Lingyu Shen , Wenxing Li , Yupeng Chen , Daogang Guan , Aiping Lu , Anqi Xu
{"title":"SuHeXiang Wan in the treatment of stroke: Prediction potentially active metabolites using a combination of in silico analysis and experimental viability assessment","authors":"Lingyu Shen , Wenxing Li , Yupeng Chen , Daogang Guan , Aiping Lu , Anqi Xu","doi":"10.1016/j.jpba.2025.117313","DOIUrl":"10.1016/j.jpba.2025.117313","url":null,"abstract":"<div><div>SuHeXiang Wan (SHXW) is a renowned traditional Chinese medicine (TCM) prescription for treating stroke, but its active components remain largely unidentified. This study aimed to screen potential active compounds of SHXW and reveal their underlying mechanisms in stroke treatment. Ingredients and compounds in SHXW were obtained from TCM databases and subjected to initial screening based on ADMET and physicochemical properties, followed by target gene prediction for each filtered compound. A comprehensive network of filtered compound–target gene–stroke pathogenic gene was constructed and optimized using a multi-objective optimization algorithm. Seventeen potential active compounds were identified, which primarily influenced neuroactive ligand-receptor interactions, arachidonic acid metabolism, and several signaling pathways including PI3K-Akt, calcium, and cAMP. Using an oxygen-glucose deprivation and reoxygenation (OGD/R) model, cirsiliol was identified as the lead compound, significantly enhancing cell viability and morphology, decreasing apoptosis, and reducing oxidative stress and inflammatory responses. Molecular docking and dynamics simulations revealed that cirsiliol stably binds to the NADPH binding pocket of CBR1 protein. Further experiments demonstrated that cirsiliol decreased 4-hydroxynonenal (4-HNE, a substrate of CBR1) levels. This study provides a methodological framework for screening active compounds in TCM prescriptions. The neuroprotective effects of cirsiliol against ischemic stroke merit further investigation.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117313"},"PeriodicalIF":3.1,"publicationDate":"2026-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733402","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Electrochemical multi-drug sensors: Current advances, challenges, and future perspectives","authors":"Vildan Sanko , Mustafa Ali Güngör , Filiz Kuralay","doi":"10.1016/j.jpba.2025.117303","DOIUrl":"10.1016/j.jpba.2025.117303","url":null,"abstract":"<div><div>The rapid growth of the pharmaceutical industry has highlighted the importance of controlling both the quality control process and appropriate dosing in drug purchasing to a critical level. In addition to this, pharmaceutical pollutants can harm the environment, especially water resources, creating a need for low-cost, sensitive, selective, and portable technologies to monitor personal health and environmental applications. Because monitoring more than one drug simultaneously provides convenience in terms of diagnosis and treatment, it increases the drug monitoring capacity and features. Therefore, various electrochemical methods and micro/nanomaterials integration have been employed to achieve well-separated peaks for drug molecules and enhance sensitivity. However, detecting more than one drug using an electrochemical method remains a challenging research topic. This review discusses electrochemical multi-drug (bio)sensing techniques, focusing on future trends. For this purpose, drugs were categorized as anticancer, anti-inflammatory, antidepressant, antibacterial, antiviral, and antifungal according to the area they act on. Moreover, integration of herbal drugs, which are highlighted by their rising therapeutic importance and intricate phytochemical compositions, has found place in electrochemical sensing. Current electrochemical (bio)sensors that detect multiple drugs for each group were discussed. In addition, mixed-type multi-drugs containing different drug groups were also discussed in a separate section.