Analytica chimica acta · 2025
Matrix solid-phase dispersion, combined with online SPE-LC-MS/MS, for the determination of tetracyclines and their main transformation products in sludge and agricultural soils.
СтатьяПоддержка исследования: вне правительства СШАНазвание и аннотация: Перевод в очереди
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García-Criado Noelia, Martín Julia, Santos Juan Luis, Aparicio Irene, Alonso Esteban
Аннотация
BACKGROUND: Tetracyclines are frequently detected in the environment due to their persistence and extensive use as antibiotics in human and veterinary medicine. They can accumulate in sludge and in agricultural soils fertilised with treated sludge or manure. This behaviour may lead to ecological risk, propagation of antibiotic resistance and can affect crops and human health through the consumption of vegetables and fruits. Analytical methods for the determination of tetracyclines and their transformation products (TPs) in sludge and agricultural soils are scarce, include a small number of tetracyclines, do not include their TPs and are not specifically developed for their determination.
RESULTS: A matrix solid-phase dispersion (MSPD) method has been optimised for the simultaneous determination of six tetracyclines and six of their main TPs in the types of sludge applied as soil fertiliser (digested sludge and composted sludge) and in agricultural soil. Analytical determination by online SPE-LC-MS/MS has also been optimised. The method was validated for each of the above-mentioned matrices, with good linearity (R2 ≥ 0.98), precision (RSD ≤12.3 %), accuracy (64-117 %) and method quantification limits (below 10 ng g-1 dry weight (dw) for most compounds). Application of the method to digested sludge, composted sludge and agricultural soils revealed high concentrations not only of the parent compounds (tetracycline and doxycycline, up to 353 ng g-1 dw and 1069 ng g-1 dw, respectively, in digested sludge) but also of their TPs (epitetracycline, anhydrotetracycline and 4-epioxytetracycline up to 327 ng g-1 dw, 117 ng g-1 dw and 10.2 ng g-1 dw, respectively, in digested sludge).
SIGNIFICANCE AND NOVELTY: This method allows the specific simultaneous determination of six tetracyclines and six of their TPs in sludge and soils. The proposed method constitutes a starting point to extend the use of MSPD, that is being applied mainly to biota and food, as a low-cost and easy-to-perform technique that allows simultaneous extraction and clean-up. Application of the method revealed the significance of the determination of TPs of tetracyclines for a proper environmental risk assessment.
RESULTS: A matrix solid-phase dispersion (MSPD) method has been optimised for the simultaneous determination of six tetracyclines and six of their main TPs in the types of sludge applied as soil fertiliser (digested sludge and composted sludge) and in agricultural soil. Analytical determination by online SPE-LC-MS/MS has also been optimised. The method was validated for each of the above-mentioned matrices, with good linearity (R2 ≥ 0.98), precision (RSD ≤12.3 %), accuracy (64-117 %) and method quantification limits (below 10 ng g-1 dry weight (dw) for most compounds). Application of the method to digested sludge, composted sludge and agricultural soils revealed high concentrations not only of the parent compounds (tetracycline and doxycycline, up to 353 ng g-1 dw and 1069 ng g-1 dw, respectively, in digested sludge) but also of their TPs (epitetracycline, anhydrotetracycline and 4-epioxytetracycline up to 327 ng g-1 dw, 117 ng g-1 dw and 10.2 ng g-1 dw, respectively, in digested sludge).
SIGNIFICANCE AND NOVELTY: This method allows the specific simultaneous determination of six tetracyclines and six of their TPs in sludge and soils. The proposed method constitutes a starting point to extend the use of MSPD, that is being applied mainly to biota and food, as a low-cost and easy-to-perform technique that allows simultaneous extraction and clean-up. Application of the method revealed the significance of the determination of TPs of tetracyclines for a proper environmental risk assessment.