Two different zinc-based metal-organic frameworks (MOFs) were investigated to remove one of the most used fluoroquinolone antibiotic, Ofloxacin (OFL), from polluted water. The most common zeolitic imidazolate framework-8 (ZIF-8) and the green Zn(II) and benzene-1,3,5-tri-carboxylate (Zn₃(BTC)₂) were prepared through a facile synthetic route and characterized by means of Fourier-Transform Infrared (FT-IR) Spectroscopy, X-ray Powder Diffraction (XRPD), and Scanning Electron Microscopy (SEM) analyses. The two MOFs were compared in terms of both adsorption and kinetic aspects under real conditions (tap water, natural pH). Results showed that OFL was adsorbed in remarkable amounts, 95 ± 10 and 25.3 ± 0.8 mg g⁻¹ on ZIF-8 and Zn₃(BTC)₂, respectively, following different mechanisms. Specifically, a Langmuir model well described the ZIF-8 profile, while for Zn₃(BTC)₂, cooperative adsorption occurred. Moreover the kinetic results were quite different, pseudo-second-order and sigmoidal, respectively. The suitability of ZIF-8 and Zn₃(BTC)₂ as adsorbent phases for water depollution was tested on tap water samples spiked with OFL 10 µg L⁻¹. The obtained removal efficiencies, of 88% for ZIF-8 and 72% for Zn₃(BTC)₂, make these materials promising candidates for removing fluoroquinolone antibiotics (FQs) from polluted waters, notwithstanding their limited reusability in tap water, as demonstrated by in-depth characterization of the two MOFs after usage.

In this work, red mud (RM) and spinel iron oxide nanoparticles (SPIONs) were added to pure silica/alumina sources (SAs) and fly ash (FA) with the aim of synthesizing and investigating the magnetic behavior of different zeolites. SAs were used to synthesize zeolite with LTA topology (zeolite A) with the addition of both red mud and spinel iron oxide nanoparticles. FA and RM were mixed to synthesize sodalite whereas only FA with the addition of SPIONs was used to form zeolite with FAU-topology (zeolite X). All the synthetic products showed magnetic properties. However, zeolites with spinel iron oxide nanoparticles (zeolites A and X) showed ferromagnetic-like behavior. Sodalite was characterized by a reduction in saturation magnetization, whereas zeolite A with red mud displayed antiferromagnetic behavior. For the first time, all the synthetic products were tested for polluted water remediation by a persistent emerging contaminant, ofloxacin (OFL) antibiotic. The four zeolite types showed good adsorption affinity towards OFL under actual conditions (tap water, natural pH). All materials were also tested for OFL removal in real waters spiked with OFL 10 µg L⁻¹. Satisfactory recoveries (90–92% in tap water, 83–87% in river water) were obtained for the two zeolites synthesized from industrial waste materials.

Given the growing interest in studying the role of choline and phosphocholine in the development and progression of tumor pathology, in this study we describe the development and validation of a fast and robust method for the simultaneous analysis of choline and phosphocholine in human plasma. Choline and phosphocholine quantification in human plasma was obtained using a hydrophilic interaction liquid chromatography–tandem mass spectrometry technique. Assay performance parameters were evaluated using EMA guidelines. Calibration curve ranged from 0.60 to 38.40 μmol/L (R² = 0.999) and 0.08–5.43 μmol/L (R² = 0.998) for choline and phosphocholine, respectively. The Limit Of Detection of the method was 0.06 μmol/L for choline and 0.04 μmol/L for phosphocholine. The coefficient of variation range for intra-assay precision is 2.2–4.1 % (choline) and 3.2–15 % (phosphocholine), and the inter-assay precision range is < 1–6.5 % (choline) and 6.2–20 % (phosphocholine). The accuracy of the method was below the ±20 % benchmarks at all the metabolites concentration levels. In-house plasma pool of apparently healthy adults was tested, and a mean concentration of 15.97 μmol/L for Choline and 0.34 μmol/L for Phosphocholine was quantified. The developed method shows good reliability in quantifying Choline and Phosphocholine in human plasma for clinical purposes.

Untargeted metabolomics faces significant challenges in standardization due to variability introduced by sample preparation and analytical workflows. We systematically evaluated the impact of biological matrices, extraction protocols, and chromatographic configurations to establish a mechanism-informed framework aimed at improving reproducibility in large-scale clinical and epidemiological studies. Three extraction protocols were compared using an in-house pooled heparin plasma: monophasic protein precipitation with isopropanol (IPA), methanol:acetonitrile (MeOH:ACN), and a modified Matyash biphasic method. The most reproducible protocol was then applied to four blood matrices. Samples were analysed using untargeted metabolomics on hydrophilic interaction liquid chromatography (HILIC) and reversed-phase (RP) HPLC columns, with mass spectrometry data processed using Compound Discoverer. Both IPA and MeOH:ACN extractions achieved over 80% of features with coefficient of variation (CV%) ≤ 30% for both RP and HILIC, whereas the Matyash method showed higher variability, with a larger proportion of metabolites exhibiting CV% > 30%. Across matrices, RP chromatography detected over 80% of metabolites with CV% < 30%, while HILIC showed higher variability, with at least 20% of metabolites above this threshold. Among matrices, serum and heparin plasma outperformed EDTA and citrate in reproducibility. We propose a standardized workflow in which monophasic extractions combined with RP chromatography maximize reproducibility and metabolite coverage, minimizing methodological artefacts and providing a reliable framework for robust biological discovery in large-scale untargeted metabolomics studies.

Background: Chronic inflammation from visceral obesity contributes to metabolic disorders and cancer through cytokine imbalance. Accurate cytokine measurement is crucial to understand these links. This study examined challenges in quantifying interleudin-6 (IL-6), tumor necrosis factor-alpha (TNF-α), leptin, and adiponectin in historical biobank samples with limited volumes and varying plasma anticoagulants. Methods: Luminex-MAGPIX platform was used to evaluate three analytical aspects. Single-well precision was assessed via intra- and inter-assay coefficients of variability (CVs). Plasma matrix effects were examined by pairwise comparison of analyte concentrations across citrate, heparin, and EDTA plasma from 10 volunteers. Cytokine stability was tested after one freeze-thaw cycle (analysis of variance). Results: Single-well measurements showed good precision (CV <10% intra-assay, <15% inter-assay). Plasma matrix affected absolute concentrations. In particular, all analytes were lower in citrate than in EDTA and heparin, but relative relationships and subject-specific rankings remained preserved. Pearson correlation coefficients for IL-6, leptin, and adiponectin were high across matrices (r-range = 0.952–0.999), whereas correlations for TNF-α were lower (r-range = 0.897–0.972). Freeze–thaw stability was analyte- and matrix-dependent: leptin remained stable in heparin and EDTA but decreased 9.5% in citrate; adiponectin was stable in citrate but decreased in heparin (−9.0%) and EDTA (−11.8%). IL-6 and TNF-α were unaffected. Conclusion: IL-6, TNF-α, leptin, and adiponectin were accurately quantified using single-well Luminex assays and showed reasonable tolerance to a single freeze–thaw cycle, offering a practical strategy for preserving valuable specimens. Although plasma anticoagulant affected absolute concentrations, the preservation of relative analyte rankings permits their use in most study designs but limit absolute value comparisons.