Analytical Methods最新文献

{"title":"Next-generation electrochemical sensors for opioid detection: from nanostructured interfaces towards real-time clinical monitoring.","authors":"Keerthana Madhivanan, Raji Atchudan, Sandeep Arya, Surendra H Mahadevegowda, Ashok K Sundramoorthy","doi":"10.1039/d6ay01225f","DOIUrl":"https://doi.org/10.1039/d6ay01225f","url":null,"abstract":"<p><p>The increasing prevalence of opioid misuse, substance abuse, and drug addiction, and the rapid emergence of highly potent synthetic analogues have intensified the demand for rapid, sensitive and decentralized analytical technologies for opioid monitoring in public healthcare. Conventional laboratory-based methods, although highly accurate, are often constrained by expensive instrumentation, complex sample preparation and limited portability, making them less suitable for real-time clinical and forensic applications. In response to these limitations, electrochemical point-of-care sensing platforms have emerged as promising alternatives due to their low cost, rapid response, portability and compatibility with miniaturized and wearable diagnostic systems. This review comprehensively discusses recent advances in electrochemical sensing technologies developed for the detection of natural opiates, semi-synthetic opioids, and synthetic opioids, with particular emphasis on point-of-care and wearable sensing devices. This review highlights the role of nanostructured materials, molecularly imprinted polymers, aptamer-based recognition systems, screen-printed electrodes, microneedle platforms, and flexible bioelectronic devices in enhancing analytical sensitivity, selectivity and real-sample applicability. Furthermore, emerging smart technologies involving smartphone-assisted sensing, artificial intelligence-driven signal processing, wireless data transmission, and Internet of Things-enabled healthcare systems are discussed as next-generation strategies for decentralized opioid surveillance and real-time monitoring. The review also critically examines current challenges associated with electrochemical opioid sensing, including electrode fouling, matrix interference, reproducibility limitations and insufficient large-scale clinical validation. Overall, this work provides a detailed overview of the recent progress, technological advancements and future directions of electrochemical point-of-care opioid sensing systems, emphasizing their growing significance in forensic toxicology, therapeutic monitoring, emergency diagnostics and personalized healthcare applications.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":3.0,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149134327","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Electrochemical detection of organophosphorus pesticides using screen-printed electrodes: a systematic literature review.","authors":"Nurul Hidayah Abu Bakar, Muhammad Hafiz Mazwir, Roshahliza M Ramli, Munawar Khalil, Wan Norfazilah Wan Ismail","doi":"10.1039/d6ay01271j","DOIUrl":"10.1039/d6ay01271j","url":null,"abstract":"<p><p>Organophosphorus pesticides are widely used in agriculture, creating a need for rapid and reliable monitoring of residues in food and environmental samples. Conventional chromatographic methods provide high sensitivity and accuracy but generally require laboratory-based instrumentation, sample preparation and skilled personnel, limiting their suitability for routine on-site screening. Screen-printed electrode (SPE)-based electrochemical sensors offer a portable and low-cost alternative; however, their practical application remains constrained by limited selectivity, enzyme instability, electrode-to-electrode variability and insufficient validation in complex samples. This systematic review evaluates 103 studies published between 2015 and 2026 to examine how electrode materials, surface modification, biorecognition strategies and electrochemical techniques have been used to address these challenges. Carbon-based SPEs remain the predominant platform, while recent developments increasingly employ hybrid architectures combining conductive carbon materials with metal or metal-oxide nanomaterials and polymeric or biopolymeric matrices. Acetylcholinesterase (AChE) remains the most widely used biorecognition element because of its established inhibition mechanism, whereas aptamers, molecularly imprinted materials and non-enzymatic interfaces are increasingly investigated to improve stability and selectivity. These approaches have enabled substantial improvements in detection limits, analytical sensitivity and operational performance, with many recent sensors achieving trace-level detection and successful analysis of food and environmental samples. Nevertheless, the reviewed literature reveals persistent challenges in long-term stability, batch-to-batch reproducibility, standardized reporting, interference assessment and validation under realistic field conditions. Future development should therefore focus on scalable electrode fabrication, standardized analytical protocols, systematic testing in complex matrices and integration with portable and digital readout systems. Overall, SPE-based electrochemical sensors show strong potential for rapid organophosphorus pesticide screening, but further validation and standardization are required before widespread field deployment.