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117303"},"PeriodicalIF":3.1,"publicationDate":"2026-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733400","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A universal LC-HRMS workflow integrating targeted and untargeted strategies for rapid and comprehensive metabolite profiling of oligonucleotide-based therapeutics","authors":"Yuqing Zhao , Yue Yang , Mingshe Zhu , Chongzhuang Tang","doi":"10.1016/j.jpba.2025.117298","DOIUrl":"10.1016/j.jpba.2025.117298","url":null,"abstract":"<div><div>Metabolite profiling and identification of oligonucleotide-based therapeutics (OBTs) is important in drug discovery and development. Conventional liquid chromatography-high resolution mass spectrometry (LC-HRMS) methods (using ProMass, BioPharma Finder) are effective for targeted analysis of predictable nuclease-derived metabolites but often miss unexpected non-nuclease-mediated ones. This study aimed to develop a universal analytical workflow for comprehensive metabolite profiling of multiple classes OBTs by integrating BioPharma Finder for targeted identification with a Background Subtraction Filter (BSF) for untargeted detection of unexpected biotransformation products. Inclisiran, a GalNAc-conjugated siRNA, was used as a model compound. Samples incubated with rat, monkey, and human liver S9 fractions were analyzed by the LC-HRMS workflow. As a result, a total of 25 (22 predicted +3 unpredicted) inclisiran metabolites were identified across the three species. BioPharma Finder enabled rapid and sensitive identification of 22 predicted metabolites, supported by automated fragment ion assignment. The BSF data processing revealed 22 metabolites not present in control samples, including SS-1GalNAc, SS-2GalNAc, and SS-3GalNAc, which were missed by BioPharma Finder and likely formed via β-<em>N</em>-acetylglucosaminidase-mediated biotransformation. The structures of BSF-detected metabolites were confirmed by comparison with BioPharma Finder-identified metabolites or characterized through manual MS/MS interpretation. Product ion spectra of these metabolites showed weak or absent diagnostic ion (<em>m</em>/<em>z</em> 94.936), a characteristic fragment of phosphorothioate-containing oligonucleotides, suggesting that the product ion filtering of this ion exhibits limited utility in discovering inclisiran metabolites. Overall, the integrated LC-HRMS workflow shows strong potential as a universal platform for biotransformation studies of OBTs.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117298"},"PeriodicalIF":3.1,"publicationDate":"2026-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145714504","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ying Xu , Nan Li , Xu Li , Xuan Cui , Rui Ju , Mingming Li , Jiaxiu Zhao , Fei Han
{"title":"Integrated analysis strategies reveal the pharmacodynamic substances and action mechanisms of Huangqi San in the treatment of Alzheimer’s disease","authors":"Ying Xu , Nan Li , Xu Li , Xuan Cui , Rui Ju , Mingming Li , Jiaxiu Zhao , Fei Han","doi":"10.1016/j.jpba.2025.117251","DOIUrl":"10.1016/j.jpba.2025.117251","url":null,"abstract":"<div><div>Alzheimer's disease (AD), as a neurodegenerative disorder characterized primarily by memory impairment in its early stages, imposes a heavy burden on society and medical resources. This study aims to investigate the therapeutic effect of Huangqi San (HQS) on AD and elucidate its potential mechanism of action. This study analyzed the rat serum after treated by HQS using UHPLC-Q-Exactive Orbitrap MS, and identified the potential active components of HQS. Subsequently, key targets and pathways were identified through network pharmacology and molecular docking techniques, and were verified in PC12 cells damaged by Aβ<sub>25–35</sub>. The verification methods included cell viability assays, analysis of inflammatory/oxidative stress markers, and regulation of the PI3K/AKT/MAPK pathway. The results showed that a total of 40 serum adsorption components and 70 common targets were identified. Network analysis revealed that the PI3K-AKT, MAPK and Rap1 signaling pathways were at the core of the network. Molecular docking demonstrated strong binding affinity between 10 core components (e.g., isoliquiritigenin, moracin M) and pivotal targets (BCL2, MAPK3, PTGS2). <em>In vitro</em> validation showed HQS significantly attenuated Aβ<sub>25–35</sub>-induced neurotoxicity by enhancing cell viability, suppressing apoptosis, reducing pro-inflammatory cytokines (TNF-α, IL-1β, IL-6) and oxidative markers (MDA, ROS, CYP2E1) while elevating GSH-Px activity. Moreover, HQS can bidirectionally regulate PI3K/AKT/MAPK pathways via upregulating PI3K/AKT/ERK1/2 and inhibiting JNK/p38 phosphorylation. In conclusion, this study innovatively established HQS as a multi-component/multi-target candidate drug for the treatment of AD. Its mechanism of action is related to its synergistic regulation of PI3K/AKT/MAPK-mediated neuroprotection. This comprehensive approach provides an example for interpreting complex traditional Chinese herbal preparations.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117251"},"PeriodicalIF":3.1,"publicationDate":"2026-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145578795","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Laerissa Reveil , Maria Lasaosa , Amanda Furman , A.M. Iqbal O’Meara , Matthew S. Halquist
