Green Metric Assessment of Analytical Techniques for the Imidazole Prodrug Olmesartan Medoxomil: A Comparative Analysis
Analytical methods for Olmesartan Medoxomil (OM) have gained significant attention in pharmaceutical analysis, aligning with the green chemistry principles. Various spectroscopic and chromatographic techniques have been developed to ensure accurate, cost-effective, and environmentally friendly quantification of the OM. UV spectroscopic strategies offer simplicity, rapidity, and minimal solvent consumption, making them ideal for routine pharmaceutical analysis. Ultraviolet (UV) spectrophotometric methods have several limitations includes need of chromophores, overlapping spectra, and less sensitivity. High-Performance Liquid Chromatography (HPLC) methods remain the gold standard for OM quantification because of their excessive sensitivity, specificity, and reproducibility but having draw backs of expensive nature of the equipment, the necessity for trained personnel, the extended duration required for analysis, the use of costly and occasionally hazardous solvents, and the complexity of sample preparation. The greenness of analytical methods is assessed using tools such as Green Analytical Procedure Index (GAPI) and the AGREE metric, which evaluate solvent consumption, energy efficiency, and waste generation. Whiteness assessment and the use of the Blue Applicability Grade Index (BAGI) provides an additional holistic assessment, integrating performance, sustainability, and analytical performance. This review highlights the greenness and blueness assessment of the analytical methods available for the determination of Olmesartan Medoxomil from 2008 to date. Overall, UV spectroscopy (Method 8) is the most practical and sustainable method, with the best AGREE (0.67) and BAGI scores (75). HPLC (Method 20) is fairly green with an AGREE score (0.67) and HPLC (Method 16 and Method 24) practical with BAGI scores (77.5).
Analytical Methods for Daptomycin Determination: Applications in Biological Matrices and Pharmaceutical Formulations
Daptomycin (DAP) is a cyclic lipopeptide antibiotic indicated for the treatment of serious Gram-positive infections, including complicated skin and soft tissue infections, bacteremia, and right-sided infective endocarditis. Due to its clinical significance, the reliable quantification of DAP in both biological and pharmaceutical matrices is essential for therapeutic drug monitoring, pharmacokinetic studies, and quality control. This review provides a comprehensive and structured overview of analytical methods developed for DAP determination, based on literature search of Web of Science, PubMed, and ScienceDirect encompassing publications from 2008 to 2025, and including fifty-one studies involving biological matrices - such as plasma, serum, urine, bone, wound fluid, and muscle - and eight studies focused on pharmaceutical formulations. The reviewed methods include liquid chromatography coupled with ultraviolet or mass spectrometric detection, as well as alternative techniques such as spectrofluorimetry, spectrophotometry, voltammetry, and capillary-zone electrophoresis. Sample preparation strategies for analyzing biological matrices, protein precipitation and solid-phase extraction, have also been systematically discussed. By offering a comparative perspective grounded in experimental evidence, this review aims to guide researchers and laboratory professionals in selecting appropriate DAP quantification strategies for both clinical and pharmaceutical applications.
Analytical Approaches for Parasitic Biomarkers Diseases Discovery: Trends and Perspectives of Metabolomics in the Clinical Laboratory
The clinical and laboratory diagnosis of diseases caused by parasites - helminths and protozoa - presents several limitations. To solve these gaps, new technologies have been developed. Metabolomics is in the spotlight due to its potential for discovering biomarkers that can be useful in the clinical laboratory. In this systematic review, we evaluate the main biomarkers identified in parasitic infections by metabolomics and the perspectives for their use in the clinical laboratory. The search was conducted on PubMed, SciELO Brasil and LILACS-Bireme platforms with the combination of descriptors "metabolomics" and "parasites" or "helminth" or "protozoan". A total of 65 studies met our eligibility criteria. , and were the most studied parasites. Experimental infections were more commonly performed, indicating that metabolomics is in the process of being standardized for its application in laboratory routine. Among all metabolites, amino acids were the most commonly observed in parasitic infections. In the context of metabolite detection, the majority of studies employed mass spectrometry (MS), whereas only a limited number utilized nuclear magnetic resonance (NMR) spectroscopy. The main advantage of employing metabolites in diagnostics is their early detectability, overcoming limitations imposed by the parasite's life cycle and excretion dynamics. We demonstrate the potential of metabolomics tools as alternatives to complement the conventional parasitological diagnosis.
