A quartz crystal microbalance-based biosensor for the specific detection of the first transgenic common bean (L.) cultivar (BRS FC401 RMD) with resistance to Bean golden mosaic virus (BGMV) was developed. The immobilization chemistry relies on the strong bond between the thiolated probe and the gold electrode surface. The probe sequence is internal to a region of the BGMV rep gene that was introduced into the common bean genome. The sensor’s analytical performance was determined using synthetic oligonucleotides. Real samples of transgenic and wild-type bean seeds were also tested. Sample pretreatment consisted only of enzymatic fragmentation, followed by a thermal denaturation step combined with blocking oligonucleotides. Different biosensor regeneration approaches were studied. Immobilization showed good reproducibility (CV% of 5.8%). The biosensor proved specific for both synthetic oligonucleotides and non-amplified genomic DNA. A linear detection range of 0–1.4 ng/µL was observed, with a detection limit of 0.18 ng/µL. Three sequential detections were performed without loss of surface activity. The results demonstrate the biosensor’s potential for direct, real-time, label-free detection of DNA samples for field screening of transgenic common bean cultivars.

Natural deep eutectic solvents (NADES) offer sustainable alternatives to conventional solvents for plant extraction, yet their influence on extract composition and bioactivity preservation requires further study. Here, choline chloride-based NADES with lactic acid or propylene glycol were evaluated for ultrasound-assisted extraction (60 °C, 30 min, 1:20 w/v) of polyphenol-rich fractions from Sanguisorba officinalis and Symphytum officinale. Spectrophotometric analysis yielded total phenolic contents of 6.49–9.67 mg GAE g−1 and total flavonoids of 0.08–0.52 mg g−1, with values dependent on the plant matrix and the NADES formulation. Targeted HPLC-MS/MS enabled identification of representative phenolic acids (chlorogenic, caffeic, ferulic, rosmarinic) and flavonoid markers (rutin, quercetin derivatives), showing qualitative differences in the detected marker profiles between solvents and matrices. Functional assays demonstrated pronounced antioxidant-related effects, including DPPH radical scavenging at 0.5–25 µg mL−1 (polyphenols), inhibition of lipid peroxidation in rat erythrocytes at 0.25–1.20 µg mL−1, and modulation of mitochondrial respiration and permeability transition in isolated rat liver mitochondria. Overall, the results indicate that choline chloride-based NADES can be used to obtain polyphenol-rich plant extracts compatible with the applied analytical workflow while preserving redox-active fractions, supporting their utility in green analytical sample preparation.

High-resolution mass spectrometry (HRMS) enables non-targeted detection of drugs and metabolites in complex matrices. Phase II metabolites—especially glucuronides—are often the only detectable biomarkers in late or postmortem samples but are underrepresented in commercial libraries. This work pursued the prediction of phase II-glucuronide conjugates in diluted urine samples by non-targeted/targeted LC-HRMS workflows. A simply “dilute-and-shoot” qualitative UHPLC-HRMS/MS method (Q Exactive HF, ddMS2) was integrated with Compound Discoverer® software for data processing. The workflow incorporated predictive strategies such as exact mass suspect lists, Structured Query Language (SQL)-based filters, compound-class and diagnostic neutral-loss rules (including the characteristic loss of 176.0321 Da for glucuronides) and MS/MS confirmation using both in-house and public spectral libraries. An additional part of the application’s performance assessment involved its validation for diluted urine sample. A qualitative validated method for more than two hundred drugs in urine samples was performed, including the method’s selectivity/specificity, limit of identification, matrix effects, and potential carryover. Most analytes fulfilled the qualitative acceptance criteria, with more than 60% successfully identified at a concentration of at least 2.5 ng/mL. Matrix effects were within acceptable limits for most compounds, and no severe ion suppression was observed. A non-targeted workflow was applied to real forensic samples (n = 16), allowing a reduction of approximately 66,800 detected features to 225 glucuronide candidates, while a targeted workflow based on exact mass lists yielded 31 high-confidence identifications. Characteristic neutral losses and diagnostic fragment ions led to the tentative identification of some glucuronide phase II metabolites such as mirtazapine–glucuronide, morphine-6–glucuronide, and glucuronide conjugates of benzodiazepines and synthetic opioids. In conclusion, the integration of biotransformation knowledge with HRMS-based predictive filtering allows for the efficient and hydrolysis-free detection of glucuronide metabolites, thereby extending detection windows and enhancing toxicological interpretation in complex forensic scenarios. This adaptable and library-independent workflow also facilitates retrospective data mining, making it suitable for the identification of emerging substances and newly characterized metabolites.

