore, the results of this work not only demonstrated the presence of AMs in the environment and the transference of these pharmaceuticals in the manure-soil-plant/vegetable chain, which puts pressure on bacteria to create resistance, but also showed the presence of their TPs, the effects of which are still unknown.


a. Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/ EHU), Leioa, Basque Country, Spain b. Research Centre for Experimental Marine Biology and Biotechnology (PIE), University of the Basque Country (UPV/EHU), Plentzia, Basque Country, Spain


c. Department of Plant Biology and Ecology, Faculty of Pharmacy, University of the Basque Country (UPV/EHU), Vitoria-Gasteiz, Basque Country, Spain


*Corresponding author at the Department of Analytical Chemistry, Faculty of Science and Technology, 48490 Leioa, Basque Country, Spain E-mail address: irantzu.vergara@ehu. eus (I. Vergara-Luis).


I.Vergara N.Bocayá J.C.Baez Millán


, M. Lacuestac


, M.Olivaresa,b,


A. Prietoa,b


M.Irazola


M.Lacuesta


M.Olivares


A.Prieto


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