Advances in Pretreatment Sample and Applications of Selective Material for Sample Treatment in the Analysis of Benzene, Phenol, Hydroquinone, and Catechol in Biological and Environmental Samples
Benzene (Bz), phenol (Phen), hydroquinone (HQ), and catechol (CAT) are volatile organic compounds (VOCs) (monoaromatic compounds) considered environmental contaminants as a consequence of human and industrial activities. Prolonged exposure affects human health, causing cancer and death. Researchers have developed and applied analytical methodologies in pretreatment samples and detection techniques to analyze these monoaromatic compounds at trace and ultra-trace concentration levels. The present study is focused on an in-depth review and comparative analysis of removal and extraction techniques, summarizing the sources (analytical matrix), interaction modes (analyte-sorbent) in extraction techniques, solid phase extraction (SPE), dispersive solid phase extraction (DSPE), magnetic solid phase extraction (MSPE), and microextraction techniques), and the determination methods (chromatographic and non-chromatographic) applied in the analysis of these monoaromatic compounds in complex matrices.
A Review of Analytical Techniques for the Analysis of Oral Smokeless Products and Heated Tobacco Products
The increasing popularity in recent years of oral smokeless products (OSPs) and heated tobacco products (HTPs) has raised significant public health and regulatory concerns. Although these products are often marketed as less harmful alternatives to traditional cigarettes, they differ considerably in both design and, more importantly, in their chemical composition. Notably, they contain potentially dangerous compounds such as tobacco-specific nitrosamines, flavorings, heavy metals, and nicotine, which can be addictive and harmful to human health at certain concentrations. This work provides an overview of the analytical techniques and methods used to analyze OSPs and HTPs, including the determination of moisture content and pH, the extraction of various compounds, the generation of HTP aerosol, and non-targeted analysis, as well as the quantification of extracted compounds using gas chromatography, liquid chromatography, and spectroscopy. Identifying and quantifying the chemical composition of OSPs and HTPs is essential for assessing their health impact and developing proper regulatory standards regarding these products.
Techniques for Gallstone Analysis: From Traditional Methods to Present Day Cutting-Edge Technologies- A Panoramic Review
Gallstones are crystalline bodies with a heterogeneous composition in relation to the type, mainly categorized as cholesterol, pigment, or mixed stones. Their physicochemical properties need to be identified to make appropriate diagnoses, establish effective treatments, and implement sound prevention measures. This review has gathered a comprehensive set of techniques applied to characterizing gallstones. Spectroscopic techniques including Fourier-transform infrared (FTIR), Raman, and Ultraviolet-visible spectroscopy (UV-Vis) spectroscopy provide crucial functional groups and molecular structures and identify organic constituents such as cholesterol, bilirubin, and calcium bilirubinate etc. Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS) and Laser-Induced Breakdown Spectroscopy (LIBS) deliver surface-sensitive elemental information, in the case of TOF-SIMS especially, to trace metals such as Fe, Cu, Zn, as well as contaminants like Pb and Cd. The thermal techniques like Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC) extract differences in cholesterol content and heat stability between the different categories of stone. Complementary methods like X-ray diffraction (XRD) and scanning electron microscopy (SEM) dissect mineral phases and surface topography. Differential elemental quantitation with inductively coupled plasma optical emission spectroscopy (ICP-OES) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS) determines Ca, Mg, and Fe to be major contributors to the development of gallstones. This review highlights the diagnostic value of elemental signatures, crystalline morphology, and thermophysical transitions in determining gallstone ethology and composition and help us in dealing with pathogenesis, with multi technique combination providing the most comprehensive description. Finally, the integration of analytical methods provides a solid basis for clinical and research gallstone analysis.
The Role of Micelles in Modern Sample Preparation Techniques for More Efficient and Sustainable Practices
Micelles, formed from surfactants, offer alternative media for separation and detection techniques, addressing challenges such as sample complexity, method sensitivity and selectivity, analysis cost and time, and environmental impact. The critical micelle concentration (CMC) plays a pivotal role in micelle formation, with normal and reverse micelles being the main structures observed. Additionally, niosomes and liposomes contribute to sample preparation methods. Polymeric micelles exhibit a core-shell configuration, allowing for modification of their properties. Micellar systems find application in various techniques, including cloud point extraction (CPE), coacervation extraction, microextraction, and supercritical fluid extraction. CPE offers environmentally friendly and cost-effective extraction, enhancing analyte solubility and detection limits. The review further discusses the applications of micellar systems in CPE, including the analysis of hazardous organic impurities and the purification of biological compounds. Metal-CPE is explored as a method for extracting organically chelated metals. The utilization of micellar systems in sample preparation showcases their potential in improving analytical methodologies.