Taraxacum mirabile Wagenitz, one of the endemic riches of Anatolia, is a species that has remained largely unexplored regarding its enzyme inhibition profile despite its pharmacological potential. The effects of T. mirabile aerial and root extracts, obtained at different polarities, were scrutinized in this study against two important enzymes: lactoperoxidase (LPO), which plays a vital role in the innate immune system, and xanthine oxidase (XO), which is prominently associated with hyperuricemia and oxidative stress. The aerial and root portions of the plant were extracted into fractions of varying polarities using petroleum ether, dichloromethane, ethyl acetate, and butanol. LPO was isolated from buffalo milk (881.6-fold purification, 22.5% yield, and 1249.9 EU/mg specific activity) via affinity chromatography and used in in vitro inhibition assays alongside commercial bovine XO enzyme. The results showed that the ethyl acetate fraction of the aerial part of the plant exhibited the strongest LPO inhibition (IC50: 15.60 ± 0.77 µg/mL) among the fractions. The petroleum ether fraction of both the aerial part (IC50: 11.17 ± 0.94 µg/mL) and the root part (IC50: 11.61 ± 0.59 µg/mL) had the highest inhibitory effect for the XO enzyme. These distinct inhibition profiles allow for significant insights into how plant extracts with varying polarities modulate XO and LPO enzymes. In conclusion, the significant inhibitory activity of T. mirabile extracts toward LPO and XO enzymes highlights their potential as a natural source for developing effective enzyme inhibitors, which could be useful for therapeutic applications.

A simple mechanical polishing treatment of commercial solid-gold electrodes (SGEs) can renew the active gold surface, reduce manufacturing-related grooves, and markedly improve the repeatability of geometric-area estimation and the analytical performance in stripping voltammetry. The work focuses on the accurate determination of the geometric area of a SGE by two voltammetric techniques. Cyclic voltammetry (CV) at different scan rates, referred to as the Randles–Ševčik equation, and voltage scans at different electrode rotation rates, based on the Levich equation, were performed. The geometric area of the SGE was also evaluated by scanning electron microscopy (SEM). Commercial SGEs show grooves on their surface, derived from the fabrication processes. The effects of these grooves on the voltammetric response were investigated. The measurements were carried out on the SGE both as received from the manufacturer and after a reduction in the grooves height by a drastic mechanical treatment. After the treatment, the estimated area values were lower and more precise (3.05 ± 0.02 mm2). Moreover, the reduction in the grooves’ height affected the area estimations in contrast with the meaning of the geometric area, as intended by the Randles–Ševčik and Levich equations. Furthermore, the gold exposed surface was measured by CV in sulphuric acid. Finally, the SGE was tested for the detection of Hg in a NaCl solution by anodic stripping voltammetry: the repeatability of the response improved after the mechanical treatment, confirming the usefulness of this step before electrode usage.

The primary objective of the current study is to establish and validate for the first time a method to determine and quantify praziquantel (PZQ) and its main degradation products loaded in poly(methyl methacrylate–co-2-(diethylamino)ethyl methacrylate) P(MMA-co-DEAEMA) microparticles. A high-performance liquid chromatography (HPLC) approach was developed and validated in accordance with the United States Pharmacopeia (USP) guidelines, addressing parameters such as accuracy, linearity, solution stability, precision, specificity, robustness, sensitivity, and system suitability. The method employed a gradient mobile phase consisting of ultrapure water and acetonitrile, flowing at a rate of 1 mL/minute over a Phenomenex Kinetex® C18 column (5 µm, 100 Å, 250 × 4.6 mm) maintained at 35 °C. Detection was performed at the wavelength of 210 nm using a DAD/UV detector. Samples of the active pharmaceutical ingredient (API) praziquantel, microencapsulated praziquantel, placebo, and a mixture of related substances (A, B, and C) were prepared with 0.5% formic acid in water/ethanol, 45:55 v/v as the diluent, and injected at 20 °C. The method demonstrated a limit of quantification (LOQ) of 0.20 µg/mL for praziquantel and related substances. The method exhibited an excellent linear response, with all correlation coefficients (R2) values exceeding 0.998, which is well above the recommended specified limit of R2 > 0.995. Percent recoveries fell within the acceptable range of (95.0–105.0%), and all results indicated a percentage of relative standard deviation (%RSD) ≤ 2.0, indicating a robust methodology. Thus, the proposed HPLC technique proved to be selective, accurate, sensitive, and consistent in analyzing both the material content and its main degradation products.

In the context of the energy transition and the increasing deployment of low-carbon gases (hydrogen, biomethane), reliable analytical monitoring is required to support integrity assessment and traceability of gas infrastructures under diverse on-site conditions while limiting analytical costs through standardized sampling and a single analytical system. We developed and validated integrated workflows combining sampling and laboratory analysis for chemical and compound-specific isotope analysis (CSIA) of natural gas and associated gaseous effluents in underground storage. An original quantification approach was implemented, linking sampling pressure to the amount of each compound collected in vials, and coupled with δ13C and δ2H measurements of alkanes (C1–C3), CO2 and H2. Two complementary sampling modes were optimized and compared: conventional high-pressure cylinders and direct collection into vacuum-sealed vials suitable for a broad range of pressures and field conditions. Using reference gas mixtures and operational samples, both approaches showed good reproducibility and isotopic accuracy during laboratory validation and over two years of monitoring. In particular, δ2H determinations for alkanes and H2 remained robust under low-pressure sampling typical of annular spaces (~1–2 bar), despite gas-composition fluctuations. These validated methodologies provide a flexible basis for routine, standardized monitoring of stored and circulating gases, including emerging low-carbon components.

