Critical reviews in analytical chemistry最新文献

{"title":"Fourier Transform Infrared Spectroscopy for Quantitative Determination of Drug Purity in Pharmaceutical Dosage Forms: Recent Advances, Validation Strategies, and Chemometric Applications.","authors":"Hiran Saber Dawood, Farouq Emam Hawaiz","doi":"10.1080/10408347.2026.2697299","DOIUrl":"https://doi.org/10.1080/10408347.2026.2697299","url":null,"abstract":"<p><p>The quantitative determination of drug purity is a critical aspect of pharmaceutical quality control, ensuring the safety, efficacy, and regulatory compliance of pharmaceutical products. Conventional analytical techniques such as high-performance liquid chromatography (HPLC) and gas chromatography (GC) provide excellent analytical performance but often require extensive sample preparation, longer analysis times, and substantial solvent consumption. Fourier Transform Infrared (FTIR) spectroscopy has emerged as a rapid, cost-effective, and environmentally friendly alternative for pharmaceutical analysis. This review critically evaluates recent advances in FTIR spectroscopy for the quantitative determination of drug purity in pharmaceutical dosage forms, with particular emphasis on sampling strategies, validation requirements, and chemometric applications. Published studies involving transmission FTIR, attenuated total reflectance (ATR-FTIR), and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) are systematically examined and compared. The role of chemometric techniques, including principal component analysis (PCA), partial least squares (PLS) regression, is discussed in overcoming spectral overlap and improving analytical performance. Validation parameters including linearity, accuracy, precision, specificity, limit of detection (LOD), and limit of quantification (LOQ) are critically assessed according to current regulatory guidelines. The reviewed studies demonstrate that FTIR spectroscopy, particularly when integrated with advanced chemometric methods, can provide reliable quantitative analysis of pharmaceutical compounds with analytical performance comparable to conventional techniques. Nevertheless, challenges related to model transferability, standardization, and regulatory acceptance remain. Future developments in machine learning-assisted spectroscopy, portable FTIR instrumentation, and harmonized validation protocols are expected to further expand the role of FTIR spectroscopy in pharmaceutical quality control and counterfeit drug detection.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-16"},"PeriodicalIF":7.7,"publicationDate":"2026-07-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148389959","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Targeting, Tracking, and Triggering: Versatile Applications of Zr-MOFs in Drug Delivery, Theranostic Platforms, and Advanced Biosensing.","authors":"Sanil Narayanan, Balasubramanian Kandasubramanian","doi":"10.1080/10408347.2026.2695929","DOIUrl":"https://doi.org/10.1080/10408347.2026.2695929","url":null,"abstract":"<p><p>Zirconium-based metal-organic frameworks (Zr-MOFs) have emerged as promising platforms for biomedical analysis owing to the exceptional chemical and hydrolytic stability imparted by their robust Zr₆ secondary building units (SBUs). Strong Zr-O coordination bonds and high framework connectivity enable these materials to retain structural integrity under physiological conditions, overcoming limitations of conventional systems such as instability, leaching, and nonspecific interactions. This review critically explores the applications of Zr-MOFs in three interconnected areas: stimuli-responsive drug delivery with integrated analytical monitoring, multimodal bioimaging (PET, CT, and near-infrared fluorescence) for real-time diagnostics, and advanced biosensing, with emphasis on electrochemiluminescence, fluorescence, and nanozyme-based detection of clinically relevant biomarkers. Organized around the concepts of Targeting, Tracking, and Triggering, the review highlights how the intrinsic stability of Zr₆ SBUs, combined with defect engineering, surface functionalization, stimuli-responsive gating, and self-calibrating strategies, enhances analytical performance. Beyond summarizing applications, it critically compares design approaches, evaluates key performance metrics, including drug loading, detection limits, matrix tolerance, and in vivo stability, and discusses major translational challenges such as scalable synthesis, real-sample validation, and long-term biocompatibility. Finally, emerging opportunities in AI-assisted inverse design and green manufacturing are highlighted to accelerate the clinical translation of Zr-MOFs.