Current Advances of Sample Preparation Techniques for Detection of Growth Promoters from Meat Samples
The unregulated use of antibiotic residues in meat samples poses a significant threat to society, as it facilitates the growth of antibiotic-resistant bacterial species and negatively impacts the human immune system. The regulatory agencies created the maximum residue levels for individual growth promoters, including steroids, β-agonists, and various veterinary drugs. Therefore, it is essential to monitor the antibiotics and growth promoters in the meat samples for the safety of public health. To identify the sub - therapeutic level of antibiotic residues in animal-originated food samples, sample preparation techniques play a vital role because of its complex nature of the sample matrix and, subsequently, various regulation bodies set the stringent minimum criterion limits. Liquid-liquid extraction, Solid-phase extraction, and QuEChERS are the most common analytical techniques for antibiotic detection in meat. In this review, we highlighted the recent advances in sample preparation techniques such as traditional and microextraction techniques to monitor growth promoters in meat samples, emphasizing their applications, limitations, and future perspectives. The review also aligns with the sustainable development goals by promoting action that enhance life on land, ensure good health and well-being, and encourage industry innovation for sustainable establishment in related studies.
Need for Reassessment of the Quality Assurance in Food Products: Meta Analysis of Mass Spectrometry of Pesticide Residues in Food Products
While mass spectrometry (MS) excels at identifying pesticides due to its high resolution, its accuracy for quantifying pesticide concentrations is problematic. This meta-analysis employed a representative random sample of publications; consequently, alternative samples might generate divergent observations. The criteria for selecting publications for the meta-analysis are comparability of technologies with each group of GC-MS/MS and LC-MS/MS, simultaneous analysis of multiple pesticides, and easy access to the data. Nevertheless, contemporary studies follow analogous analytical principles. The meta-analysis findings comprise a full re-calculation of reported data from 28 analyzed publications (14 GC-MS/MS, 14 LC-MS/MS) on pesticide quantification. Outliers were reported by only one publication. Analysis (using PoPC) revealed a critical bias-negative calibration slopes were systematically discarded, indicating researchers likely repeated calibrations until obtaining positive slopes. This invalidates the statistical validity of the methods. The ensuing quantifications were therefore postulated to be unreliable. The calibration slopes were too shallow, leading to extremely high relative uncertainties (often ∼100% or more). This makes reliable quantification impossible. A matrix-effect problem was disclosed; the massive uncertainties mean the reported "abundant matrix effects" cannot be reliably distinguished from the measurement error itself. Claims about matrix effects were made with high precision but low accuracy. Due to the methodological bias and resulting high uncertainty, the actual concentration of pesticides in these studies remains scientifically undetermined. Potential bias may lead to uncertain conclusions, and issues with statistical methods and reproducibility were noted, warranting future attention. Pre-concentrating pesticides could improve reliability, as the PoPC showed lower variability at higher concentrations.
Review on LC-MS/MS Methodologies for Analysis of N-Nitrosamine Drug-Substance-Related Impurities
N-nitrosamine drug-substance-related impurities (NDSRIs) pose an important safety challenge in the pharmaceutical industry due to their potential carcinogenic and genotoxic properties. Their formation from secondary or tertiary amines within active pharmaceutical ingredients (APIs) and their structural similarity to the parent drug make their detection at trace levels a complex analytical task. Recognizing these risks, the nitrosamine class of impurities has been classified as a "cohort of concern" by global regulatory bodies, thereby requiring stringent control. This review provides a concise overview of the key factors driving NDSRI formation and highlights state-of-the-art analytical techniques, such as LC-MS/MS, for their precise quantification. In response to this risk, global regulatory authorities have mandated rigorous risk assessment and mitigation strategies. This review is an essential resource for pharmaceutical scientists and manufacturers, offering the critical knowledge needed to control these impurities and ensure the safety of manufactured medicines. It also addresses regulatory considerations for establishing the acceptable intake (AI) of NDSRIs, incorporating the recently approved CPCA concepts, and includes an overview of LC-MS/MS quantification methods for NDSRIs published between January 2022 and April 2025.
