BMC Chemistry最新文献

{"title":"Correction: In silico drug evaluation by molecular docking, ADME studies and synthesis, characterization, biological activities, DFT, SAR analysis of the novel Mannich bases","authors":"Veysel Tahiroğlu, Kenan Gören, Gül Kotan, Haydar Yüksek","doi":"10.1186/s13065-025-01644-6","DOIUrl":"10.1186/s13065-025-01644-6","url":null,"abstract":"","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12477802/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145190546","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Qualitative and quantitative assessment of related substances for ketoconazole cream based on national drug sampling inspection in China","authors":"Changying Xin,&nbsp;Yanbin Xun,&nbsp;Yi Zhou,&nbsp;Fei Wang,&nbsp;Feng Li,&nbsp;Qiong Wu,&nbsp;Panpan Wu,&nbsp;Demin Ding,&nbsp;Liqun Liu,&nbsp;Longshan Zhao,&nbsp;Lihong Yang","doi":"10.1186/s13065-025-01629-5","DOIUrl":"10.1186/s13065-025-01629-5","url":null,"abstract":"<div><h3>Background</h3><p>Establishing an analytical method for the detection of related substances in ketoconazole cream is essential for improving product quality standards and ensuring the safety of this formulation.</p><h3>Methods</h3><p>In the 2024 National Drug Sampling Specification, we developed a novel high-sensitivity high-performance liquid chromatography (HPLC) method that effectively separates six known impurities, four preservatives, and one antioxidant present in ketoconazole creams. These creams were sourced from random market sampling and exhibited variations in prescription composition across 14 different manufacturers. Subsequently, we conducted the extraction, isolation, and characterization of common unknown impurities from these creams using mass spectrometry (MS), nuclear magnetic resonance spectroscopy (NMR), and infrared (IR) techniques. Furthermore, the structural analysis of unknown impurities within a specific enterprise was performed using high-resolution mass spectrometry and specialized software.</p><h3>Results</h3><p>The established method has been thoroughly validated, demonstrating its specificity, accuracy, sensitivity, and excellent repeatability, thereby confirming its suitability for determining related substances in ketoconazole creams from various manufacturers. This method allowed for both quantitative and qualitative evaluations of impurity content across different manufacturers, identifying sulfonated impurities in ketoconazole creams for the first time and analyzing their formation mechanisms. Furthermore, strategies to reduce these impurities were proposed through correlation analysis and process validation. Additionally, this study innovatively introduced a solvent smoothing agent to mitigate solvent effects, thereby preventing the degradation of the active pharmaceutical ingredient (API) during the heating and dissolution process of the cream matrix. This technique is applicable to the pretreatment of various cream-related substance determinations.</p><h3>Conclusions</h3><p>This method provides substantial reference value for establishing analytical methods for related substances in Ketoconazole cream and offers technical support for regulatory agencies in evaluating the quality of Ketoconazole cream.</p></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-09-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01629-5","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145169633","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Entrance-channel plugging by natural sulfonamide antibiotics yields isoform-selective carbonic anhydrase IX inhibitors: an integrated in silico/ in vitro discovery of the lead SB-203207","authors":"Emadeldin M. Kamel,&nbsp;Noha A. Ahmed,&nbsp;Saleh Maodaa,&nbsp;Bassam A. Abuamarah,&nbsp;Sarah I. Othman,&nbsp;Adil Abalkhail,&nbsp;Faris F. Aba Alkhayl,&nbsp;Al Mokhtar Lamsabhi","doi":"10.1186/s13065-025-01634-8","DOIUrl":"10.1186/s13065-025-01634-8","url":null,"abstract":"<div><p>Carbonic anhydrase IX (CA IX) is a hypoxia-induced pH regulator whose over-expression drives tumor progression and therapy resistance. Most CA inhibitors rely on zinc chelation and lack isoform selectivity, limiting clinical utility. Here we combined structure-based docking, 200 ns molecular-dynamics simulations and steady-state enzyme kinetics to assess four rare sulfonamide/sulfone