The rapid growth and diversification of the cosmetic industry have led to increasingly complex formulations containing numerous bioactive ingredients, excipients, and synthetic additives, often delivered through advanced nanostructured systems. Ensuring product safety, efficacy, and regulatory compliance requires analytical approaches capable of accurately detecting both declared components and hazardous contaminants such as heavy metals, phthalates, nitrosamines, and banned preservatives or dyes. Traditional sample preparation methods are often solvent-intensive, time-consuming, and environmentally burdensome, prompting a shift toward green microextraction strategies aligned with the principles of green analytical chemistry. Techniques including solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE), and dispersive liquid–liquid microextraction (DLLME) offer miniaturized, solvent-efficient workflows with improved selectivity and sensitivity for complex cosmetic matrices. This review summarizes advances from the past five years in green microextraction methods for the determination of organic and inorganic species in cosmetic products. Emphasis is placed on their integration with separation techniques and applicability across product categories. Emerging trends, analytical challenges, and future directions toward more sustainable cosmetic safety assessment are also highlighted.

Molting is an important biological and physiological stage in penguins, influenced by environmental and nutritional factors. Feather composition analysis before and after molting can consequently place boundaries on element bioaccumulation and excretion. We quantified and compared elemental concentrations in African penguin (Spheniscus demersus) feathers collected pre- and post-molt across three zoos to evaluate how molt stage and zoo-specific conditions influence feather elemental composition. Feathers were retrieved from individual penguins at Zoom Torino (Italy), Overloon ZooParc (Netherlands), and Zoo Magdeburg (Germany). Quantification of elemental concentrations were performed by analytical methods, with both ICP-OES and HR-ICP-MS techniques. A statistical approach involving MANOVA and factorial analysis helped identify important trends. Pre-molt features had more variability than post-molt, with both showing significant differences in elemental concentrations. Factorial analysis showed geogenic trends in Mg, Sr, and Ni trends as well as anthropogenic trends in Pb. While Na and K differed among all treatment groups, this likely points to physiological adaptations in response to increased demand during feather regrowth. Additionally, inter-zoo comparisons highlighted distinct elemental profiles linked to local environmental and dietary conditions, particularly in Zoo Magdeburg, where Na levels were markedly elevated. This study highlights the influence of environmental and dietary conditions on feather composition during molt, offering insights for improving captive penguin welfare and broader ecological implications related to climate change and pollution.

Oats (Avena sativa L.) are a rich source of β-d-glucans, dietary fibre, proteins, and lipids. However, the behaviour of these components in wheat–oat composite systems during baking, particularly with regard to matrix-dependent analytical responses, remains unclear. This study evaluated the compositional changes, technological performance, and sensory quality of wheat bread enriched with various forms of oat. Composite flours containing 5–15% wholegrain oat flour, commercial oat bran, milled commercial oat flakes, or milled sprouted oat grain (sprouted under laboratory conditions for three days at 25 °C) were prepared using the Slovakian oat cultivar ‘Peter’. The raw materials, flour blends, and baked breads were analysed for β-d-glucans (BG), total dietary fibre (TDF), starch, proteins, and lipids using standardised enzymatic, gravimetric, and polarimetric methods. Bread quality was assessed through loaf volume measurements and a sensory evaluation using a 5-point hedonic scale by seven trained panellists. Multivariate statistical analysis was applied to integrate compositional, technological, and sensory data. Compared to wheat flour (0.24% BG and 3.45% TDF), the incorporation of oats significantly increased the contents of BG, TDF, proteins, and lipids, with oat bran showing the strongest enrichment effect (owing to 15.69% TDF in the raw material). Baking induced oat-form-dependent changes in the measured BG and TDF content. The level of BG diminished in wholegrain oat blends but increased or remained stable in bran-rich systems. This reflects differences in matrix structure and analytical extractability, rather than true compositional gains. Meanwhile, starch content consistently declined across all composite breads. Fibre-rich formulations exhibited reduced loaf volume and altered both bread geometry and morphology, particularly at 15% substitution. Breads containing 5% oat flour or moderate levels of oat bran (5 or 10%) were considered the most acceptable in terms of nutritional enhancement and quality attributes. Germinated oat breads showed the greatest technological impairment and the lowest sensory scores. Overall, moderate oat enrichment strikes a balance between nutritional improvement and technological performance without significantly compromising sensory quality. These findings emphasise the significance of matrix effects when interpreting standard total dietary fibre and β-d-glucans analyses and offer an integrated analytical and technological framework for the rational design of fibre-enriched cereal products.