Exploring the Pharmaceutical Significance and Analytical Landscape of Ropinirole: An In-Depth Review of an Indole-Based Dopaminergic Therapeutic Agent
Ropinirole, an indole-based dopamine agonist with high affinity for D2, D3, and D4 receptors, is widely used for Parkinson's disease (PD) and restless legs syndrome (RLS) due to its neuroprotective effects and ability to mitigate levodopa-induced motor complications. Despite well-established clinical efficacy and pharmacokinetics characterized by rapid absorption, hepatic metabolism CYP1A2, and predominant renal excretion - comprehensive analytical profiling remains incomplete, particularly in stability-indicating methods, forced degradation studies, and impurity characterization. This review systematically evaluates ropinirole's pharmacological properties, formulation strategies (immediate-release [IR] and extended-release [ER]), and marketed products. It critically analyzes analytical methodologies, including HPLC, UHPLC (guided by Analytical Quality by Design [AQbD]), HPTLC, UV spectrophotometry, and LC-MS/MS, focusing on sensitivity, specificity, robustness, and regulatory compliance. HPLC dominates routine quantification, while UHPLC and LC-MS/MS excel in impurity profiling and pharmacokinetic studies. However, inconsistent reporting of forced degradation and stability assessments reveals critical gaps that hinder regulatory compliance and quality assurance. The indole moiety's influence on therapeutic action and analytical behavior underscores the need for tailored, validated methods addressing stability and impurities. Recommendations include developing robust stability-indicating protocols, implementing controlled stress testing, employing orthogonal techniques, and ensuring mass balance verification using advanced detectors and hyphenated tools. This review bridges pharmacological and analytical perspectives, advocating for next-generation platforms to enhance method sensitivity, selectivity, and reproducibility. Adopting validated, stability-indicating approaches will strengthen regulatory acceptance and improve therapeutic monitoring and quality control (QC) for ropinirole formulations.
Recent Advances of Electrochemical Sensors Based on Carbon-Based Nanoparticles for Dental Infection and Periodontitis Detection
Effective treatment, lower long-term expenses, and the avoidance of significant consequences, such as tooth loss, depend on the early identification of periodontitis (PD) and other dental diseases. Dentists can significantly enhance patient outcomes by implementing preventive measures and individualized treatment regimens through early diagnosis and treatment. Novel biosensors are crucial because they identify specific biomarkers in biofluids, including saliva and gingival crevicular fluid (GCF), enabling early, precise, and noninvasive diagnosis. Compared to traditional approaches, our methodology provides a faster and more accurate assessment of periodontal health. For this reason, electrochemical biosensors are a game-changing technology that provides quick, noninvasive, and reasonably priced point-of-care (POC) diagnostics. These sensors detect disease-specific biomarkers in GCF and saliva, enabling the accurate and real-time evaluation of periodontal health. The use of carbon nanoparticles (CNPs), such as graphene (GPH), carbon nanotubes (CNTs), and graphene quantum dots (GQDs), which improve sensor performance due to their large surface area and improved electrical conductivity, is a significant development in this sector. This study highlights the importance of CNPs in the development of highly sensitive and accurate electrochemical biosensors for the diagnosis of Parkinson's disease and other oral disorders. Lastly, we discuss the present drawbacks and potential future developments of this intriguing diagnostic methodology.
Dioxins and Dioxin-Like Compounds: Current Challenges in Sensing and Future Perspectives
Polychlorinated dibenzo--dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) are highly toxic, persistent organic pollutants that pose severe environmental and public health risks due to their widespread distribution in air, water, and soil. Although global emissions have decreased from 287 kg I-TEQ to 97 kg I-TEQ by 2025, concerning concentrations persist in environmental matrices, with soil contamination ranging from 0.017 ppt in China to 540,000 ppt in Japanese paddy fields. These observations highlight the urgent need for sensitive, selective, and rapid detection strategies capable of addressing trace-level dioxin contamination. Conventional analytical approaches, including gas chromatography mass spectrometry (GC-MS), high-resolution mass spectrometry (HRMS), biosensors, and optical detection techniques, have facilitated monitoring efforts but remain limited by high cost, operational complexity, restricted stability, and suboptimal selectivity. Cyclodextrin (CD)-based sensing platforms have demonstrated significant success in detecting a wide range of environmental pollutants owing to their well-defined hydrophobic cavities and lipophilic interiors, which enable the formation of stable inclusion complexes in aqueous environments. Given the strongly lipophilic nature of dioxins, CDs are conceptually well-suited as recognition scaffolds for selective molecular binding. However, to date, no experimental CD-based fluorescent or colorimetric systems have been reported for dioxin detection, and investigations have been limited to computational simulations predicting binding affinity and selectivity. These insights underscore a critical gap in sensor development and highlight the potential of CD-derived optical sensors as a next-generation platform for highly selective, sensitive, and rapid dioxin monitoring.