natural products (altemicidin, SB-203207, SB-203208 and sulfadixiamycin A) as non-classical CA IX blockers. Docking located every ligand at the mouth of the catalytic funnel (<b>−</b> 7.2 to <b>−</b> 9.4 kcal mol⁻¹) without coordinating Zn²⁺. MD-derived free-energy landscapes and MM/PBSA calculations confirmed durable entrance-bound complexes for SB-203207/208 and sulfadixiamycin A (ΔG_total ≈ − 24 to <b>−</b> 27 kcal mol⁻¹) but frequent dissociation of altemicidin ( ≈ − 2 kcal mol⁻¹). Per-residue-decomposition pinpointed a hydrophobic wall (Leu91, Val121, Phe131, Leu198, Pro202, Phe243) plus anchoring H-bonds to Thr199 and Gln92. Recombinant-enzyme assays validated these predictions: SB-203207, SB-203208 and sulfadixiamycin A inhibited CA IX esterase activity with IC₅₀ = 73 ± 1, 99 ± 2, and 114 ± 3 nM, respectively, versus 41 ± 1 nM for reference acetazolamide. Crucially, SB-203207 showed marked selectivity, with SI = 28 (hCA I/IX) and SII = 14 (hCA II/IX), far exceeding the &gt; 10-fold benchmark; SB-203208 and sulfadixiamycin A also met this threshold, whereas altemicidin was both weaker (1.90 µM) and less selective. Steady-state esterase kinetics were consistent with non-competitive inhibition and <i>K</i>_i values that mirrored the IC₅₀ rank order. SwissADME/ADMETlab profiling highlighted SB-203207 as the most developable hit. Together, these results establish entrance-channel plugging as an alternative mechanism for CA IX inhibition, identify SB-203207 as a potent and isoform-selective lead.</p></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01634-8","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145110469","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development of two ion-selective sensors for determining benzydamine hydrochloride in the presence of its oxidative degradant across various matrices: greenness, whiteness, and blueness appraisals","authors":"Khadiga M. Kelani,&nbsp;Ragab A. M. Said,&nbsp;Mohammad A. El‑Dosoky,&nbsp;Lobna M. Abd El Halim,&nbsp;Ahmed R. Mohamed","doi":"10.1186/s13065-025-01625-9","DOIUrl":"10.1186/s13065-025-01625-9","url":null,"abstract":"<div><p>Two sensitive and selective ion-selective electrodes (ISEs) were developed for the determination of benzydamine hydrochloride (BNZ·HCl): a conventional polyvinyl chloride (PVC) electrode and a coated graphite all solidstate ion-selective electrode (ASS-ISE). Both sensors were constructed using an ion-pair formed between BNZ⁺ and the lipophilic anion tetraphenylborate (TPB⁻), incorporated into the sensing membranes. The sensors exhibited near-Nernstian responses with slopes of 58.09 And 57.88 mV/decade, over a Linear range of 10^–5–10^–2 M, and detection Limits of 5.81 × 10^–8M and 7.41 × 10^–8 M, respectively. They demonstrated high accuracy and precision for the determination of BNZ·HCl in pure form, pharmaceutical cream, and biological fluids, with no matrix interference. The method also proved stability-indicating, successfully detecting BNZ·HCl in the presence of its oxidative degradant. Validation was performed according to ICH guidelines, and the method showed strong environmental compatibility based on greenness, whiteness, and blueness assessments, supporting its suitability for sustainable pharmaceutical analysis.</p></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01625-9","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145110468","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development and validation of a sustainable spectrofluorimetric method for simultaneous quantification of amlodipine and aspirin using genetic algorithm-enhanced partial least squares regression","authors":"Taha Alqahtani,&nbsp;Ali Alqahtani,&nbsp;Ahmed A. Almrasy","doi":"10.1186/s13065-025-01624-w","DOIUrl":"10.1186/s13065-025-01624-w","url":null,"abstract":"<div><p>The widespread clinical utilization of amlodipine-aspirin combinations, despite potential pharmacodynamic interactions and the high prevalence of drug-drug interactions in cardiovascular patients, necessitates robust analytical methods for pharmaceutical quality control and therapeutic drug monitoring. Current analytical approaches face limitations including lengthy analysis times, substantial solvent consumption, and high operational costs. This study presents a novel spectrofluorimetric method coupled with genetic