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A automated microextraction method based on temperature-responsive deep eutectic solvents (TRDESs) was developed for the determination of synthetic dyes in food samples. The system employs a homogeneous aqueous TRDES solution, composed of lidocaine and heptanoic acid (1:1 mol/mol), which acts both as extraction medium and as a thermally induced phase-separating agent. Upon heating above the lower critical solution temperature, spontaneous phase separation occurs, allowing direct collection of the enriched TRDES phase without centrifugation or manual handling. The entire process from sample introduction to extract collection is integrated into a programmable flow-based platform. The method was optimized and validated for four banned synthetic dyes: Rhodamine 6G, Sudan I, II, and III. Good linearity (0.025-100 mg L^-1), low limits of detection (0.001-0.008 mg L^-1), and high intra-/inter-day precision (RSDs: 2-7 %) were achieved. Real beverage samples were successfully analyzed, and spiked recoveries showed good agreement with a reference DLLME method (relative bias: 1-5 %). All steps were performed without the use of toxic organic solvents or centrifugation. Molecular dynamics simulations confirmed that π-π stacking and van der Waals interactions between rhodamine and lidocaine govern the extraction mechanism. Additionally, the green performance of the method was assessed using AGREEprep and ComplexGAPI, demonstrating high environmental sustainability. Overall, the proposed method offers a robust, automated, and environmentally friendly solution for trace-level screening of banned dyes in complex food matrices.

Complete surgical resection is the cornerstone of therapy for early-stage colorectal cancer. However, accurate intraoperative tumor localization remains a clinical challenge. Targeted fluorescent probes have emerged as effective tools to assist real-time tumor visualization during surgery. EPH-3-DBS is an EphA2-targeted NIR-I/NIR-II fluorescent molecular probe, composed of the novel cyanine-based dye DBS and the high-affinity EphA2-targeting peptide EPH-3. EPH-3-DBS exhibits excellent optical properties and high binding specificity for EphA2-expressing tumors. In vivo imaging demonstrated that EPH-3-DBS selectively accumulates in tumor tissues, whereas the non-targeted DBS shows no significant tumor affinity. Superior imaging performance was observed in both orthotopic colorectal cancer and liver metastasis models. Owing to its high tumor-to-background ratio (TBR>2.0) and prolonged imaging window, EPH-3-DBS holds significant potential for application in fluorescence-guided surgery.

Biosimilars offer safe and effective treatment options for patients with chronic diseases at potentially lower cost while maintaining equivalent safety, efficacy, and quality relative to innovator products. Biologics are structurally complex and sensitive molecules that require extensive physicochemical, structural, and functional characterization to support biosimilarity development and assess interchangeability. This could be done by ensuring biosimilars exhibit structural and functional equivalence to their reference products. In this study, a head-to-head comparative analytical biosimilarity orthogonal protocol was used for the evaluation of critical quality attributes (CQA) that define the performance of etanercept (a fusion protein) biosimilar in comparison to its innovator, with a novel integration of green and white analytical chemistry assessment, to evaluate the sustainability of the used orthogonal biosimilarity protocol. The analytical assessment methods used were based on peptide mapping-reverse phase HPLC, size exclusion HPLC, dynamic light scattering (DLS), reducing and non-reducing Sodium Dodecyl Sulfate-Polyacrylamide Gel Electrophoresis (SDS-PAGE), and reverse phase (RP-HPLC), direct UV spectrophotometry, and Enzyme-Linked Immunosorbent Assay (ELISA) technique were used to determine the content and protein binding activity of both products, respectively. The results obtained from the biosimilarity assessment showed similar profile for both products under normal conditions in terms of peak areas, retention times, apparent molecular weight bands, and binding affinity. The environmental sustainability of the studied protocol was assessed using Green Certificate-modified eco-scale evaluation, Green Analytical Procedure Index (GAPI), and Analytical Greenness metric (AGREE), in addition to the recently developed red, green, and blue 12-mode that was used to evaluate the whiteness features. Ensuring that biosimilarity evaluations meet both regulatory and environmental international standards.