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-12"},"PeriodicalIF":7.7,"publicationDate":"2026-07-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148396330","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Recent Progress in Fluorescent Probes for Hydrazine Detection with Double-Bond Structural Features.","authors":"Fuyang Dong, Junwei Zhu, Zehao Ye, Guixiao Cao, Da-Jun Xiang, Wen-Long Wang","doi":"10.1080/10408347.2026.2689429","DOIUrl":"https://doi.org/10.1080/10408347.2026.2689429","url":null,"abstract":"<p><p>Hydrazine (N₂H₄) is widely used in industrial and academic fields, yet its high toxicity poses serious risks to environmental safety and human health. Reliable and sensitive quantification of trace N₂H₄ in environmental and biological systems is therefore of great importance. To meet this demand, a wide variety of fluorescent probes have been developed in recent years. Among them, probes employing hydrazine-responsive functional groups as recognition units are particularly common. Despite significant advances in this field, no systematic review currently exists that focuses exclusively on fluorescent probes containing double bonds as a structural feature. In this review, we have summarized recently reported fluorescent probes for detecting N₂H₄. These fluorescent probes classified by double bond type include carbon-oxygen double bonds (forming aldehyde motifs) and carbon-carbon double bonds (malononitrile, benzothiazole-2-acetonitrile, barbituric acid, 1,3-indanedione and 2,2-Dimethyl-1,3-dioxane-4,6-dione motifs). All these double bonds react with hydrazine to form hydrazine derivatives as the final products. Furthermore, the comments for improving probe performance are proposed. This review aims to provide valuable insights for the rational design of novel fluorescent probes for N₂H₄ detection.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-22"},"PeriodicalIF":7.7,"publicationDate":"2026-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148374833","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Research Progress of Purely Organic Luminophores in the Field of Electrochemiluminescence.","authors":"Jiayin Cai, Zejun Jiang, Guangyan Liu, Yanjun Guo, Shili Hou","doi":"10.1080/10408347.2026.2694609","DOIUrl":"10.1080/10408347.2026.2694609","url":null,"abstract":"<p><p>Electrochemiluminescence (ECL) is recognized as an analytical technique that integrates the principles of electrochemistry and spectroscopy. In ECL systems based on purely organic luminophores, optical signals can be directly generated through electrical excitation, thereby achieving efficient ECL emission. The selection and optimization of ECL luminophores are considered to exert a critical influence on the overall performance and application value of the ECL system. Purely organic luminophores are regarded as exhibiting significant application potential in the ECL field, which is attributed to their prominent advantages such as straightforward synthesis, facile structural modification, favorable biocompatibility, and tunable optical properties. Currently, ECL sensors based on purely organic luminophores have been successfully employed for the highly selective detection of metal ions, organic pollutants, and biomolecules. Consequently, they are considered to exhibit broad application prospects in areas such as environmental protection, food safety, and clinical diagnosis. In this review, a systematic overview is provided regarding the relationship between the molecular structure, ECL mechanisms, and luminescence properties of various types of purely organic luminophores reported in recent years. Furthermore, their applications in ECL sensors are summarized. This review is intended to offer a theoretical basis and technical reference for the molecular design of novel purely organic luminophores and for further investigations into their ECL performance, thereby promoting the advancement of their applications in the ECL field.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-39"},"PeriodicalIF":7.7,"publicationDate":"2026-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148374847","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Characterization of Coffee Residues and Derived Biochar via Fourier-Transform Infrared Spectroscopy: Current Status and Outlook.","authors":"Runyu Zheng, Mohammed Kamruzzaman","doi":"10.1080/10408347.2026.2696478","DOIUrl":"https://doi.org/10.1080/10408347.2026.2696478","url":null,"abstract":"<p><p>Coffee processing generates large amounts of solid residues, including spent coffee grounds, husks, parchment, and silverskin, which represent an abundant biomass resource with significant potential for valorization. Thermal conversion of these residues into biochar has attracted increasing attention due to its applications in soil amendment, adsorption, energy production, and environmental remediation. Fourier-transform infrared (FTIR) spectroscopy is one of the most widely used techniques for characterizing properties of biomass and biochar because of its rapid analysis, minimal sample preparation, and ability to identify functional groups. This review summarizes the current state of FTIR applications in the characterization of coffee residues and derived biochar. Spectral features across feedstock types, thermal processes, and certain application scenarios are discussed, along with emerging areas such as semi-quantitative analysis, dynamical inspection, and predictive modeling. Particular attention is given to the interpretation of functional group assignments and transformations, the use of spectral indices, and the limitations of FTIR in complex biomass-biochar systems. Finally, future perspectives highlight the need for standardized spectral metrics, integration with complementary analytical techniques, and development of chemometric and modeling approaches to enable more quantitative and mechanistic interpretation of FTIR data in coffee residue and biochar research.