{"title":"Enhancing Pharmaceutical Analysis with Analytical Quality by Design in UHPLC: A Review of Methodological Innovations (2014-2025).","authors":"Rajendra Kotadiya","doi":"10.1080/10408347.2025.2516607","DOIUrl":"https://doi.org/10.1080/10408347.2025.2516607","url":null,"abstract":"<p><p>The integration of analytical quality by design (AQbD) in ultrahigh-performance liquid chromatography (UHPLC) has enhanced pharmaceutical method development by improving robustness, efficiency, and regulatory compliance. Despite its growing adoption, a dedicated evaluation remains limited. Among 26 review articles on AQbD, none exclusively focuses on UHPLC, while 52 research papers detail its pharmaceutical applications. This review bridges this gap by consolidating reported methods and advancements in risk assessment, experimental design, and optimization strategies for defining the method operable design region (MODR). Screening designs like Plackett-Burman design (PBD) and risk assessment tools like Ishikawa diagrams identify critical method parameters (CMPs), while response surface methodology (RSM)-based models optimize performance. The impact of stationary phases, mobile phase composition, and flow rate adjustments is examined, emphasizing ethylene-bridged hybrid octadecylsilane columns and mobile phase trends favoring water-acetonitrile (CAN) combinations with formic acid (FA) or ammonium acetate. Gradient elution is frequently applied for complex separations, with optimized flow rates (0.2-0.5 mL/min) enhancing efficiency and sustainability. Unlike previous reviews, this study systematically evaluates AQbD-driven UHPLC, offering critical insights for regulatory compliance, lifecycle management, and future pharmaceutical analysis advancements.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-21"},"PeriodicalIF":4.2,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144274317","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":"Microfluidic Systems for Isolation of White Blood Cells: From Design to Practical Applications.","authors":"Sanjay Mane, Dhiraj B Puri, Vadiraj Hemadri, Sunil Bhand, Siddhartha Tripathi","doi":"10.1080/10408347.2025.2514795","DOIUrl":"https://doi.org/10.1080/10408347.2025.2514795","url":null,"abstract":"<p><p>White blood cells (WBCs) are key immune cells that defend against infections and regulate immunity. For accurate diagnosis, WBCs must be separated from red blood cells (RBCs), which can interfere with analysis. Microfluidic methods provide an efficient solution for high-purity WBC isolation, utilizing miniaturized devices that need minimal blood and enable on-chip disease detection and cell counting, thus enhancing point-of-care accessibility. This review focuses on passive microfluidic techniques, known for their simplicity and scalability, which separate WBCs by leveraging factors like RBC concentration, channel geometry, and flow dynamics. The low WBC-to-RBC ratio (1:1000) remains a major challenge, with few current technologies integrating WBC isolation and disease detection. This work emphasizes the principles and applications of passive separation methods and examines biological assays of isolated WBCs. Additionally, we discuss commercial devices and highlight opportunities for innovation in microfluidic platforms to address existing gaps, particularly in improving diagnostic efficiency and usability. By advancing versatile and user-friendly technologies, microfluidic systems have the potential to revolutionize point-of-care diagnostics and healthcare delivery.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-25"},"PeriodicalIF":4.2,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144282756","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}
Gibin George, Raghav G R, Neethu Rose Thomas, Sivasankar Rao Ede, Shivamurthy B, Abhinav K Nair, Senthil T
{"title":"Gold Nanoparticles-Based Gas Sensors: A Comprehensive Review of Design, Mechanisms, and Applications.","authors":"Gibin George, Raghav G R, Neethu Rose Thomas, Sivasankar Rao Ede, Shivamurthy B, Abhinav K Nair, Senthil T","doi":"10.1080/10408347.2025.2512174","DOIUrl":"10.1080/10408347.2025.2512174","url":null,"abstract":"<p><p>Accurate detection of various gases is possible using gold nanoparticles (AuNPs) owing to their distinct physical, chemical, optical, and electronic properties. The review highlights the synergic properties of AuNPs, which allow them to detect many hazardous and greenhouse gases, such as NO<sub>2</sub>, H<sub>2</sub>S, CO, NH<sub>3</sub>, volatile organic compounds (VOCs), etc. The role of AuNPs in enhancing the performance of gas sensors, with a particular focus on the detection of toxic and environmentally significant gases at trace levels, is also discussed. The novelty of this work lies in its comprehensive analysis of strategies to tune the sensitivity and selectivity of AuNPs-based gas sensors through controlled variation in particle size, shape, and surface functionalization. Furthermore, their hybridization with other nanomaterials like graphene, carbon nanotubes (CNTs), and metal oxides to enhance the performance is discussed in detail. Altogether, this article presents the role of AuNPs in enhancing the performance of gas-sensing devices. In addition, the application of AuNPs-based gas sensors in various fields of science and engineering is discussed briefly. Moreover, the challenges of AuNPs-based sensors from an industrial point of view are covered toward the end of this article.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-39"},"PeriodicalIF":5.2,"publicationDate":"2025-06-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144265448","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}
