The pursuit of peak athletic performance has transitioned from subjective coaching intuition to a data-driven science, demanding objective, molecular-level insights into an athlete’s physiological state. Exercise, as a potent physiological stressor, induces a cascade of changes in endogenous biomarkers, offering a window into training adaptation, fatigue, recovery, and nutritional status. This review critically evaluates the application of hyphenated chromatography–mass spectrometry (chromatography–MS), primarily gas chromatography–mass spectrometry (GC–MS) and (ultra-high-performance) liquid chromatography–tandem mass spectrometry ((U)HPLC–MS/MS), for the analysis of these exercise-induced biomarkers. We provide a comprehensive examination of analytical workflows, from the established utility of GC–MS for steroid profiling to contemporary (U)HPLC–MS/MS methods that enable high-throughput metabolomics and proteomics by coupling fast LC separations online to MS/MS detection. Finally, we synthesize these findings to propose a new integrated framework: rather than competing with emerging real-time wearable sensors, chromatography–MS must serve as the periodic “ground truth” validator. We discuss how this symbiotic relationship addresses current limitations in noninvasive monitoring and enables the multiomics data integration necessary for truly individualized sports science decision-making.
An innovative, straightforward, sustainable, and sensitive fluorescent turn off-on sensing probe was developed for quick assay of tobramycin. Tobramycin (TBM) is one of aminoglycosides, which is frequently utilized for the management of gram negative bacterial infections. Developing an analytical procedure for the assay of TBM is challenging due to its structure that lacks chromophore. This study aims to establish a sensing strategy that relies on the quenching of the of fluorescence of salicylate at 410 nm upon the addition of ammonium ferric sulfate after excitation at 299 nm. The capability of tobramycin to displace salicylate from ferric salicylate complex results in turning on salicylate fluorescence. Box-Behnken design (BBD) was selected for efficient optimization of the key experimental factors. A linear response was achieved throughout concentrations of TBM ranging from 6.0 to 30.0 mu g/mL (equivalent to 12.8-64.2 & micro;M) with limits of detection and quantitation equal 1.26 mu g/mL and 3.81 mu g/mL, respectively. The proposed probe was implemented for analysis of TBM in eye drops with mean percent recovery of 99.72 % +/- 1.11. The ecological friendliness of the developed platform was proved according to several metrics for whiteness, blueness, and greenness. Moreover, compliance with many sustainability development goals (SDGs) was evidenced.
A molecularly imprinted solid-phase extraction (MISPE) sorbent has been developed for the separation of RIV from serum sample. Molecularly imprinted polymer (MIP) was prepared via non-covalent imprinting technique using RIV as a template molecule, methacrylic acid (MAA) as a functional monomer, ethylene glycol dimethacrylate (EGDMA) as a crosslinker, N, N-azobisisobutyronitrile (AIBN) as an initiator, and dimethylsulfoxide (DMSO) as a porogenic solvent. An imprinting factor of 3.4 was achieved for the RIV imprinted MIP. Adsorption behavior of the sorbent followed Langmuir model and reached a maximum adsorption capacity of 20.7 mg/g. Adsorption kinetics was also investigated using pseudo-first and second-order models. MIP and NIP sorbents were dry-packed into solid-phase extraction cartridges and eluates from cartridges were analyzed. Limit of detection and limit of quantification values were 0.635 and 1.92 & micro;g/mL, respectively. Recovery values for the MIP and NIP sorbents were 72.6 and 17.2 %, respectively. Excellent within-day (0.22-1.34 % RSD) and between-day (0.43-1.46 % RSD) precision values were also achieved for the MIP sorbent as well. Our findings prove that the developed MISPE method exhibits high precision and selectivity towards RIV in serum sample containing high number of interfering compounds.
Phenylenediamines (PDs) and their N,N′-substituted derivatives (PPDs) are widely used antiozonants in rubber and polymer manufacturing, with significant release into the environment via tire wear particles. Once emitted, they undergo oxidative transformations, producing quinone derivatives and other products through ozonolysis, photooxidation, and hydrolysis. Among these transformation products, quinone derivatives are the most extensively studied due to their enhanced stability and high toxicity, exemplified by 6PPDQ-induced mortality in coho salmon at ng/L levels. Their occurrence has been reported in water, soils, air, dust, and food products, raising concerns over ecological risks and potential human exposure. This review critically assesses current analytical methodologies, highlighting liquid chromatography–mass spectrometry as the most powerful tools, complemented by tailored extraction approaches such as solid-phase extraction (SPE), liquid–liquid extraction (LLE), Quick, Easy, Cheap, Effective, Rugged, and Safe extraction (QuEChERS), and accelerated solvent extraction (ASE). Despite methodological advances, major challenges persist, including low environmental concentrations, chemical instability, and lack of certified standards. Future priorities include harmonized protocols, interlaboratory validation, and development of emerging analytical and real-time monitoring technologies.
This study aims to develop and experimentally implement a novel portable electrochemical sensor based on screen-printed carbon electrodes (SPCEs) and an original bath-injection electrochemical cell for real-time environmental monitoring of pollutants. The scientific novelty of this work lies in the design of a simplified yet highly effective electrochemical cell that eliminates the need for a liquid carrier through an innovative self-washing mechanism using excess sample volume. This feature significantly reduces system complexity and enhances sensor reliability in field applications. The advantages of microfluidic technologies in the development of SPCE-based sensors are highlighted, and detailed protocols for modifying SPCEs with mercury, bismuth, and gold films are presented. Surface characterization is supported by micrographs, ensuring reproducibility of the electrode surface and analytical results. Voltammograms for various individual ions and their mixtures are provided, along with the corresponding electrode modifications and analytical conditions. The developed system demonstrates a broad linear concentration range and a detection limit as low as 5–10 μg/L. Field trials of the sensor were conducted using water samples from the Zeravshan river, a major source of drinking water in the region. Elevated concentrations of several toxic ions were detected, with the results confirmed by atomic absorption and inductively coupled plasma atomic emission spectroscopy. The proposed sensor system proves to be a promising solution for on-site pollutant detection under limited infrastructure conditions, supporting rapid response to both anthropogenic and natural environmental emergencies.