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-23"},"PeriodicalIF":7.7,"publicationDate":"2026-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148374785","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Real-Sample Validation of Microchemical Sensors: Matrix Effects, Chemometric Reliability, and Field-Ready Analytical Performance.","authors":"Wajid Zaman, Asma Ayaz","doi":"10.1080/10408347.2026.2695427","DOIUrl":"https://doi.org/10.1080/10408347.2026.2695427","url":null,"abstract":"<p><p>Microchemical sensors are increasingly used in food safety, clinical diagnostics, environmental monitoring, agriculture, forensics, and industry because they offer rapid, sensitive, miniaturized, and portable detection. However, performance is often judged mainly by limit of detection, linear range, sensitivity, selectivity, and recovery in spiked samples, which do not establish reliability in complex matrices. Real samples contain proteins, lipids, salts, pigments, enzymes, humic substances, particles, microbes, and variable pH or ionic strength that can alter recognition, calibration, signal generation, and interpretation. This review proposes a real-sample validation framework integrating sampling, pretreatment, matrix-effect assessment, realistic interference testing, calibration, reproducibility, inter-device variation, stability, authentic sample analysis, reference-method comparison, uncertainty, greenness, portability, and field readiness. It also evaluates chemometrics and artificial intelligence for electrochemical, optical, spectral, image-based, and sensor-array data, emphasizing risks of overfitting, data leakage, small datasets, weak external validation, and poor transferability. Unlike reviews centered on materials or ultralow detection limits, this review identifies validation intelligence as the missing link between laboratory sensitivity and real-world reliability. Ranking sensors by real-sample readiness rather than sensitivity alone provides a practical roadmap for robust, transparent, sustainable, and decision-ready sensing systems.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-20"},"PeriodicalIF":7.7,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148367421","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synergistic CRISPR-Cas and Nanozyme-Based Fluorescent Sensors for Ultrasensitive Heavy Metal Detection.","authors":"Lang Cheng, Dongxiu Liu, Hui Zhang, Hongkun Lin, Ping Zhang, Jing Dong, Chen Li, Fei Ren, Xiuhong Ge, Shanshan An, Feiyan Yang, Jiahan Liu, Jiabo Fu, Furui Tang, Feifei Wang, Tianzi Liu, Hongzhi Pan, Lina Zou, Jian Zhou, Hongkun Ma, Shengzhong Rong","doi":"10.1080/10408347.2026.2684551","DOIUrl":"https://doi.org/10.1080/10408347.2026.2684551","url":null,"abstract":"<p><p>Heavy metal pollution poses a serious threat to ecological balance and human health. Traditional detection methods, such as atomic absorption spectrometry and inductively coupled plasma mass spectrometry, suffer from complex procedures, high costs and susceptibility to interference, making them unable to meet the requirements of on-site rapid detection. To address this bottleneck, this review focuses on the innovative solution of the synergistic detection strategy combining nanozymes and the CRISPR-Cas systems. The core advantages of this strategy are as follows: it leverages the excellent specific recognition and signal amplification capabilities of the CRISPR-Cas system to achieve a precise response to heavy metal trigger signals; meanwhile, it utilizes the high stability and enzyme-mimicking catalytic activity of nanozymes to convert signals into readable outputs, thereby constructing an efficient detection platform. We elaborate on how this synergistic mechanism enables high-sensitivity detection without sample pretreatment and remarkably improves analytical performance, with a wider linear range and a lower detection limit. Numerous studies have demonstrated that this combined strategy lays a solid foundation for developing portable, high-sensitivity heavy metal detection devices suitable for complex matrices such as food, water and blood samples, holding great promise for field on-site detection applications.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-21"},"PeriodicalIF":7.7,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148359796","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"From Data to Decision: Standardization, Validation, and Regulatory Readiness of AI-Driven Analytical Chemistry Workflows.","authors":"Samah Abo El Abass, Abdulmalik S A Altamimi, Taibah Aldakhil, Pintu Prajapati","doi":"10.1080/10408347.2026.2694610","DOIUrl":"https://doi.org/10.1080/10408347.2026.2694610","url":null,"abstract":"<p><p>Artificial intelligence (AI) is fundamentally reshaping analytical chemistry by enabling automated data interpretation, intelligent method optimization, and increasingly autonomous analytical workflows across pharmaceutical quality control, environmental monitoring, and clinical diagnostics. Despite remarkable recent advances, widespread regulatory-ready deployment remains constrained by critical translational barriers, including insufficient external validation, inadequate model interpretability, and the absence of coherent lifecycle governance frameworks. This review critically evaluates the current landscape of AI-driven analytical chemistry with particular emphasis on