{"title":"Corrigendum to “Validation and quantitation of six neurotransmitters in rat plasma and brain using liquid chromatography quadrupole-time-of-flight mass spectrometry” [J. Pharm. Biomed. Anal., 267 (2026) 117145]","authors":"Laerissa Reveil , Maria Lasaosa , Amanda Furman , A.M. Iqbal O’Meara , Matthew S. Halquist","doi":"10.1016/j.jpba.2025.117314","DOIUrl":"10.1016/j.jpba.2025.117314","url":null,"abstract":"","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117314"},"PeriodicalIF":3.1,"publicationDate":"2026-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733399","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Jeremy P. Koelmel , Paula S. Ramos , Kaylie Anne Costa , Krystal J. Godri-Pollitt , Diane L. Kamen , John A. Bowden
{"title":"Lipidome changes indicate oxidative stress, inflammation, and specific loss of glycerophosphoserine inflammatory protection in patients with lupus","authors":"Jeremy P. Koelmel , Paula S. Ramos , Kaylie Anne Costa , Krystal J. Godri-Pollitt , Diane L. Kamen , John A. Bowden","doi":"10.1016/j.jpba.2025.117302","DOIUrl":"10.1016/j.jpba.2025.117302","url":null,"abstract":"<div><div>Systemic lupus erythematosus (SLE, lupus) is a chronic autoimmune disease which has a complex etiology and suffers from both high false positive rates and false negative rates in diagnosis and classification. Substantial lipid changes have been observed previously in lupus patients, hence we carried out the most comprehensive lipidomics study in lupus to date using LipidMatch Flow. In this study, we investigated various sub-categories of lupus including lupus nephritis, active versus non-active lupus, as well as comparisons to non-lupus controls. A total of 1105 unique lipids spanning 36 lipid classes (or sub-classes) were annotated in blood plasma samples; of these, 111 lipids changed significantly between controls and active lupus. We determined for the first time, specific oxidized lipid markers, with oxidized triacylglycerols being the most significantly increased lipid sub-class in active lupus as compared to controls. Other indicators of oxidative stress included decreased lipids containing ether linkages and/or polyunsaturated fatty acids. Increased Cer(d18:1/16:0) and decreased C20–22 containing species (especially C20:4) indicated an inflammatory response in patients with active lupus. Furthermore, we determined a significant decrease of glycerophosphoserines, which are known inflammation suppressors, in patients with lupus and a decrease in Coenzyme Q9 and Q10; supplementation of lupus patients with Coenzyme Q10 has been shown to be protective [1–4]. Several unique lipids with unknown biology are also shown to significantly changed in active lupus. Many of these trends were also observed in non-active lupus, suggesting lipidomics related changes may occur early in disease development. In conclusion, this comprehensive lipidomics study expands our knowledge of the lipid alterations associated with lupus, providing insights into disease pathogenesis and depleted lipids, which could serve as therapeutic targets.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117302"},"PeriodicalIF":3.1,"publicationDate":"2026-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733396","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Berfu Bekmez , Fatma Budak , Ahmet Cetinkaya , Sibel A. Ozkan