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8550-8582"},"PeriodicalIF":3.0,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149079003","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"<i>Ginkgo biloba</i> leaf polysaccharide-modified Cu_2-<i>x</i>Se nanozymes for smartphone-assisted colorimetric detection of food additive propyl gallate.","authors":"Yuqi Chen, Cong Jiang, Jiahui Zou, Linfeng Pang, Xueer Lin, Jiaying Zhou, Yuyue Wu, Yanyan Huang","doi":"10.1039/d6ay01310d","DOIUrl":"10.1039/d6ay01310d","url":null,"abstract":"<p><p>Propyl gallate (PG), a widely used synthetic phenolic antioxidant, has raised health concerns due to its potential risks from overexposure. Traditional methods such as chromatography are typically time-consuming, labor-intensive, and not suitable for on-site rapid screening. In this work, we successfully fabricated ultra-small Cu_2-<i>x</i>Se nanoparticles using plant-derived <i>ginkgo biloba</i> polysaccharide (GBLP) as a protective agent and ascorbic acid (AA) as a reducing agent. The generated Cu_2-<i>x</i>Se nanoparticles exhibited excellent peroxidase-like activity to catalyze the chromogenic reaction of H₂O₂ and 3,3',5,5'-tetramethylbenzidine (TMB). The presence of PG could inhibit this reaction owing to its antioxidant properties, enabling quantitative detection of PG with a detection limit (LOD) of 2.25 µM. By incorporating a smartphone and ImageJ software, a portable colorimetric device was developed for visual intelligence detection, achieving a LOD of 6.87 µM. Experimental data of real samples demonstrated that the recoveries of PG ranged from 101.52% to 106.60%, confirming the accuracy and practicality of the method. This work offered a novel nanozyme-based strategy for rapid and intelligent monitoring of PG in food products and provides a reliable, low-cost technical option for PG detection in edible oils, with prospects in the rapid screening of actual food samples.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8634-8640"},"PeriodicalIF":3.0,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148816724","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Enhancing soluble dietary fiber prediction in barley <i>via</i> Boruta-based feature selection and mid-infrared spectroscopy.","authors":"Qing-Xiao Ma, Hao Liu, Long-Yan Zhang, Guo-Ao Xie, Jie Ren, Fei-Ming Li","doi":"10.1039/d6ay01435f","DOIUrl":"10.1039/d6ay01435f","url":null,"abstract":"<p><p>Barley (<i>Hordeum vulgare</i> L.) is a major cereal crop whose soluble dietary fiber (SDF) offers significant health benefits, yet conventional SDF determination methods are time-consuming, labor-intensive, and destructive to samples. This study developed a rapid, non-destructive method for SDF quantification in barley using mid-infrared (MIR) spectroscopy combined with a Boruta-based partial least squares (PLS) hybrid approach. A total of 280 barley grain samples were subjected to Fourier-transform infrared (FTIR) spectral acquisition from 2000 to 650 cm^-1, with reference SDF values determined by the association of official analytical chemists (AOAC) 991.43 enzymatic-gravimetric method. The Boruta algorithm selected 165 informative wavenumbers out of 363, reducing the variable space by 54.5%. The developed Boruta-PLS model achieved excellent predictive performance with a coefficient of determination for the training set (<i>R</i>²_C) of 0.9695 and for the test set (<i>R</i>²_P) of 0.9601 and a root mean squared error for the training set (RMSE_C) of 0.7464%, and for the test set (RMSE_P) of 0.7340%, substantially outperforming the full-spectrum PLS model with an <i>R</i>²_P of 0.7759 and an RMSE_P of 1.7387%, as well as conventional wavelength selection methods including variable importance in projection (VIP), competitive adaptive reweighted sampling (CARS), and uninformative variable elimination (UVE). The selected wavenumbers were predominantly located in chemically relevant regions at 1000-1200 cm^-1 and 1500-1700 cm^-1, confirming model interpretability. This Boruta-PLS approach provides a rapid, non-destructive, and cost-effective alternative for SDF quantification, with strong potential for high-throughput screening and real-time quality monitoring of barley samples.