Journal of Chromatography B最新文献

{"title":"Sishen pill alleviates ulcerative colitis via the NLRP3/ASC/Caspase-1 signaling pathway: Comprehensive validation through UPLC-Q-TOF/MS, network pharmacology, molecular docking, and in vivo experiments","authors":"Qian Luo ,&nbsp;Hongping Long ,&nbsp;Chun Guo ,&nbsp;Xingxu Wei ,&nbsp;Xinyu Wang ,&nbsp;Haiyue Zhang ,&nbsp;Shuangyang Luo ,&nbsp;Zilong Liu ,&nbsp;Jiemin Liu ,&nbsp;Sainan Zhou ,&nbsp;Xiaoyuan Lin","doi":"10.1016/j.jchromb.2025.124735","DOIUrl":"10.1016/j.jchromb.2025.124735","url":null,"abstract":"<div><h3>Background</h3><div>The “Sishen Pill” (SSP) is a traditional Chinese medicinal formulation traditionally employed in the treatment of diarrhea attributed to spleen-kidney yang deficiency, and it has exhibited notable clinical efficacy in managing ulcerative colitis (UC). Nevertheless, the bioactive compounds and the underlying mechanisms by which SSP exerts its therapeutic effects on UC remain inadequately elucidated.</div></div><div><h3>Objectives</h3><div>This study sought to systematically elucidate the bioactive constituents and the mechanism of action of SSP in the treatment of UC through the application of ultra-high-performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF/MS), network pharmacology, molecular docking, and animal experimentation.</div></div><div><h3>Methods</h3><div>The chemical constituents of SSP were characterized using UPLC-Q-TOF/MS. Network pharmacology was employed to predict the principal chemical constituents and core targets of SSP in the context of UC treatment, while molecular docking was utilized to assess their binding affinities. Subsequently, a rat model of UC was established, and mechanistic validation was performed using a range of techniques, including hematoxylin and eosin (HE) staining, transmission electron microscopy, immunofluorescence staining, Western blotting, reverse transcription-polymerase chain reaction (RT-PCR), and enzyme-linked immunosorbent assay (ELISA).</div></div><div><h3>Results</h3><div>In this study, a total of 79 chemical constituents were identified in SSP. Through network pharmacology analysis, Citric acid, Eugenol, Daidzein, 7-Hydroxycoumarin, 4-Hydroxycoumarin, Astragalin, and Octadecenoic acid were determined to be the core chemical constituents, with Caspase-1 and IL-1β identified as the primary targets. Molecular docking studies indicated a strong affinity between these core targets and chemical constituents. In vivo experiments demonstrated that SSP significantly mitigated weight loss symptoms, enhanced the disease activity index (DAI), and reduced colonic tissue damage in UC rats. Furthermore, SSP was found to decrease the protein expression levels of NLRP3, ASC, and Caspase-1 in colonic tissue, as well as downregulate serum levels and mRNA expression of IL-18 and IL-1β in colonic tissue.</div></div><div><h3>Conclusions</h3><div>SSP may exert its therapeutic effects on UC by modulating the NLRP3/ASC/Caspase-1 signaling pathway, thereby attenuating intestinal inflammatory responses and facilitating the repair of the intestinal mucosal barrier.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124735"},"PeriodicalIF":2.8,"publicationDate":"2025-07-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144634266","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":"Separation and enrichment of fingolimod and citalopram active drug ingredients by fabric phase sorptive extraction followed by high performance liquid chromatographic analysis with diode array detection","authors":"Esra Durgun ,&nbsp;Halil İbrahim Ulusoy ,&nbsp;İbrahim Narin ,&nbsp;Abuzar Kabir ,&nbsp;Marcello Locatelli","doi":"10.1016/j.jchromb.2025.124730","DOIUrl":"10.1016/j.jchromb.2025.124730","url":null,"abstract":"<div><div>Multiple Sclerosis (MS) is a chronic disorder affecting the central nervous system. The treatment of MS often involves a combination of pharmaceutical agents, including Fingolimod (FIN) and Citalopram (CIT). The analysis of these drug compounds plays a crucial role in various stages of health sciences, ranging from drug development to therapeutic monitoring. In this study, a rapid and sensitive analytical method was developed for the trace determination of FIN and CIT using fabric phase sorptive extraction (FPSE) as a sample pretreatment technique, followed by high-performance liquid chromatography coupled with diode array detection (HPLC-DAD). Key FPSE parameters—including pH, adsorption