Rising Millifluidics: A Practical Approach Towards Wide Application
This study provides a comprehensive review of millifluidic devices, the devices that handle liquids on the millimeter scale. Millifluidics is being developed as an extension of microfluidic technology. Millifluidic devices share a similar design, fabrication, and characterization approach compared to microfluidics; however, millifluidic devices have the advantages of low cost, high throughput, and visible fluid flow, and are much more accessible to researchers in various fields. The application fields of millifluidics are also similar to those of microfluidics, for example, chemical/bio reactions, micro/nanoparticle synthesis, droplet generation, and detection. According to recent developments in microfluidics and millifluidics, in certain fields, millifluidics tends to partially replace microfluidics, e.g., particle synthesis. In addition, more fluidics handling devices (e.g., test cartridges) have combined features of fluid manipulation structures in the micrometer and millimeter ranges. Artificial intelligence and machine learning have also been used for the design and control of millifluidic devices. This study provides a new insight into the conventional application field of microfluidics, which could be a low-cost, more accessible, high-throughput solution to real-world tasks in the chemical, biomedical, and environmental fields.
A Critical Review on Non-Enzymatic Electrochemical Strategies for L-Glutamate Monitoring in Biological Systems
An essential excitatory neurotransmitter and metabolic intermediary, L-glutamate is vital for multiple physiological functions, such as memory, learning, and synaptic transmission. A variety of neurological and neurodegenerative conditions have been attributed to aberrant glutamate levels, emphasizing the significance of reliable and continual monitoring in biological systems. Despite their remarkable sensitivity, classical analytical techniques are sometimes compromised by intricate procedures, outrageous expenses, and constrained applicability for point-of-care applications. However, enzymatic electrochemical sensors exhibit higher selectivity; their high production costs and inconsistent functioning make them impractical for long-term use. Nonenzymatic electrochemical sensors, on the other hand, have become a viable alternative due to their superior stability, cost-effectiveness, and ease of manufacture. Recent advancements in nonenzymatic glutamate sensors are thoroughly investigated in this review, with a focus on innovative material strategies that enable enhanced sensitivity, selectivity, and detection limits over a wide concentration range. The aforementioned strategies comprise metal and metal oxide nanostructures, carbon-based platforms, and hybrid composites. It also explores substantial breakthroughs in sensor architecture, operation, and practical applications in intricate biological matrices. These enzyme-free systems' expanding prominence in contemporary biosensing technologies is illustrated by their promise in therapeutic diagnostics, neurochemical research, and point-of-care testing.
Advances and Challenges in LSD Detection: Analytical Techniques, Matrix Selection, and Validation Gaps in Forensic Toxicology
Lysergic acid diethylamide (LSD) remains a significant forensic and public health concern due to its widespread abuse and association with drug-facilitated crimes. Detecting LSD and its analogs in biological specimens, particularly postmortem matrices, presents analytical challenges stemming from its low dosage, rapid metabolism, and structural similarities to novel lysergamides. This review critically examines trends in validated analytical methods for LSD detection in forensic toxicology. A systematic review of literature from 1978 to 2025 was conducted using databases, such as PubMed, ScienceDirect, and Google Scholar. The analysis focused on reported methodologies for LSD and its metabolites across various matrices, including blood, urine, hair, oral fluid, and vitreous humor. Extraction techniques (LLE, SPE, DLLME) and analytical platforms (GC-MS/MS, LC-MS/MS, CE-MS) were compared, with emphasis on validation parameters, such as sensitivity, specificity, recovery, LOD, LOQ, matrix effects, and stability. The review identifies LC-MS/MS as the most sensitive and widely validated technique; however, discrepancies remain in matrix-specific validations and stability assessments. Challenges include the lack of certified reference materials for LSD analogs, matrix-dependent degradation, and limited methods for emerging sample types, such as dried blood spots (DBS). Few studies fully comply with modern forensic validation guidelines, limiting the reproducibility and admissibility of results in legal settings. This review highlights critical gaps in current forensic LSD detection protocols and underscores the need for standardized, validated methods applicable to diverse matrices. Future research should prioritize the development of rapid, eco-friendly, high-throughput methods capable of detecting LSD and its analogs at ultra-trace levels.