algorithm-enhanced partial least squares (GA-PLS) regression for simultaneous quantification of amlodipine and aspirin in pharmaceutical formulations and biological plasma samples. Synchronous fluorescence spectroscopy at Δλ = 100 nm in 1% sodium dodecyl sulfate-ethanolic medium enhanced spectral characteristics, while chemometric approaches were essential to address remaining spectral overlap for accurate quantification. The GA-PLS approach demonstrated superior performance over conventional partial least squares regression, achieving relative root mean square errors of prediction (RRMSEP) of 0.93 and 1.24 for amlodipine and aspirin respectively, with limits of detection of 22.05 and 15.15 ng/mL. Genetic algorithm optimization reduced spectral variables to approximately 10% of the original dataset while maintaining optimal model performance with only two latent variables. Method validation according to ICH Q2(R2) guidelines demonstrated excellent accuracy (98.62–101.90% recovery) and precision (RSD &lt; 2%) across the analytical range of 200–800 ng/mL. Statistical comparison with established HPLC reference methods showed no significant differences, while application in human plasma achieved recoveries of 95.58-104.51% with coefficient of variation below 5%. Multi-dimensional sustainability assessment using the MA Tool and RGB12 whiteness evaluation achieved an overall score of 91.2%, demonstrating clear superiority over conventional HPLC-UV (83.0%) and LC-MS/MS (69.2%) methods across environmental, analytical, and practical dimensions. The developed method provides a sustainable, cost-effective alternative for routine pharmaceutical analysis, demonstrating enhanced performance through intelligent variable selection and improved operational efficiency.</p></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01624-w","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145110470","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Electrochemical synthesis of spirooxindole-pyranopyrazole and spirooxindole-chromene derivatives as inhibitors of acetylcholinesterase","authors":"Reem M. Elsapagh,&nbsp;Eman O. Osman,&nbsp;Ahmed M. Hafez,&nbsp;Hala B. El-Nassan","doi":"10.1186/s13065-025-01618-8","DOIUrl":"10.1186/s13065-025-01618-8","url":null,"abstract":"<div>\u0000 \u0000 <p>An efficient, reliable, and cost-effective approach was applied for the electrochemical synthesis of spirooxindole-pyranopyrazole and spirooxindole-chromene derivatives. The compounds were prepared in high yields and short reaction times by electrochemical synthesis using LiClO₄ as an electrolyte and Cu/graphite as electrodes. The synthesized products were tested as acetylcholinesterase (AChE) inhibitors. Compounds <b>4e</b> and <b>6b</b> demonstrated potent inhibitory activity against AChE enzyme with IC₅₀ values of 0.51 and 0.84 mM, respectively. Both compounds showed low cytotoxicity and preserved normal cell morphology, confirming their safety. The in-silico study of the ADME properties of compounds <b>4e</b> and <b>6b</b> revealed a high bioavailability score without affecting any of the CYP isoforms. Kinetic studies were performed to detect the mode of inhibition of the most active compounds, <b>4e</b> and <b>6b.</b> Also docking studies were performed for both compounds, to evaluate their binding patterns compared to donepezil. The docking and kinetic studies indicated that both compounds inhibited AChE through a competitive mechanism predominantly targeting the catalytic anionic site CAS.</p>\u0000 </div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-09-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01618-8","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145057727","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"UPLC-ESI-QTRAP-MS/MS identification and antioxidant activity of hawthorn with different infestation levels","authors":"Yunxia Cheng,&nbsp;Zhenying Liu,&nbsp;Jian Yang,&nbsp;Zhimao Chao","doi":"10.1186/s13065-025-01611-1","DOIUrl":"10.1186/s13065-025-01611-1","url":null,"abstract":"<div><p>This study employed UPLC-ESI-QTRAP-MS/MS metabolomics technology (MRM mode) to analyze two hawthorn varieties infested by <i>Plodia interpunctella</i> (Hüb.) and <i>Tribolium castaneum</i> (Hbst.) at different infestation levels (3 biological replicates per treatment), aiming to investigate