and desorption conditions, and extraction time—were systematically optimized. Analytical performance characteristics of the proposed method were evaluated under optimized conditions in accordance with international guidelines. Chromatographic separation of FIN and CIT was achieved via isocratic elution using a mobile phase composed of acetonitrile, pH 3.0 phosphate buffer, and methanol (50:40:10, <em>v</em>/v/v) at a flow rate of 1.0 mL min⁻¹. The limits of detection (LOD) for FIN and CIT were determined to be 7.46 ng mL⁻¹ and 5.97 ng mL⁻¹, respectively. The method demonstrated good precision, with relative standard deviation (RSD) values below 6.0 % for spiked samples. Recovery rates from synthetic urine and saliva matrices ranged between 93.1 % and 105.0 % for both analytes, confirming the method's accuracy and applicability to biological samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124730"},"PeriodicalIF":2.8,"publicationDate":"2025-07-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144631251","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":"Trimethylaminoethyl ester derivatization and stable isotope derivatization for enhanced analysis of fatty acids in biological samples by electrospray ionization tandem mass spectrometry","authors":"Liu Yang ,&nbsp;Qingchun Wang ,&nbsp;Weiwei Chen ,&nbsp;Ji Yang ,&nbsp;Yu Lin ,&nbsp;David M. Lubman","doi":"10.1016/j.jchromb.2025.124733","DOIUrl":"10.1016/j.jchromb.2025.124733","url":null,"abstract":"<div><h3>Background</h3><div>Abnormal fluctuations in free fatty acids (FFAs) are associated with cardiovascular diseases. However, conducting a thorough analysis of individual FFAs via mass spectrometry has historically posed challenges due to their low ionization efficiency and the absence of distinctive fragment ions.</div></div><div><h3>Results</h3><div>In this study, we introduce a method utilizing paired stable isotope derivatization coupled with liquid chromatography–triple quadrupole mass spectrometry (ID-LC-QQQ-MS) for thorough identification and relative quantification of fatty acids in serum samples. This method involves the derivatization of the carboxyl groups of FFAs using a pair of isotope reagents, resulting in the formation of FA trimethylaminoethyl ester (FA-TMAE-<em>h</em>₃/<em>d</em>₃), which can yield two distinct neutral fragments with masses of 59 and 62 Da during collision-induced dissociation (CID). Consequently, a quadruple neutral loss scan (QNLS) approach was utilized for the non-targeted profiling of FFAs in serum samples. The derivative peak pairs displaying matching retention times and distinct mass differences were extracted from the two QNLS spectra and recognized as potential FFAs. Subsequently, a multiple reaction monitoring (MRM) detection protocol was established for the relative quantification of fatty acids in the serum of Syrian Golden Hamsters subjected to various treatments, utilizing a pooled sample labeled with a heavy isotope as an internal standard. Partial least squares discriminant analysis (PLS-DA) revealed notable variations in these 23 fatty acids across the four groups.</div></div><div><h3>Significance</h3><div>The current stable isotope derivatization (ID) method, in conjunction with tandem mass spectrometry (MS/MS) analysis, stands out as a promising approach for identifying and quantifying FFAs in real samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124733"},"PeriodicalIF":2.8,"publicationDate":"2025-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144634267","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":"Targeted metabolomics for cardiovascular disease: Validation of a high-throughput HPLC-MS/MS assay","authors":"Sabina N. Baskhanova ,&nbsp;Natalia E. Moskaleva ,&nbsp;Ksenia M. Shestakova ,&nbsp;Maria V. Kozhevnikova ,&nbsp;Ekaterina O. Korobkova ,&nbsp;Victor M. Samoylov ,&nbsp;Svetlana A. Appolonova","doi":"10.1016/j.jchromb.2025.124732","DOIUrl":"10.1016/j.jchromb.2025.124732","url":null,"abstract":"<div><div>Cardiovascular diseases (CVD) remain a leading cause of mortality worldwide, necessitating innovative diagnostic tools to improve early detection and management. This study represents the optimization and validation of a high-throughput HPLC-MS/MS method for simultaneous quantification of 98 metabolites in human plasma, including amino acids and its derivatives (<em>n</em> = 29), tryptophan pathway metabolites (<em>n</em> = 17), nucleosides (<em>n</em> = 4), water-soluble