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8670-8678"},"PeriodicalIF":3.0,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148838490","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Near-infrared esterase-activated fluorescent probes for tumor cell identification and <i>in vivo</i> heterogeneity imaging.","authors":"Shuai Fan, Ziwen Xiao, Xiaoyang Li, Jiaxin Shao, Yuting Wang, Mengke Zhang, Panpan Zhang, Jiemin Wang, Deyan Gong","doi":"10.1039/d6ay01386d","DOIUrl":"10.1039/d6ay01386d","url":null,"abstract":"<p><p>Esterases constitute vital hydrolases participating in lipid metabolism, prodrug activation, and tumor progression. Due to the significant heterogeneity in their expression levels across different types of tumor microenvironments, esterases have emerged as promising biomarkers for cancer diagnosis. This probe achieves fluorescence quenching through an intramolecular photoinduced electron transfer (PET) mechanism. Under the catalysis of the esterase, the amide bond is hydrolyzed and the heptafluorobutyramide group is cleaved, restoring the electron-donating capacity of the amino group, blocking the PET effect, and restoring the fluorescence signal. <i>CYF</i> exhibits high sensitivity (limit of detection as low as 0.04749 U mL^-1), excellent selectivity, and good photostability. Molecular docking and theoretical simulations show that <i>CYF</i> can stably bind to the esterase's active pocket through multiple molecular forces, with a binding affinity of -9.3 kcal mol^-1. The HOMO-LUMO band gap clearly elucidates the probe's fluorescence response mechanism. <i>CYF</i> demonstrates good biocompatibility and low cytotoxicity, effectively distinguishing disparities in esterase activity between normal thyroid cells (Nthy-ori3-1) and thyroid cancer cells (TPC-1), with significantly upregulated esterase activity observed in TPC-1 cells. In 4T1 tumor-bearing mice, the fluorescence intensity of probe <i>CYF</i> in the tumor region was significantly lower than in normal tissue; this signal was further suppressed following pretreatment with the inhibitor AEBSF. These results confirm the low expression of esterase activity in the breast cancer intratumoral microenvironment and demonstrate <i>CYF</i>'s capability for the time-dependent, <i>in situ</i> dynamic tracking of esterase activity <i>in vivo</i>.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8720-8726"},"PeriodicalIF":3.0,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148862744","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Competitive immunoassay-based magneto-stress-electric coupled biosensor for ultrasensitive detection of NT-proBNP.","authors":"Biaobiao Wang, Haoyu Wang, Xingbo Yu, Sitong Wu, Xing Guo, Jianlong Ji, Shengbo Sang, Chuangang Zhou, Dong Zhao, Deliang Shen","doi":"10.1039/d6ay00950f","DOIUrl":"10.1039/d6ay00950f","url":null,"abstract":"<p><p>Salivary N-terminal pro-B-type natriuretic peptide (NT-proBNP) is a promising non-invasive biomarker for heart failure (HF); however, its ultralow concentration hinders its clinical application. In this study, a magneto-stress-electric coupled (MSEC) mechanical biosensor integrated with a competitive immunoassay (CIA) has been developed for the sensitive detection of salivary NT-proBNP. Based on the magnetostrictive effect of an Fe-Ga alloy under a uniform magnetic field, the gravitational interference on the sensor film is effectively eliminated, and the film deformation induced by specific antigen-antibody binding is significantly enhanced. Concurrently, the competitive binding between free NT-proBNP antigen and magnetic bead-NT-proBNP antigen conjugates enables the sensor to detect extremely low concentrations of free NT-proBNP with high sensitivity. The biosensor achieves an ultralow detection limit of 0.01 pg mL^-1, with excellent specificity, selectivity, stability, and batch-to-batch reproducibility. Furthermore, accurate and reproducible detection of NT-proBNP in artificial saliva samples is performed by the sensor, with recovery rates ranging from 98.0% to 103.3%. In this work, magnetic signal enhancement, stress-to-electric conversion, and competitive immunorecognition are integrated into a single sensing platform. Consequently, a novel, low-cost, and reliable strategy is established for the non-invasive and highly sensitive detection of NT-proBNP, which holds great promise for point-of-care testing and early auxiliary diagnosis of heart failure.