gas/MS is crucial for accurately assessing hydrogen isotope ratios, including tritium (³H), in fields like environmental forensics, nuclear science, and analytical chemistry. To provide a global perspective and experimental demonstration to obtain accurate tritium (³H) ratios, this work combines bibliometric analysis (i.e evaluation of leading countries, research hotspots, interrelationships of keywords), revealing rapid growth in hydrogen isotopes detection methods, while highlighting research gaps and emerging directions in studies focusing on tritium (³H). Additionally, an experimental approach for the analysis of tritium using gas/MS for samples containing hydrogen isotopologues (i.e H₂, HD, D₂ and ³H) was used to determine LOD (i.e 1.3 to 3.6 μmolmol^-1) at 90Pa, and sensitivity in typical complex samples, such as sample X1 and sample X2. X1 had the highest mole fraction of 101.4 mmol mol^-1 of tritium-based species (T₂ and HT), having and the predicted mole fraction of ³H being 76.2 % while X2 showed little isotopic activity, with 0.073 mmol mol^-1 of ³He detected. D₂, DT, and T₂ were all below the detection limits. gas/MS remains a core analytical chemistry approach for hydrogen isotope determination due to its sensitivity, selectivity, and adaptability in various environments. Furthermore, the integration of bibliometric analysis with experimental verification, the work shows a strong link between global research trends to laboratory feasibility, providing a view of current capabilities and future opportunities in hydrogen isotope quantification.

Sulfur-containing compounds (SCCs) play critical roles in physiological and pathological processes, but their abnormal levels are linked to diseases such as cancer and neurodegenerative diseases. Consequently, the development of accurate quantification and discrimination methods for SCCs is of great significance, providing a powerful tool for the early diagnosis of diseases. In the present study, we designed a confinement-enhanced fluorescence strategy utilizing zirconium-layered double hydroxide microspheres (ZrLDHMs) to encapsulate bimetallic AuAg nanoclusters (AuAgNCs), achieving remarkable enhancement in fluorescence properties including emission intensity, quantum yield, and fluorescence lifetime. Capitalizing on the redox activity of 2,6-dichlorophenol indophenol (DCIP) and the reducing ability of SCCs, a novel dual-mode (fluorescence/colorimetry) sensing platform was constructed based on ZrLDHMs@AuAgNCs for rapid SCCs detection. The fabricated sensor exhibited high sensitivity toward five SCCs (GSH, Cys, MPA, Na₂S, and Na₂SO₃). Taking GSH as a representative, the sensor demonstrated limit of detection of 0.64 μM (fluorescence) and 0.09 μM (colorimetry) with a linear range of 2-70 μM at pH 7.0. Furthermore, by leveraging the differences in the reduction capabilities of DCIP among various types of SCCs, different responses are generated on the sensor array, thereby forming "fingerprint" features. Based on the extracted fingerprint features, the sensor array enabled rapid discrimination of multiple SCCs with high specificity. It was successfully applied to discriminate different types of SCCs in real serum and urine samples. Notably, this work not only demonstrates ZrLDHMs as effective confinement matrices for metal nanoclusters fluorescence enhancement, but also establishes a versatile sensing platform for the quantification and discrimination of SCCs, offering a versatile tool for clinical diagnostics.

Cardenolides are steroidal glycosides characterized by structural complexity and both medicinal and ecological relevance, necessitating precise and reliable analytical methods for their detection and quantitation. Although cardenolide MS/MS fragmentation has been extensively studied, no method has previously enabled simultaneous detection and quantitation of all glycosides derived from a given genin. In this study, we developed group-specific MS/MS methods for comprehensive screening of cardenolide glycosides containing 31 distinct genin backbones, i.e. aglycones. Application of these 31 genin-specific methods enabled detection of more than 300 glycosides in 23 plant species, several of which were represented in multiple tissue types. The approach successfully distinguished all genins from each other, including those with identical m/z values at the same time minimizing false positives from structurally related steroids such as bufadienolides and saponins. Method validations demonstrated low limits of detection (LOD) and limits of quantitation (LOQ), where the lowest limit of detection (LLOD) values varied between 1.5 and 74.6 ng/mL, apart from a single outlier exhibiting a substantially higher LLOD. Wide linear ranges were also achieved, with most upper limits of quantitation (ULOQ) between 1 and 5 μg/mL. Matrix effect and repeatability assessments indicated only minor variation for most methods. The genin-specific MS/MS strategy enables rapid, high-throughput analysis of cardenolide glycosides without loss of sensitivity or selectivity, where comparisons with compound-specific methods revealed only minor differences in analytical performance. These results highlight the robustness and effectiveness of the group-specific methodology for both qualitative and quantitative applications in cardenolide research.