Silver Nanomaterial-Doped Layered Double Hydroxides for Advanced Electrochemical Sensing: A Critical Review
Silver-doped layered double hydroxides (Ag-LDHs) have gained prominence as a high-performing class of electroactive materials suited to advanced electrochemical sensors, exhibiting remarkable sensitivity, selectivity, and long-term stability in environmental, biomedical, and food analytical settings. Silver incorporation not only narrows the band gap of the LDH host but also endows the heterostructure with enhanced electrical conductivity, surface reactivity, and rapid redox cycling, clearly outpacing both pure and conventional-metal-doped LDH architectures. These hybrids utilize the inherent ion-exchange capacity and extensive surface area of LDHs, further enhanced by integration with functional materials such as carbon allotropes, metal oxides, and conductive polymers, leading to a synergistic improvement in electrocatalytic performance and mechanical resilience. Despite several studies on these composites, a comprehensive study that critically compares structural designs, synthesis methods, and functional performance in electrochemical sensing is absent. This article addresses that gap by providing a systematic, side-by-side comparison of contemporary Ag-LDH synthetic routes, surface-modification protocols, and sensing metrics. Application-centric evaluations encompass the quantification of pollutants in aqueous matrices, the diagnosis of disease-relevant biomarkers, and the deterrence of unsafe food items. Enduring barriers, including the scale-up of manufacture with consistent quality, stability over extended operational lifetimes, and the realization of cost-competitive fabrication, are rigorously appraised alongside prospective pathways, such as eco-conscious synthesis protocols, hybrid nanoscale architectures, and machine-learning-augmented ideation of sensor designs. Collectively, the compiled findings furnish a coherent roadmap for the translational maturation of Ag-LDH-based electrochemical sensing technologies that transcend proof-of-principle and advance toward the reliable point-of-care deployment beyond controlled laboratory environs.
Application of Raman and ATR-MIR Spectroscopy in Colorectal Cancer Diagnosis Combined with Chemometrics Techniques: A Review
Colorectal Cancer (CC) is recognized as the third most prevalent cancer worldwide and constitutes a major cause of cancer-related fatalities among both genders. Current diagnostic approaches for CC exhibit several notable limitations; they are frequently invasive, their accuracy may vary based on the operator and the patient, and they might lack sufficient precision. Raman Spectroscopy (RS) and Infrared (IR) spectroscopy have surfaced as promising alternatives owing to their potential as swift and noninvasive diagnostic modalities. Nevertheless, spectroscopic methods produce extensive and intricate datasets characterized by overlapping peaks and subtle differences, which complicates direct visual interpretation. This review is dedicated to examining the chemometric techniques utilized in RS and IR spectroscopy for the diagnosis and evaluation of CC. Throughout this paper, we explore the experimental applications of chemometrics in conjunction with RS and IR spectroscopy. Chemometric algorithms, when integrated with RS and IR spectroscopy, have demonstrated their efficacy as robust tools for the detection, classification, and analysis of various colorectal cancer matrices. Indeed, it has been shown how chemometrics can be effectively applied in a variety of CC analysis.
Voltammetric Determination of Alkaloids and Metabolites: From Structural Classification to Bioanalytical Applications and Regulatory Insights
Alkaloids represent one of the most significant classes of compounds of natural and synthetic origin due to their pronounced biological activity and broad applications in pharmacy, medicine, and toxicology. Their determination in complex matrices such as biological fluids or pharmaceutical formulations necessitates the use of highly sensitive, selective, and reliable analytical techniques. Among these, electrochemical methods, particularly voltammetry, provide rapid, cost-effective, and precise detection. This review systematically evaluates voltammetric approaches for the determination of alkaloids and their metabolites, with a particular focus on studies published over the last two decades (2005-2025). More than 90 publications have been critically analyzed, covering voltammetric methodologies applied to 26 alkaloids and their metabolites, and highlighting key trends in electrode selection, experimental conditions, and strategies to enhance analytical performance. Special emphasis is placed on linking the electrochemical behavior of alkaloids to their chemical structure and functional group affiliation, providing insights into reaction mechanisms and detection sensitivity. The review also incorporates illustrative schemes of representative alkaloids and their electrochemical transformations, demonstrating practical applications for pharmaceutical analysis, food safety, and forensic monitoring. By critically assessing the strengths and limitations of current methodologies, this work offers a valuable resource for researchers and professionals in electroanalytical chemistry, pharmaceutical sciences, biomedicine, and toxicology, supporting the development of more selective and efficient voltammetric techniques for alkaloid investigation.