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8603-8614"},"PeriodicalIF":3.0,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148816796","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Bacterial catalase-responsive colorimetric array driven by nanozyme cascade for pathogen identification and phenotypic susceptibility testing.","authors":"Yi Yu, Xueni Yang, Yinghui Song, Baojun Yang, Jifeng Liu, Xia Gao","doi":"10.1039/d6ay01416j","DOIUrl":"10.1039/d6ay01416j","url":null,"abstract":"<p><p>The rapid discrimination of bacterial species and assessment of their antibiotic susceptibility are critical for combating antimicrobial resistance. Herein, we report a metabolism-driven colorimetric sensor array based on bacterial catalase-responsive hydrogen peroxide (H₂O₂) consumption coupled with an Au@PB (gold-coated Prussian blue) nanozyme cascade, which relies on a single 3,3',5,5'-tetramethylbenzidine (TMB) probe. Bacteria with different intrinsic catalase activities consume varying amounts of H₂O₂, leaving distinct residuals that drive Au@PB-catalyzed TMB oxidation to produce three characteristic absorption peaks at 370, 652, and 880 nm. These three-wavelength signals serve as unique phenotypic fingerprints. Combined with linear discriminant analysis (LDA), the single-probe array successfully discriminates multiple bacterial species and mixtures, exhibiting a linear quantitative response across 10⁴-10⁷ CFU mL^-1. Furthermore, by monitoring real-time changes in catalase activity upon antibiotic exposure, the platform enables phenotypic antimicrobial susceptibility testing (AST) with a rapid assay time of ∼75 min for standardized bacterial suspensions, expediting the evaluation process compared to culture-based methods. Validated in water samples and clinical isolates, the AST results showed good agreement with the clinical laboratory standards institute (CLSI) gold standard. Therefore, this nanozyme-driven, single-probe sensor array provides a sensitive, and cost-effective tool for integrated pathogen identification and rapid AST.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8771-8780"},"PeriodicalIF":3.0,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148862599","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Beyond conventional glucose assays: a dual smartphone-Arduino point-of-care diagnostic platform based on Fe-Zn bimetallic nanozymes.","authors":"Ola G Hussein, Ibrahim A Naguib, Roula Bayram, Abdullah H Alluhayb, Reham Ali, Mohammed Gamal","doi":"10.1039/d6ay01292b","DOIUrl":"10.1039/d6ay01292b","url":null,"abstract":"<p><p>The increasing demand for decentralized healthcare has accelerated the development of portable point-of-care (POC) diagnostic systems capable of providing rapid, accurate, and user-friendly glucose monitoring. Herein, we report an Fe-Zn bimetallic nanozyme-based colorimetric sensing platform that integrates smartphone-assisted digital image analysis and Arduino-based signal acquisition for portable glucose determination. The Fe-Zn bimetallic nanoparticles (Fe-Zn BNPs) were synthesized through a simple aqueous route and exhibited excellent intrinsic peroxidase-like activity toward the hydrogen peroxide-mediated oxidation of 3,3',5,5'-tetramethylbenzidine (TMB). Coupling the nanozyme with a glucose oxidase (GOx)-mediated cascade reaction enabled sensitive and selective glucose detection through catalytic signal amplification. The synthesized Fe-Zn BNPs exhibited excellent peroxidase-like catalytic activity toward hydrogen peroxide with a broad linear range of 10-700 µM and an excellent correlation coefficient (<i>R</i>² = 0.9996). Steady-state kinetic analysis revealed a low apparent <i>K</i>_m of 0.0647 mM and a <i>V</i>_max of 1.75 × 10^-9 M s^-1 confirming the high substrate affinity and catalytic efficiency of the developed nanozyme. The proposed glucose sensing platform displayed a wide linear range of 10-500 µM with excellent analytical performance using UV-Vis spectrophotometry (<i>R</i>² = 0.9980), Arduino-assisted detection (<i>R</i>² = 0.9975), and smartphone-based digital image analysis (<i>R</i>² = 0.9967). The platform demonstrated high selectivity toward glucose over common biological interferents and was successfully validated in human serum providing a glucose concentration of 5.07 ± 0.15 mM which was in excellent agreement with that of the reference clinical method (4.93 ± 0.14 mM). The environmental sustainability of the developed platform was comprehensively assessed using the Nanomaterial Assessment Tool (NAT), Blue Applicability Grade Index (BAGI), Red Analytical Performance Index (RAPI), and Environmental Performance-Practicality Index (EPPI) achieving scores of 78, 75, 70, and 84.8, respectively, demonstrating excellent compliance with the principles of green and white analytical chemistry. By integrating efficient Fe-Zn nanozyme catalysis with dual smartphone-Arduino portable detection, the proposed platform provides a sensitive, sustainable, and practical strategy for next-generation point-of-care glucose diagnostics.