In the process of coupling ion mobility spectrometry (IMS) and droplet microfluidics, the sample to be analyzed is ionized by electrospray ionization (ESI), thereby transferring the liquid samples into the gas phase with concurrent ionization. In contradistinction to conventional ESI, in droplet microfluidics the sample to be analyzed is present in individual droplets, which are separated from each other by an oil phase resulting in the process of ESI becoming discontinuous due to alternating sample droplets and oil phase. Typically, averaging is necessary in IMS to suppress noise and thus improve detection limits. However, in combination with droplet microfluidics, continuous averaging leads to reduced signal-to-noise ratio, because the spectra of the oil phase not containing any information are included into averaging. To avoid this effect, it is imperative to synchronize the ESI-IMS with the droplet microfluidics using a suited trigger signal. Therefore, we present a fast, low-noise, high-gain current amplifier that can operate at high electrical potential and allows for monitoring the ESI current in both polarities. The design of this amplifier is predicated on the current change of the ESI current during the volume transition between oil and droplet inside the emitter. This transition has been mathematically modelled and incorporated as a volume-dependent term within an existing equation for the ESI current. Finally, we present experimental data to support the idea of increasing signal-to-noise ratio by triggering the ESI-IMS via the electrospray current. Furthermore, triggering the IMS facilitates droplet-wise storage of data.

The newly-emerged gas sensing detection of 1-octen-3-ol biomarker is expected to indirectly monitor foodborne illnesses caused by Salmonella-contaminated meat, which requires high selectivity and a ppb-concentration detection limit. Here, surface-doped ruthenium over tungsten oxide nanocubes (Ru/WO₃ NCBs) have been synthesized by a wet-chemical approach for highly selective and ppb-concentration 1-octen-3-ol sensing. As-prepared Ru/WO₃ NCBs exhibit a polycrystalline structure and consist of NCBs that have an average side length of ∼131 nm, and the Ru/WO₃ NCBs show a high sensing response toward 5 ppm 1-octen-3-ol (R_a/R_g = 406), excellent selectivity, 50 ppb detection limit, 70 % relative humidity tolerance, and 54 days stability at 220 °C. The excellent sensing performance might be attributed to the electronic and chemical sensitization of Ru, which thickens the electron depletion layer and increases adsorbed oxygen to promote interfacial electron transfer and 1-octen-3-ol oxidation. Practically, Ru/WO₃ NCBs have been integrated into a sensing device to simulate detecting 1-octen-3-ol, which has the potential for Salmonella detection in the future.

Organic nanogrids are versatile molecular hornstones and nanoplatforms of organic high-dimensional, low-entropy materials. It is urgent to construct virtual databases of organic nanomers for accelerating the discovery and performance optimization of novel 0/1/2/3-dimensional nanopolymer optoelectronic materials. In this study, we generated a comprehensive dataset of 11,224 ladder-type gridarenes, covering a wide range of chemical compositions and structural variations. A random selection of 220 small sample sets was aggregated, and fragment-level constrained density functional theory (CDFT) was employed to extract molecular descriptors. These descriptors were then used to train machine learning models with high predictive accuracy for band gap, highest occupied molecular orbital (HOMO), and lowest unoccupied molecular orbital (LUMO) energies (the coefficient of determination values of 0.94, 0.92, and 0.87, respectively). During the active learning process, 3112 representative gridarenes were iteratively selected from our 11,224-compound library, refining band-gap predictions to a mean absolute error below 0.11 eV. This process pinpointed top candidates for blue-light emission and demonstrated an accelerated, data-driven route to next-generation organic optoelectronic nanomaterials.

Accurate detection of NADH levels plays a critical role in the diagnosis and management of conditions ranging from metabolic disorders to neurodegenerative diseases such as Parkinson and Alzheimer. It also holds potential for therapeutic interventions targeting mitochondrial function and energy metabolism. Herein, we designed the miniaturized sharp-edged hyper-branched gold microneedles (Au MNDs) decorated with pencil graphitic microelectrodes (PGME) via single-step, green electrochemical deposition strategy in the absence of any redox mediators, organic solvents and enzymes, etc. The as-prepared Au microneedles demonstrate impressive direct electrocatalytic properties for NADH oxidation. Their sharp edges of the microneedles and the optimized transducers ionic mobility effectively enhance electrochemically active surface area and intrinsic charge transfer efficiency, making this electrode a powerful enzyme-mimic platform for detecting NADH. This morphology, combined with the unique surface features, fosters a highly ideal conditions for the rapid electron transfer from NADH to the Au MNDs @PGME. The nanostructures improve the mobility directly influences the speed and efficiency of electronic charge carriers, which accelerates the rate of electron transfer. This enhances the electrochemical kinetics of the system, contributing to rapid and sensitive detection of NADH. These attributes indicate that Au MNDs-modified microsensor holds great potential for high sensitivity (62.80 μA/μM cm^-2), two distinct linear ranges: 0.1-4.5 μM and 4.5-54.5 μM, fast response (<2 s), and lower LOD for the reliable NADH detection. The miniaturized microsensors had a strong ability to prevent anti-interference from sensing of NADH. Notably, the current micro sensing platform, which is based on Au MNDs @PGME, has proven to be useful in clinical diagnostics by successfully testing for NADH sensing in human serum and urine samples in biomedical application.