Yunes M M A Alsayadi, Raghav Dogra, Vimal Arora, Aditya Shiven
{"title":"Innovations in the Detection of N-Nitrosamine Impurities in Pharmaceuticals: Analytical and Regulatory Challenges.","authors":"Yunes M M A Alsayadi, Raghav Dogra, Vimal Arora, Aditya Shiven","doi":"10.1080/10408347.2025.2512443","DOIUrl":"10.1080/10408347.2025.2512443","url":null,"abstract":"<p><p>The emergence of N-nitrosamine impurities (NAIs) in pharmaceutical products has raised significant global concern due to their confirmed carcinogenic and genotoxic potential. Their presence in widely prescribed medications like metformin, ranitidine, and valsartan has triggered widespread recalls and prompted stringent guidelines by agencies like the USFDA and EMA. Despite technological advancements, the detection and quantification of NAIs at the trace level remain analytically challenging, primarily due to their structural diversity and exceptionally low permissible thresholds for detection. Given the recent surge in regulatory scrutiny and product recalls, this review offers an up-to-date critical evaluation of the origin, mechanism of formation, toxicological implications, and evolving regulatory framework for NAIs. Particular emphasis is placed on the state-of-the-art analytical techniques, including LC-MS, GC-MS, and emerging high-resolution mass spectrometry (HRMS) platforms, along with current practices in sample preparation and method validations. Methodological gaps, including challenges in sample preparation and instrument-specific limitations, are thoroughly analyzed to propose future strategies for robust, high-throughput, and regulatory-compliant analysis of NAIs in complex pharmaceutical matrices. A comprehensive literature search spanning 2018-2025 was performed using PubMed, Web of Science, ScienceDirect, and Scopus. Keywords, such as \"nitrosamine impurities\", \"N-nitrosodimethylamine (NDMA)\", and \"regulatory guidelines\" were used to select articles relevant to ongoing method optimization and harmonization to ensure consistent monitoring and mitigation of NAIs. This work also aims to serve as a valuable resource for pharmaceutical scientists, chemists, toxicologists, and regulatory professionals in their commitment to enhance drug safety and protect public health.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-26"},"PeriodicalIF":4.2,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144257543","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}
Niluh Indria Wardani, Thidarat Samkumpim, Untika Pengsomjit, Mohamed Aly Saad Aly, Nur Nadhirah Mohamad Zain, Waleed Alahmad
{"title":"Assessing the Environmental Sustainability of Gel Electromembrane Extraction Approaches: A Critical Evaluation of the Greenness.","authors":"Niluh Indria Wardani, Thidarat Samkumpim, Untika Pengsomjit, Mohamed Aly Saad Aly, Nur Nadhirah Mohamad Zain, Waleed Alahmad","doi":"10.1080/10408347.2025.2513012","DOIUrl":"https://doi.org/10.1080/10408347.2025.2513012","url":null,"abstract":"<p><p>This review evaluates gel electromembrane extraction (G-EME) as an environmentally friendly alternative to conventional extraction methods. By replacing hazardous organic solvents with biodegradable gels, such as agarose, agar, polyacrylamide, and chitosan, G-EME adheres to the core principles of green analytical chemistry, significantly reducing waste production. The review systematically compares various G-EME approaches-including conventional, miniaturized, additive-enhanced, and sensing modalities-using a suite of greenness assessment tools (NEMI, ESA, complexGAPI, AGREE, AGREEprep, and Hexagon-CALIFICAMET) to provide a comprehensive evaluation of their environmental impact. Key findings indicate that while traditional G-EME methods offer substantial improvements over older techniques, further advancements through miniaturization and incorporation of functional additives can lead to even greater sustainability and analytical performance. However, challenges such as limited extraction efficiency for certain analytes and the need for broader application scopes persist. This review not only highlights the current state of G-EME but also identifies critical research gaps and encourages the development of more versatile and sustainable G-EME strategies for diverse analytical applications.