{"title":"Selective and sensitive determination of amlodipine in binary mixtures using a nanomaterial-assisted molecularly imprinted electrochemical sensor","authors":"Berfu Bekmez , Fatma Budak , Ahmet Cetinkaya , Sibel A. Ozkan","doi":"10.1016/j.jpba.2025.117316","DOIUrl":"10.1016/j.jpba.2025.117316","url":null,"abstract":"<div><div>Cardiovascular disease, one of the leading causes of death in developing countries, is mainly caused by the combination of arterial hypertension and dyslipidemia as major risk factors. Amlodipine (AML) is a calcium channel blocker that inhibits extracellular calcium influx across the membranes of myocardial and vascular smooth muscle cells, thereby reducing contraction and dilating coronary and systemic arteries. This study aimed to design a nanoparticle-supported molecularly imprinted polymer (MIP)-based electrochemical sensor with selective and sensitive sensitivity for the quantitative analysis of both binary drug mixtures and AML. The modified sensor was produced by the electropolymerization (EP) method in the presence of 4-aminobenzoic acid (4-ABA) as the functional monomer, pyrrole (Py) as the copolymerization monomer, and the target molecule AML. The incorporation of silver nanoparticles (AgNPs) into the MIP-based electrochemical sensor increased its active surface area and porosity. The AML/4-ABA-co-Py@AgNPs/MIP-GCE sensor was characterized both electrochemically (electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV)) and by surface morphology (scanning electron microscopy (SEM)). The quantification of AML was performed using differential pulse voltammetry (DPV) with the direct method in a 5.0 mM [Fe(CN)<sub>6</sub>]<sup>3-/4</sup> solution, yielding a linear range of 0.1–1.0 pM. The applicability and accuracy of the sensor were evaluated by recovery studies in tablet forms containing binary mixtures. In addition, to demonstrate the sensor's selectivity, a selectivity study was performed in the presence of components with chemical structures similar to those of AML, and its high selectivity was confirmed by the relative suppression factors for AML. In conclusion, this newly developed sensor for AML offers many advantages, such as selective, sensitive, fast, and inexpensive analysis.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117316"},"PeriodicalIF":3.1,"publicationDate":"2026-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733477","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Medapati Nikitha Lakshmi Suseela , Patharaj Gokul , Rajnish Kumar , Matte Kasi Viswanadh , Jyotsana Pandey , M. Sterlin Leo Hudson , Joseph Selvin , Madaswamy.S. Muthu
{"title":"Solid phase extraction of palbociclib from palbociclib-loaded therapeutic micelles: Novel synthesis of hybrid reduced graphene oxide–modified magnetic iron oxide (rGO@SiO2@Fe3O4)nanosorbent-based plasma extraction and pharmacokinetics study in rats","authors":"Medapati Nikitha Lakshmi Suseela , Patharaj Gokul , Rajnish Kumar , Matte Kasi Viswanadh , Jyotsana Pandey , M. Sterlin Leo Hudson , Joseph Selvin , Madaswamy.S. Muthu","doi":"10.1016/j.jpba.2025.117270","DOIUrl":"10.1016/j.jpba.2025.117270","url":null,"abstract":"<div><div>Accurate and sensitive quantification of anticancer agents in biological matrices is challenging yet crucial for pharmacokinetic evaluation and therapeutic monitoring. In this study, a reduced graphene oxide–modified magnetic iron oxide nanosorbent (<span><math><mrow><msub><mrow><mi>rGO@SiO</mi></mrow><mrow><mn>2</mn></mrow></msub><msub><mrow><mi>@Fe</mi></mrow><mrow><mn>3</mn></mrow></msub><msub><mrow><mi>O</mi></mrow><mrow><mn>4</mn></mrow></msub></mrow></math></span>) was synthesized via <em>in-situ</em> co-precipitation and the same was applied for the selective extraction and enrichment of palbociclib (PLB), using bosutinib (BSTB) as an internal standard. The nanosorbent was comprehensively characterized by electron microscopy with elemental mapping (FE-SEM/EDX), surface vibrational spectroscopy (ATR-FTIR), powder X-ray diffraction (PXRD), and superconducting quantum interference device (MPMS) magnetometer. The synthesized hybrid nanosorbent demonstrated favourable morphological, structural, and magnetic properties, enabling rapid magnetic separation and enhanced surface interactions. The established chromatographic analysis showed excellent linearity across 100–10,000 ng/mL, alongside a quantification limit of 100 ng/mL and a minimum detectable concentration of 50 ng/mL. Application of the developed method to rat plasma samples yielded good recovery and reproducibility, validating its performance in real biological matrices. In addition, PLB-loaded TPGS micelles (100, 125, and 150 mg) were successfully formulated, exhibiting particle sizes of 13.3–15.8 nm, supporting their potential for drug delivery applications. The integration of magnetic separability with enhanced sorption capacity makes <span><math><mrow><msub><mrow><mi>rGO@SiO</mi></mrow><mrow><mn>2</mn></mrow></msub><msub><mrow><mi>@Fe</mi></mrow><mrow><mn>3</mn></mrow></msub><msub><mrow><mi>O</mi></mrow><mrow><mn>4</mn></mrow></msub></mrow></math></span> a reusable and environmentally sustainable platform for plasma extraction. This work offers a promising strategy for sensitive, reliable, and environmental friendly quantification of PLB.