the alterations in flavonoid metabolites and their effects on antioxidant activity under different infestation levels. A total of 32 previously characterized flavonoids were identified, covering flavonols, isoflavones, dihydroflavones, flavones, flavanols, dihydroflavonols, and chalcones. The observed flavonoid reduction following infestation aligned with established mechanisms of insect-plant interactions, including potential contributions from both direct feeding and metabolic consumption and associated microbial metabolism. Using screening criteria of <i>P</i> &lt; 0.05 with FC &gt; 1.5 for upregulation or ≤ 0.8 (for downregulation), eight shared differential metabolites strongly associated with insect infestation were identified. Spearman correlation analysis revealed a significant association (<i>P</i> &lt; 0.05) between insect-induced reduction in flavonoid cs and the decline in antioxidant capacity, with this correlation being closely related to the characteristic structural groups of the flavonoid compounds. Epicatechin and genistin were selected as effective markers for characterizing the reduction of antioxidant activity in hawthorn after insect infestation. This study identified significant associations among insect infestation, flavonoid variation, and antioxidant activity in hawthorn. These findings provide insights into the co-occurring changes in nutritional and functional properties during infestation, offering potential indicators for post-harvest quality monitoring.</p></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01611-1","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144923293","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A chitosan-lignin biocomposite adsorbent for RO16 dye and Cr(VI) heavy metal removal from aqueous solutions: new interpretations via experiments and statistical physics analysis","authors":"Ismahene Ben Khemis,&nbsp;Fatma Aouaini,&nbsp;Salah Knani,&nbsp;Ghadeer Mohsen Albadrani,&nbsp;Besma Graba,&nbsp;Mohamed Houcine Dhaou,&nbsp;Abdelmottaleb Ben Lamine","doi":"10.1186/s13065-025-01621-z","DOIUrl":"10.1186/s13065-025-01621-z","url":null,"abstract":"<div><p>A biocomposite composed of chitosan and lignin was synthesized for the removal of dyes and metals from aqueous solutions. The structural and surface properties of the adsorbent were characterized using FT-IR spectroscopy, SEM micrograph, X-ray diffraction, nitrogen adsorption-desorption isotherms, BJH pore size distribution, and zeta potential evolution. This study also presented a physicochemical investigation of the adsorption mechanism of reactive orange 16 (RO16) dye and hexavalent chromium (Cr(VI)) ions on chitosan-lignin biocomposite, using both experimental adsorption data and theoretical modeling based on statistical physics theory to elucidate the underlying interactions. An advanced statistical physics adsorption model, namely heterogeneous monolayer model with two functional groups (HMLM2FG), was employed to simulate the adsorption behavior, indicating that RO16 and Cr(VI) interacted with two distinct functional groups on the chitosan + 50% lignin surface. This model enabled detailed stereographic and energetic studies of the tested adsorption systems. Hence, stereographic analysis revealed that the studied adsorbent functional groups preferentially capture the attached species with <i>n</i> &gt; 1 at specific temperatures, suggesting a multi-ionic mechanism with significant aggregation. The total maximum adsorbed quantities of chitosan-lignin adsorbent, determined by the proposed model HMLM2FG, were found to be 59.43–79.76 mg/g for RO16 and 52.06–72.61 mg/g for Cr(VI). Chitosan + 50% lignin demonstrated then greater efficiency in removing RO16 and Cr(VI) from aqueous solutions, showing an exothermic adsorption process characterized by adsorption energies ranging from 4.88 to 16.97 kJ/mol. These energy values were consistent with physisorption mechanisms. Overall, this study combined experimental findings with a theoretical approach to offer a novel microscopic and macroscopic analysis of the adsorption behavior of two major industrial pollutants on chitosan-lignin biocomposite.</p><p><b>Clinical trial number</b>: Not applicable.