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-19"},"PeriodicalIF":4.2,"publicationDate":"2025-06-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144224633","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":"An Overview of Thermal Methods Within the Analytical Framework of Cultural Heritage Studies.","authors":"Mina Magdy","doi":"10.1080/10408347.2025.2511142","DOIUrl":"https://doi.org/10.1080/10408347.2025.2511142","url":null,"abstract":"<p><p>The article offers an overview of thermal methods in the field of heritage conservation and research. Thermal analysis encompasses a family of analytical methods in which the property of a sample is monitored to gain a deeper understanding of material properties under various thermal conditions. Thermal methods can provide profound insights into the thermal behavior of heritage materials, including thermogravimetric analysis (TGA), differential thermal analysis (DTA), differential scanning calorimetry (DSC), thermo-mechanical analysis (TMA), thermodilatometric analysis (TDA), dynamic mechanical analysis (DMA), dielectric thermal analysis (DETA), thermal conductivity (TC), infrared thermography (IRT), and thermoluminescence (TL). These methods serve as a valuable means of recording thermal events across a broad range of temperatures, such as glass transition temperature, melting temperature, crystallization temperature, specific heat capacity, thermal expansion coefficient, thermal curing, thermal shrinkage, TC, and thermal imaging. Combining multiple methods in a single measurement enhances the collection of more information simultaneously. Thermo-kinetic parameters play a crucial role in interpreting the results obtained from thermal analysis to predict the behavior of materials at different temperatures and understand the underlying mechanisms driving thermal transformations. The key advantage of thermal analysis practice is to answer questions regarding materials performance, materials selection, conservation treatments, and preventive measures.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-18"},"PeriodicalIF":4.2,"publicationDate":"2025-06-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144224632","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}
Fan Wang, Siyu Fu, Shutong He, Chen Chen, Shoudong Chen, Qi Liu, Dongsheng Wang
{"title":"Functionalized Cellulose Derivatives: Challenge or Opportunity in the Field of Chiral and Achiral Sensing.","authors":"Fan Wang, Siyu Fu, Shutong He, Chen Chen, Shoudong Chen, Qi Liu, Dongsheng Wang","doi":"10.1080/10408347.2025.2512176","DOIUrl":"https://doi.org/10.1080/10408347.2025.2512176","url":null,"abstract":"<p><p>Cellulose is recognized as an abundant, renewable, and optically active carbohydrate polymer resource. Among numerous cellulose derivatives, microcrystalline cellulose derivatives primarily consist of ester derivatives such as benzoate, phenyl carbamate, and formate. These complex derivatives have stable helical configurations and abundant recognition sites. Moreover, the polymer chain can also amplify the recognition signal, which can significantly enhance the sensitivity and binding affinity of the recognition group to specific substrates, thereby improving their overall performance in targeted interaction. They exhibit excellent sensing performance and demonstrate significant potential in both chiral and non-chiral sensing applications. The development of sensing materials through grafting fluorescent functional groups onto microcrystalline cellulose frameworks is identified as a crucial approach for high-value utilization of cellulose. This review systematically summarized the applications of microcrystalline cellulose derivatives in chiral sensing from the perspectives of chiral chromatographic separation and chiral fluorescence sensing, while their emerging applications in non-chiral sensing were reviewed through the lens of metal ion recognition. Future directions and application prospects were discussed for phenyl carbamate and formate derivatives of cellulose in both chiral and non-chiral domains. The findings were expected to provide valuable references for researchers engaged in microcrystalline cellulose functionalization studies and to inspire novel approaches for advanced cellulose modification.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-18"},"PeriodicalIF":4.2,"publicationDate":"2025-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144215177","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}
Karolina Morawska, Tomasz Sikora, Michał Grabka, Monika Wiśnik-Sawka, Zygfryd Witkiewicz
{"title":"Early Detection of Threat Agents, a Review of Bioimmunosensors and Their Prospects.","authors":"Karolina Morawska, Tomasz Sikora, Michał Grabka, Monika Wiśnik-Sawka, Zygfryd Witkiewicz","doi":"10.1080/10408347.2025.2507346","DOIUrl":"https://doi.org/10.1080/10408347.2025.2507346","url":null,"abstract":"<p><p>Early detection of biological threat agents plays a crucial role in public health protection, food safety, and environmental monitoring. Bioimmunosensors, utilizing specific antigen-antibody interactions, represent a promising technology in these applications due to their high sensitivity and specificity. This review explores the current state of knowledge regarding bioimmunosensors, highlighting recent technological innovations, such as integration with nanotechnology, microfluidic techniques, and the development of novel detection platforms based on optical and electrochemical biosensors. Key challenges in their development, including the stability of biological detection elements, cost reduction, and the scalability of technology for real-world applications, are also discussed. The analysis of future application prospects points to the growing potential of bioimmunosensors in areas such as medical diagnostics, pathogen detection in the environment, food quality control, and bioterrorism defense. Increased integration of bioimmunosensors with the Internet of Things (IoT) systems and the development of portable analytical devices may revolutionize the approach to monitoring and rapid response to biological threats in the coming years.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-15"},"PeriodicalIF":4.2,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144198452","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}