hyphenated chromatographic platforms-especially reverse-phase high-performance liquid chromatography (RP-HPLC) and its hyphenated configurations-as primary technological substrates for AI integration. The roles of Explainable AI (XAI), Uncertainty Quantification (UQ), FAIR data governance, and continuous lifecycle validation are assessed against key international regulatory frameworks, including ICH Q2(R2), ICH Q14, GAMP 5, FDA Computer Software Assurance (CSA) guidance, Good Machine Learning Practice (GMLP), and EMA AI perspectives. Two translational gaps are defined and critically examined: the <i>Validation Gap</i> (disconnect between high internal model performance and limited external reproducibility evidence) and the <i>Discrepancy Gap</i> (deterioration of model performance under real-world deployment conditions due to domain shift and instrument heterogeneity). The review further presents a milestone timeline for RP-HPLC hyphenation, a critical comparative analysis of hyphenated techniques including LC-MS/MS, LC-NMR, LC-ICP-MS, and LC-HRMS, and a new comprehensive table of reported AI/ML applications in chromatographic method development. Key recommendations are provided for bridging the path from proof-of-concept AI tools to trustworthy, decision-ready analytical ecosystems.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-47"},"PeriodicalIF":7.7,"publicationDate":"2026-06-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148350925","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Electrochemical Detection in Electromembrane Extraction: A Critical Review of Principles, Challenges, and Recent Advances.","authors":"Mostafa Jafari, Saeed Nojavan","doi":"10.1080/10408347.2026.2691866","DOIUrl":"https://doi.org/10.1080/10408347.2026.2691866","url":null,"abstract":"<p><p>Electromembrane extraction (EME) combined with electrochemical detection (ECD) provides a selective and sensitive strategy for enriching electroactive analytes in complex biological, environmental, and food matrices. This review critically summarizes recent advances in EME-ECD, with particular emphasis on voltammetric techniques, electrode surface engineering, and different degrees of system integration, ranging from offline configuration to fully online platforms. Reported applications include the determination of heavy metals, pharmaceuticals, and environmental pollutants, demonstrating the versatility of this approach. Despite considerable progress, several limitations continue to hinder its broader adoption, including dependence on offline detection, limited electrode stability, and insufficient validation using real-world samples. Additional concerns include methodological inconsistencies, overstated performance claims, and limited comparison with established chromatographic techniques. Promising future directions include microfluidic integration, multi-analyte electrode arrays, durable nanostructured electrode materials, and the application of machine learning for method optimization. The development of standardized protocols, certified reference materials, and lifecycle assessments will be essential for improving reproducibility, reliability, and sustainability. Continued interdisciplinary innovation is expected to advance EME-ECD toward a robust analytical platform for environmental, clinical, and food safety monitoring.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-13"},"PeriodicalIF":7.7,"publicationDate":"2026-06-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148338142","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"X-Ray Fluorescence Spectrometry in Botanical Drugs' Research - Applications, Methodologies, and Future Perspectives.","authors":"Ling Gao, CongYing Zhang, RuiLin Sun","doi":"10.1080/10408347.2026.2693588","DOIUrl":"https://doi.org/10.1080/10408347.2026.2693588","url":null,"abstract":"<p><p>X-ray fluorescence (XRF) spectrometry is increasingly used in botanical drug research for rapid, nondestructive, multi-elemental analysis. This systematic review examines the principles and applications of major XRF techniques-including energy-dispersive XRF (EDXRF), wavelength-dispersive XRF (WDXRF), total reflection XRF (TXRF), synchrotron radiation XRF (SR-XRF), and portable XRF (pXRF)-in medicinal plant analysis. Key applications include heavy metal safety screening, nutritional profiling, provenance traceability, and authenticity verification, particularly when integrated with chemometrics and machine learning. Advances in sample preparation, matrix effect correction, and speciation analysis are discussed. Emerging interdisciplinary applications, such as metallomics, multidimensional characterization, and green nanomaterial analysis, are also highlighted. Despite challenges with detection limits and matrix effects, ongoing hardware and software innovations continue to expand XRF capabilities. Future integration with spatial metabolomics and multimodal imaging promises to reveal the spatial relationship between inorganic elements and bioactive organic constituents, positioning XRF is one of the pivotal methods for modern botanical drug quality control.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-19"},"PeriodicalIF":7.7,"publicationDate":"2026-06-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148327247","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}