vitamins (<em>n</em> = 3), acylcarnitines (<em>n</em> = 39), and others (<em>n</em> = 6). The method utilizes chemical derivatization to enhance retention and sensitivity of polar metabolites providing accurate analysis across diverse physicochemical properties. The presented method was validated in accordance with EMA guidelines and included assessment of linearity, accuracy, precision, matrix effects, recovery, and stability. Parallelism testing confirmed the suitability of a surrogate matrix for calibration. The method was applied for the analysis of plasma samples from 399 patients with cardiovascular diseases and 75 healthy controls, revealing significant metabolic alterations in pathways associated with inflammation, nitric oxide metabolism, and mitochondrial function. The presented comprehensive approach may serve as a rapid screening method for the identification of selective CVD biomarkers using targeted metabolomic profiling.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124732"},"PeriodicalIF":2.8,"publicationDate":"2025-07-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144631252","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":"Cross-species comparison of resolvin E and resolvin D biosynthesis: Quantification by liquid chromatography mass spectrometry in fish and human cells exposed to alpha-linolenic acid, eicosapentaenoic acid, and docosahexaenoic acid","authors":"Pedro Araujo ,&nbsp;Marit Espe ,&nbsp;Elisabeth Holen ,&nbsp;Maren Hoff Austgulen ,&nbsp;Sarah Iqbal ,&nbsp;Bjørg Kristine Hundal","doi":"10.1016/j.jchromb.2025.124729","DOIUrl":"10.1016/j.jchromb.2025.124729","url":null,"abstract":"<div><div>Resolvins are lipid mediators essential for resolving inflammatory processes in living organisms. Studies have shown that fish and human cells share enzymatic pathways to produce resolvins E (RvE) and D (RvD) from eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), respectively. However, cross-species comparisons of resolvin production from dietary α-linolenic acid (ALA), an indirect precursor to resolvins as it is the metabolic precursor to EPA and DHA, remain limited. To address this, a liquid chromatography mass spectrometry method was validated for quantifying RvE and RvD released into culture media by salmon head kidney cells and human peripheral blood mononuclear cells exposed to ALA, EPA, and DHA. The assay performance was evaluated using both fish and human cell culture media, demonstrating acceptable results according to international guidelines. Key performance parameters included selectivity, range (0.5–50 ng/mL), linearity (<em>R</em>^<em>2</em> = 0.98–0.99), limits of detection (∼0.02–0.09 ng/mL), limits of quantification (∼0.08–0.3 ng/mL), and accuracy (∼97–109 %). The validated method enabled a reliable cross-species comparison and revealed that the DHA → RvD conversion is the predominant pathway in both fish and human cells. In contrast, the EPA → RvE and ALA-indirect pathways (ALA→EPA/DHA → RvE/RvD) contributed minimally in both species. Notably, the study also indicated, the involvement of a retroconversion pathway: DHA → EPA → RvE not being reported yet.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124729"},"PeriodicalIF":2.8,"publicationDate":"2025-07-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144613972","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":"Development and computational analysis of new alkaloid derivatives as potential inhibitors of the SARS-CoV-2 Mpro","authors":"Gulim Mukusheva ,&nbsp;Manshuk Nurmaganbetova ,&nbsp;Zharkin Zhumagaliyeva ,&nbsp;Madina Aliyeva ,&nbsp;Nurizat Toigambekova","doi":"10.1016/j.jchromb.2025.124718","DOIUrl":"10.1016/j.jchromb.2025.124718","url":null,"abstract":"<div><div>This study focused on developing and evaluating new alkaloid derivatives as potential inhibitors of the SARS-CoV-2 main protease (M^pro). Five novel alkaloid derivatives were synthesized using standard organic techniques and characterized via infrared and NMR spectroscopy. Pharmacokinetic properties were assessed using Lipinski's Rule of Five and computational tools. Density Functional Theory calculations and molecular docking with AutoDock Vina were employed to analyse molecular properties and interactions with SARS-CoV-2 M^pro. Anti-aggregation and anticoagulant activities were evaluated using aggregometry and coagulation assays. The synthesized compounds exhibited favourable pharmacokinetic properties, including