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117270"},"PeriodicalIF":3.1,"publicationDate":"2026-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145622352","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Evaluation of photochemical behavior of ebastine and elucidation of its photoproducts","authors":"Kohei Kawabata , Yukina Tokunaga , Yoko Nunome , Shiori Akimoto , Naoto Uramaru , Masanori Inagaki , Hiroyuki Nishi","doi":"10.1016/j.jpba.2025.117288","DOIUrl":"10.1016/j.jpba.2025.117288","url":null,"abstract":"<div><div>Ebastine (EB) is a second-generation histamine H<sub>1</sub> receptor antagonist and utilized for the relief of allergy symptoms. In this study, the photodegradability of EB in an aqueous media was evaluated and the chemical structures of generated photoproducts were elucidated. EB photodegradation was monitored using high-performance liquid chromatography (HPLC), and two EB photoproducts were observed in HPLC chromatograms along with the decrease of EB contents in sample solutions. To elucidate their chemical structures, electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) analysis was carried out. From the mass to charge ratio values of molecular ion peaks and the fragmentation patterns, two EB photoproducts were designated as benzophenone and 4′-tert-butylacetophenone, respectively. Moreover, for the better understanding of EB photodegradation, photodegradation pathways of EB were speculated based on the structures of photoproducts. The photodegradation pathways of EB seemed to be an oxidative elimination of diphenyl methylene moiety and a Norrish type Ⅱ reaction. Finally, in silico toxicity prediction was performed for the estimation of toxicological potencies of EB photoproducts, suggesting the nature of EB might be changed by the photodegradation. In conclusion, two novel EB photoproducts were clarified and their formation mechanisms were proposed, which might make it possible to the better understanding of EB photodegradability.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117288"},"PeriodicalIF":3.1,"publicationDate":"2026-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145678054","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Azam Safarnejad , Fatma Budak , Ahmet Cetinkaya , Burcu Dogan-Topal , Sibel A. Ozkan
{"title":"Voltammetric analysis of entacapone, levodopa, and carbidopa in tablets: A chemometric approach","authors":"Azam Safarnejad , Fatma Budak , Ahmet Cetinkaya , Burcu Dogan-Topal , Sibel A. Ozkan","doi":"10.1016/j.jpba.2025.117275","DOIUrl":"10.1016/j.jpba.2025.117275","url":null,"abstract":"<div><div>The objective of the present work is to develop a voltammetric method for the determination of entacapone (ENT) in the presence of levodopa (LEV) and carbidopa (CAR) in synthetic mixtures and pharmaceutical formulations, using a multivariate approach. ENT is an inhibitor of Catechol-O-methyltransferase (COMT), used in the treatment of Parkinson’s disease as an adjunct for the combination therapy with LEV and CAR. With the optimized parameters in a pH 3.0 Britton-Robinson buffer, the quantitative analyses were assessed by the root mean square error in prediction (RMSEP), as well as the root mean square error of calibration (RMSEC) and the relative error of prediction (REP). The Radial Basis Function Artificial Neural Network (RBF-ANN) and Partial Least Squares regression (PLS) were applied for the determination of ENT in the presence of LEV and CAR. In the RBF-ANN model, the REP of 0.87 and RMSEP of 2.14<span><math><mo>×</mo></math></span>10<sup>−7</sup> are obtained for the test data when quantifying the ENT. The RBF model, as a nonlinear calibration method, was successful for predicting ENT concentration. To evaluate the validity of the recommended method, a commercial pharmaceutical tablet (Stalevo ® 200 mg) was analyzed. RBF model has the ability to overcome difficulties such as non-linearity and overlaps in the voltammograms.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117275"},"PeriodicalIF":3.1,"publicationDate":"2026-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145555398","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}