Micro-matrix solid-phase dispersion method for the multiresidue determination of tetracycline antibiotics and their transformation products in radish

Parent tetracyclines and their transformation products can be present in vegetables growth in soils amended with manure, treated sewage sludge, or irrigated with reclaimed urban wastewater. The presence of some tetracycline antibiotics and transformation products is already regulated in foodstuffs o...

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Detalles Bibliográficos
Autores: García-Criado, Noelia, Martín Bueno, Julia, Santos Morcillo, Juan Luis, Aparicio Gómez, Irene, Alonso Álvarez, Esteban
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2026
País:España
Institución:Universidad de Sevilla (US)
Repositorio:idUS. Depósito de Investigación de la Universidad de Sevilla
OAI Identifier:oai:dnet:idus________::3e537d942700c0fb382aa7f71f9ae451
Acceso en línea:https://hdl.handle.net/11441/185113
https://doi.org/10.1016/j.microc.2026.117682
Access Level:acceso abierto
Palabra clave:μ-MSPD
Online SPE
LC-MS/MS
Epimers
Greenness assessment
ComplexGAPI
AGREEprep
Descripción
Sumario:Parent tetracyclines and their transformation products can be present in vegetables growth in soils amended with manure, treated sewage sludge, or irrigated with reclaimed urban wastewater. The presence of some tetracycline antibiotics and transformation products is already regulated in foodstuffs of animal origin but not yet in vegetables. In this paper, an analytical method is proposed for the determination of seven parent tetracycline antibiotics and six transformation products. Selected transformation products correspond to epimers and dehydration products, which have been reported to be the most toxic ones. The proposed method is based on miniaturized matrix solid-phase dispersion (μ-MSPD) method combined with online solid-phase extraction–liquid chromatography–tandem mass spectrometry (online SPE–LC–MS/MS) determination. The method has been validated in radish edible parts (leaves and bulb), to be used for food monitoring, and in roots, to be used in pollutant plant uptake and translocation studies. Proposed method provides MQLs lower than 5ngg⁻¹ dw, accuracy in the range 85–100%, and RSD% lower than 5.5%, for most of the compounds and matrices. Application of the method to radish samples revealed the presence of transformation products of tetracycline antibiotics even in samples where their respective parent compound was not detected. Greenness assessment, using ComplexGAPI and AGREEprep Green Analytical Chemistry metrics, revealed the highest greenness degree of the proposed method in comparison to other methods reported in literature for determination of tetracycline antibiotics in vegetables.