Yujin Yang, Huijuan Qi, Xiangting Hou, Min Gao, Shaohua Gong
{"title":"Recent Advances (2019-2025) in Mercury Ion Detection.","authors":"Yujin Yang, Huijuan Qi, Xiangting Hou, Min Gao, Shaohua Gong","doi":"10.1080/10408347.2025.2511136","DOIUrl":"https://doi.org/10.1080/10408347.2025.2511136","url":null,"abstract":"<p><p>As a persistent bioaccumulative toxin, mercury ion (Hg<sup>2+</sup>) presents grave environmental and public health risks due to their extreme toxicity and neurological damage potential. The advancement of reliable Hg<sup>2+</sup> detection methodologies become imperative for safeguarding ecological security and food supply chains. In recent years, different signal output modes have been explored for Hg<sup>2+</sup> detection. This review systematically summarizes the latest detection techniques and strategies for Hg<sup>2+</sup> based on electrochemical signal, fluorescence signal, SERS signal and colorimetric signal. Innovation designs of functional materials, small molecules, nanoprobes and strategies for Hg<sup>2+</sup> detection have been introduced and their detection performances including sensitivity, selectivity and portability are compared with each other. The comparison results show that some methods can achieve ultrasensitive detection of Hg<sup>2+</sup> at fM level. In addition, the challenges and perspective for Hg<sup>2+</sup> detection have been discussed. The review is expected to provide insights for the development of highly sensitive and portable detection tools for Hg<sup>2+</sup>, and promote the transformation of Hg<sup>2+</sup> detection technology from the laboratory to industrialization.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-17"},"PeriodicalIF":4.2,"publicationDate":"2025-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144191608","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}
Huiqin Pan, Guyu Zhao, Yannan Tan, Shui Miao, Xiuhong Mao, Shen Ji, Heng Zhou, Qing Hu
{"title":"Liquid Chromatography Coupled to High-Resolution Mass Spectrometry for High-Throughput Pesticide Residue Detection: Methodological Advances and Insights for Herbal Medicine Analysis.","authors":"Huiqin Pan, Guyu Zhao, Yannan Tan, Shui Miao, Xiuhong Mao, Shen Ji, Heng Zhou, Qing Hu","doi":"10.1080/10408347.2025.2511140","DOIUrl":"https://doi.org/10.1080/10408347.2025.2511140","url":null,"abstract":"<p><p>The safety evaluation of herbal medicines faces a critical challenge due to exogenous pesticide residues, where traditional detection methods struggle to address the dual complexity of highly variable phytochemical matrices and trace-level multi-residue contaminants. Recent regulatory shifts emphasizing large-scale detection have positioned liquid chromatography coupled with high-resolution mass spectrometry (LC-HRMS) as a transformative solution. This review systematically examines cutting-edge LC-HRMS workflows tailored for complex herbal matrices, with three pivotal technical dimensions: (1) Matrix-specific optimization spanning from QuEChERS-based sample preparation to chromatographic separation protocols that reduce matrix interferences; (2) Intelligent data acquisition strategies balancing selectivity and coverage through adaptive MS/MS triggering and narrow-window fragmentation; (3) Integrated analytical frameworks combining targeted screening with expanding pesticide databases and non-targeted approaches leveraging retrospective HRMS data mining. While LC-HRMS has demonstrated exceptional performance in food safety domains, its application in herbal medicine analysis remains constrained by insufficient method harmonization and underutilized data potential. We critically evaluate how emerging techniques, including comprehensive two-dimensional liquid chromatography, ion mobility mass spectrometry, structure-informed parameter prediction, suspect screening based on biotransformation, and metabolomics-driven non-targeted screening, could overcome current limitations in compound identification confidence and pesticide coverage. By bridging technological advancements with the challenges faced in practical residue analysis of herbal medicines, this review provides actionable guidelines to empower researchers in developing robust, future-proof analytical schemes that meet evolving regulatory standards and public health expectations.</p>","PeriodicalId":10744,"journal":{"name":"Critical reviews in analytical chemistry","volume":" ","pages":"1-15"},"PeriodicalIF":4.2,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144172892","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}