</p></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01621-z","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144923348","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Significant impacts of metal ions from ancient oceans on nucleoside phosphorylation","authors":"Qian Wu,&nbsp;Shuyi Lu,&nbsp;Chao Zhang,&nbsp;Wenda Zhong,&nbsp;Hua Zhao,&nbsp;Yufen Zhao,&nbsp;Biling Huang","doi":"10.1186/s13065-025-01619-7","DOIUrl":"10.1186/s13065-025-01619-7","url":null,"abstract":"<div><p>Nucleotides, such as 5’-AMP and ATP, are essential biomolecules in modern organisms. The phosphorylation of nucleosides to generate nucleotides occurs in complex prebiotic environments, where metal ions played a pivotal role, particularly in the metal-rich ancient oceans. Investigating the impact of prebiotic metal ions on nucleotide formation is critical to understanding their contributions to chemical evolution. Herein, we examined adenosine phosphorylation in the presence of various metal ions (Mn²⁺, Fe²⁺, Fe³⁺, Co²⁺, Ni²⁺, and Mg²⁺) under wet-dry cycling conditions. The results reveal that these systems can produce 5’-AMP, 2’/3’-AMP, 2’,3’-cAMP, ADP, ATP, c-di-AMP, and the oligomeric nucleotide pApA. The yields of these nucleotides varied depending on the metal ions present and were lower than in the metal-free system. The concentrations and combinations of metal ions in a solution markedly impact the levels of nucleotides. Notably, 5’-AMP emerged as the dominant product, exhibiting high 5’-regioselectivity, strongly supporting the RNA world hypothesis. Moreover, Co²⁺ and Ni²⁺ enhanced nucleotide cyclization, while iron proved crucial for oligonucleotide formation. Intriguingly, hydrolysis experiments revealed nucleotides interconversion. Furthermore, metal accelerated hydrolysis of nucleotides compared to the metal-free system, directly impacting the efficiency and final yield of nucleoside phosphorylation. These findings underscore the multifaced role of metal ions in regulating phosphorylation, facilitating hydrolysis, and promoting nucleotides interconversion, thereby advancing our understanding of prebiotic chemical evolution and providing empirical support for environments rich in metals, as plausible settings for the emergence of primordial RNA-based life.</p></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01619-7","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144923292","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A novel RP-HPLC approach for simultaneous determination of dapagliflozin, linagliptin, and metformin in pharmaceutical formulations","authors":"Samkit Shah,&nbsp;Rajendra Kotadiya","doi":"10.1186/s13065-025-01620-0","DOIUrl":"10.1186/s13065-025-01620-0","url":null,"abstract":"<div><p>A simple, precise, and stability-indicating reverse-phase high-performance liquid chromatography method was developed and validated for the simultaneous estimation of dapagliflozin, linagliptin, and metformin hydrochloride in fixed-dose combination tablets. Chromatographic separation was achieved using a Phenomenex Luna C18 column (250 × 4.6 mm, 5 μm) with a mobile phase consisting of acetonitrile and phosphate buffer (pH 6.8) in a 40:60 v/v ratio; the buffer was modified to the mentioned pH with triethylamine and orthophosphoric acid. The flow rate was maintained at 0.8 mL/min, with detection at 230 nm. The method demonstrated excellent linearity within the ranges of 20–140 µg/mL for metformin hydrochloride, 0.2–1.4 µg/mL for linagliptin, and 0.6–2.8 µg/mL for dapagliflozin, with correlation coefficients (R²) &gt; 0.995. The validation was performed as per ICH Q2 (R2) guidelines, confirming the method’s accuracy, precision (%RSD &lt; 2%), robustness, specificity, and sensitivity. Forced degradation studies under acidic, basic, oxidative, thermal, and photolytic conditions confirmed the method’s capability to resolve each analyte from its degradation products, affirming its stability-indicating nature. Application of the method to a commercial formulation yielded assay values of 101.41%, 100.04%, and 99.73% w/w for metformin hydrochloride, linagliptin, and dapagliflozin, respectively. These results validate the method’s applicability for routine quality control and stability testing of multi-drug antidiabetic formulations.</p></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01620-0","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144923281","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}