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8781-8799"},"PeriodicalIF":3.0,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148862594","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"AI-assisted sustainable pharmaceutical bioanalysis: critical review of LC-MS, matrix effects, and white analytical chemistry.","authors":"Hemn A H Barzani, Rebaz Anwar Omer, Khalamala Ibrahim Salih Barzani, Hazha Omar Othman, Ali Sedeeq Noaman, Kovan Dilawer Issa, Seerwan Hamadameen Sulaiman","doi":"10.1039/d6ay01554a","DOIUrl":"10.1039/d6ay01554a","url":null,"abstract":"<p><p>Pharmaceutical bioanalysis has undergone remarkable technological advancement with the widespread adoption of liquid chromatography-mass spectrometry (LC-MS) platforms, enabling highly sensitive and selective quantification of pharmaceuticals, metabolites, biomarkers, peptides, proteins, and oligonucleotides. Despite these developments, persistent challenges, including matrix effects, analytical instability, biological matrix complexity, data overload, and sustainability concerns, continue to compromise analytical reliability and translational applicability. This critical review comprehensively evaluates the current state of pharmaceutical bioanalysis by examining emerging LC-MS technologies, sustainable analytical strategies, and the growing role of artificial intelligence (AI) and machine learning (ML) in analytical optimization, spectral interpretation, biomarker discovery, and autonomous decision-making. Particular emphasis is placed on White Analytical Chemistry (WAC) as a multidimensional framework that simultaneously considers analytical performance, environmental sustainability, and practical feasibility. The review critically assesses the limitations of current AI-assisted and sustainability-driven approaches, highlighting issues with algorithmic transparency, regulatory acceptance, standardization, and insufficient real-world validation. Furthermore, it explores intelligent analytical ecosystems that integrate advanced LC-MS platforms, explainable AI, digital twins, automation, and cloud-based infrastructure. Finally, realistic future priorities are proposed to facilitate the transition to autonomous, reliable, and environmentally sustainable pharmaceutical bioanalysis that supports precision medicine and next-generation drug development.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8458-8498"},"PeriodicalIF":3.0,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148904686","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Comprehensive evaluation of analytical methods for determination of ansamycins across diverse matrices.","authors":"Hemn A H Barzani, Rebaz Anwar Omer, Ali Hussein Mer, Hazha Omar Othman, Seerwan Hamadameen Sulaiman","doi":"10.1039/d6ay01442a","DOIUrl":"10.1039/d6ay01442a","url":null,"abstract":"<p><p>Ansamycins (ANs), including rifampicin (RIF), rifabutin (RFB), rifapentine (RPT), rifalazil (RFL), and rifaximin (RFX), are structurally distinctive macrocyclic antibiotics whose analytical determination is complicated by very low systemic exposure (especially RFX), high protein binding and intracellular sequestration (notably RFB and RFL), and extensive hepatic metabolism. The reviewed articles were retrieved from major scientific databases, including Scopus, Web of Science, ScienceDirect, Google Scholar, and PubMed, and were limited to English-language publications. This review aims to provide a comprehensive and comparative evaluation of chromatographic, spectroscopic, and electroanalytical strategies used over the past 25 years to quantify clinically important ANs across biological and pharmaceutical matrices, linking analytical performance to drug-specific physicochemical properties, stability constraints, and bioanalytical applications. The reviewed literature shows that high-performance liquid chromatography remains the core methodology, with LC-MS/MS representing the gold standard for trace-level determination, particularly for RFB, RPT, RFL, and RFX, due to its superior structural selectivity and sensitivity, whereas UV-based HPLC remains suitable mainly for pharmaceutical quality control because co-absorbing rifamycin derivatives frequently compromise accuracy in biological matrices, while electroanalytical and spectroscopic methods, despite their simplicity and lower cost, face limitations in complex matrices due to selectivity constraints. Overall, matrix complexity and analyte instability were the dominant contributors to variability in AN quantification. Looking forward, advances are expected to arise from continued refinement of LC-MS/MS workflows, greater use of orthogonal separation strategies, improved stabilization protocols, and sustainable, miniaturized sample-preparation approaches, thereby ensuring reliable, high-sensitivity AN determination to support therapeutic drug monitoring, clinical pharmacokinetics, and pharmaceutical quality control.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8518-8549"},"PeriodicalIF":3.0,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149078952","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}