molecular weights below 500 and suitable polar surface areas for bioavailability. Molecular docking revealed strong binding affinities for M^pro, with binding energies ranging from −7.6 to −8.8 kcal/mol. Compounds 1 and 2 showed significant inhibition of platelet aggregation and anticoagulant activity, prolonging prothrombin and activated partial thromboplastin times at 50 μM concentration. Biological activity analysis indicated moderate to high activity as GPCR ligands and protease inhibitors. The synthesized alkaloid derivatives demonstrated high potential as SARS-CoV-2 M^pro inhibitors with additional anti-aggregation and anticoagulant properties. These findings suggest promise for further development as therapeutic agents against COVID-19, although further research is necessary to understand their mechanisms, safety, and clinical application prospects.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124718"},"PeriodicalIF":2.8,"publicationDate":"2025-07-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144596846","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":"PeakClimber: A software tool for the accurate quantification of complex HPLC chromatograms","authors":"Joshua T. Derrick ,&nbsp;Pragney Deme ,&nbsp;Norman J. Haughey ,&nbsp;Steven A. Farber ,&nbsp;William B. Ludington","doi":"10.1016/j.jchromb.2025.124721","DOIUrl":"10.1016/j.jchromb.2025.124721","url":null,"abstract":"<div><div>High-performance liquid chromatography (HPLC) is a common medium-throughput technique to quantify the components of complex mixtures like those typically obtained from biological tissue extracts. However, analysis of HPLC data from multianalyte samples is hampered by a lack of tools to accurately determine the precise analyte quantities on a level of precision equivalent to mass spectrometry approaches. To address this problem, we developed a tool we call PeakClimber that uses a sum of bidirectional exponentially modified Gaussian (BEMG) functions to accurately deconvolve overlapping, multianalyte peaks in HPLC traces. Here we show that HPLC peaks are well-fit by a BEMG function, that PeakClimber more accurately quantifies known peak areas than standard industry software and other open-source software packages for HPLC, and that PeakClimber accurately quantifies differences in triglyceride abundances between colonized and germ-free fruit flies.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124721"},"PeriodicalIF":2.8,"publicationDate":"2025-07-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144605750","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":"pH-gradient cation exchange purification of IgG2 disulfide isoforms","authors":"Mark Chipley,&nbsp;Kristine Wells,&nbsp;James L. DuMontelle,&nbsp;Jacquelynn Smith,&nbsp;Thomas W. Powers,&nbsp;Thomas F. Lerch","doi":"10.1016/j.jchromb.2025.124716","DOIUrl":"10.1016/j.jchromb.2025.124716","url":null,"abstract":"<div><div>Immunoglobulin (IgG) based therapies are used to treat a wide range of diseases. The IgG2 subclass can have variable disulfide bond connectivity in the hinge region, leading to different isoforms. Interchain disulfide bonding isoforms that constrain the Fab arm structure may impact potency. Therefore, it is important to understand the abundance of IgG2 isoforms and the impact of function for IgG2s under development. In this work, a pH-gradient cation exchange separation was developed to purify IgG2 disulfide isoforms in their native state. The IgG2 mAb used for this study was not amenable to previously reported purification methods using salt-gradient cation exchange. Collected fractions were analyzed by high-resolution denaturing reversed phase chromatography and isoform content was determined with fluorescence detection. Fractions were then combined to generate solutions with varying amounts of IgG2-B isoform, ranging from 20.3 % to 80.8 % IgG2-B isoform. Across the range of IgG2-B isoform content abundances, all samples had similar levels of product related impurities and were amenable to potency testing. The work herein demonstrates a novel approach to natively fractionate disulfide isoforms for an IgG2 mAb that was not amenable to previous reported methods.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124716"},"PeriodicalIF":2.8,"publicationDate":"2025-07-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144613971","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":"Quantitative analysis of propylene glycol in saliva of e-cigarette users by gas chromatography-mass spectrometry","authors":"Mei-Kuen Tang ,&nbsp;Steven G. Carmella ,&nbsp;Yingchun Zhao ,&nbsp;Laura Maertens ,&nbsp;Laura G. Pimentel ,&nbsp;Dorothy K. Hatsukami ,&nbsp;Stephen S. Hecht","doi":"10.1016/j.jchromb.2025.124719","DOIUrl":"10.1016/j.jchromb.2025.124719","url":null,"abstract":"<div><div>A method was developed for the quantitation of propylene glycol in human saliva as a potentially useful biomarker for e-cigarette use. Saliva was collected from e-cigarette users, cigarette smokers, and non-users of any tobacco or nicotine product with approval from the University of Minnesota Human Research Protection Program Institutional Review Board. Two separate protocols, termed programmed and non-programmed, were used. In the programmed protocol, e-cigarette users (<em>n</em> = 20) and cigarette smokers (<em>n</em> = 20) brushed their teeth, waited 15 min, then used their product every 30 s for 5 min and collected a 2 mL saliva sample immediately after the last puff. In the non-programmed protocol, cigarette smokers (<em>n</em> = 30) and e-cigarette users (<em>n</em> = 21) came to the clinic and directly provided a saliva sample for analysis. Non-users (<em>n</em> = 29) of any nicotine or tobacco product served as controls. Propylene glycol in saliva was quantified by gas chromatography–mass spectrometry as its heptafluorobutyrate ester, using propylene glycol-<em>d</em>_<em>8</em> as the internal standard. Accuracy and precision of the assay were established. Levels of salivary propylene glycol (mean ± S.D.) were 269 ± 319 and 8.04 ± 8.22 μg/mL saliva in e-cigarette users and cigarette smokers, respectively, in the programmed protocol, while the corresponding levels in the non-programmed protocol were 4.94 ± 8.68 and 1.91 ± 1.99 μg/mL. These amounts were all significantly greater than those found in non-users of any tobacco or nicotine product (0.39 ± 0.32 μg/mL). This straightforward validated assay is expected to be useful in future clinical studies of e-cigarette use.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124719"},"PeriodicalIF":2.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144563698","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":"Determination of glucose impurities in glucose-salt complex pharmaceutical products by HPLC-RID method: Analytical method development and validation study","authors":"Harun Ergen ,&nbsp;Yasin Gökekin ,&nbsp;Remziye Azra Kartop ,&nbsp;Büşra Çetin Ersen ,&nbsp;Müge Güleli ,&nbsp;Sevgi Kocaoba ,&nbsp;Cem Çalışkan","doi":"10.1016/j.jchromb.2025.124717","DOIUrl":"10.1016/j.jchromb.2025.124717","url":null,"abstract":"<div><div>Pharmaceutical products containing glucose and salt are widely used in the health sector and play a vital role. These pharmaceutical products are usually encountered as a part of drugs used in treatment and medical procedures. However, the analytical determination and quantification of active ingredients and impurities belonging to active ingredients in such products is a complicated process. This is because the retention time of impurities belonging to the glucose molecule in these pharmaceutical structures and the presence of salts that give peaks in similar places complicate the analysis process. Moreover, when the British Pharmacopoeia (BP), European Pharmacopoeia (EP) and US Pharmacopoeia (USP) are examined, it is seen that there are only monographs belonging to glucose raw material and there is no record regarding the determination of impurities belonging to glucose in pharmaceutical products containing glucose-salt complex structures. A new method has been developed within the scope of the study to prevent this complexity. As a result of the method development studies, the specific solvent method was optimized and a relatively simple pre-purification process with high recovery was applied to avoid salt interference. In addition, high-precision determination and validation studies of glucose and its impurities were carried out using the High Performance Liquid Chromatography-Refractive Index Detector (HPLC-RID) method. This new analytical approach is expected to contribute to the development of reliable and high-quality products in the healthcare field by raising industry standards.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124717"},"PeriodicalIF":2.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144572137","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}