Journal of Chromatography B最新文献

{"title":"Pharmacokinetics and tissue distribution of key sesquiterpene glycosides in Dendrobium nobile analyzed by UHPLC-Q-Trap-MS/MS","authors":"Xingdong Wu ,&nbsp;Chunxue Gao ,&nbsp;Ya Huang ,&nbsp;Lin Qin ,&nbsp;Zhou Yang ,&nbsp;Di Wu ,&nbsp;Ya Wang ,&nbsp;Qianru Zhang ,&nbsp;Daopeng Tan ,&nbsp;Yongxia Zhao ,&nbsp;Jiajia Wu ,&nbsp;Shanyong Yi ,&nbsp;Yanliu Lu ,&nbsp;Yuqi He","doi":"10.1016/j.jchromb.2024.124386","DOIUrl":"10.1016/j.jchromb.2024.124386","url":null,"abstract":"<div><div><em>Dendrobium nobile</em> (<em>D. nobile</em>), a traditional herb known for its immunomodulatory and neuroprotective properties, contains characteristic alkaloids and sesquiterpene glycosides. While alkaloids have been extensively studied, research on sesquiterpene glycosides remains limited. This study established and validated a UHPLC-Q-Trap-MS/MS method for detecting six sesquiterpene glycosides in <em>D. nobile</em>, applying it to pharmacokinetic and tissue distribution studies in rats following oral administration of the <em>D. nobile</em> aqueous extract. Plasma and tissue samples were prepared using methanol for protein precipitation and separated on a Waters Acquity UPLC BEH C18 column. Quantification was performed using multiple reaction monitoring (MRM) in negative electrospray ionization (ESI) mode. Method validation demonstrated specificity, selectivity, precision, accuracy, stability, matrix effects, and recovery rates meeting the criteria for <em>in vivo</em> drug analysis. Pharmacokinetic results indicated that dendronobiloside A, dendronobiloside C, and dendronobiloside D were rapidly absorbed with low plasma concentrations and quick elimination. In contrast, dendronobiloside E, dendroside G, and dendromoniliside D were rapidly absorbed with higher plasma concentrations but also eliminated quickly. Tissue distribution studies revealed that dendronobiloside A, C, and D were detectable in the heart, liver, spleen, lungs, kidneys, stomach, large intestine, small intestine, thymus, and pancreas, but almost undetectable in the brain. And dendronobiloside E, dendroside G, and dendromoniliside D were detectable in all tissues. Overall, the six sesquiterpene glycosides reached various tissues within 2 h of administration, with distribution levels ranked as follows: small intestine &gt; stomach &gt; large intestine &gt; pancreas &gt; lungs &gt; kidneys &gt; liver &gt; heart &gt; thymus &gt; spleen &gt; brain. These findings provide insights into the immunomodulatory mechanisms of <em>D. nobile</em> sesquiterpene glycosides and inform clinical dosing considerations.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1250 ","pages":"Article 124386"},"PeriodicalIF":2.8,"publicationDate":"2024-11-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142737931","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":"Structural characterization of degradation products of phenol red used as zero permeability marker in in-situ rat intestinal permeability studies by LCMS-IT-TOF","authors":"Saniye Özcan ,&nbsp;Mustafa Sinan Kaynak","doi":"10.1016/j.jchromb.2024.124380","DOIUrl":"10.1016/j.jchromb.2024.124380","url":null,"abstract":"<div><div>In this study, the quantitative determination of phenol red with using HPLC, the permeability marker widely used in gastrointestinal studies, and its stability in various apolar phase solvents were investigated. In addition, the mechanisms of degradation products obtained were tried to be elucidated by using the LCMS-IT-TOF device. The proposed HPLC method utilizes a Perkin Elmer C₁₈, 5 μm, 250 mm × 4.6 mm i.d. column, a mobile phase consisting of phosphate buffer and methanol in the proportion of 50:50 (<em>v/v</em>) with apparent pH adjusted to 3.2 and detected at 430 nm using a photodiode array detector. The method exhibits linearity within the concentration range of 5–200 µg/mL, with a calculated R² of 0.9981. In situ conditions, the recovery is in the range of 89.8–103.6 %. Furthermore, high-resolution mass studies were identified three degradation products that occur when phenol red was dissolved either ethanol or methanol medium. The method has a low cost of consumables and is very easy to apply to the procedure and analyze degradation products while easily applied to phenol red analysis in various mediums. High-resolution mass screening analysis confirmed the proposed structure of the degradation product. The validation and robustness studies were fulfilled to display the performance of the method in various analytical environments. The greenness and blueness evaluations of the developed method were also made in detail. The AGREE score of the method was calculated as 0.64, AGREEprep 0.68, MoGAPI 0.78, and BAGI scale score as 65.0. In short, the method is perfectly green, applicable, and practical. Finally, phenol red concentrations analyzed in samples obtained in <em>in-situ</em> animal studies were conducted to demonstrate the applicability of the developed method.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1250 ","pages":"Article 124380"},"PeriodicalIF":2.8,"publicationDate":"2024-11-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142692295","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":"Investigating the stability of a cerebral vasodilator drug using chromatographic methods: Evaluation of methods’ practicality and environmental aspects","authors":"Amal M. Al-Mohaimeed ,&nbsp;Maha F. El-Tohamy ,&nbsp;Mohamed G.H. Ali ,&nbsp;Neven M. Habib ,&nbsp;Nada S. Abdelwahab ,&nbsp;Maha M. Abdelrahman ,&nbsp;Hamada M. Mahmoud ,&nbsp;Aml A. Emam","doi":"10.1016/j.jchromb.2024.124371","DOIUrl":"10.1016/j.jchromb.2024.124371","url":null,"abstract":"<div><div>A vinca alkaloid; vinburnine (VNB) is utilized as an effective vasodilator. As a cyclic amide-containing drug, it is likely susceptible to hydrolytic degradation. This study examined the degradation profile of VNB, findings indicated that VNB undergoes degradation solely in the presence of alkali, generating a carboxylic acid derivative (DEG). The present study aimed to design and apply green TLC-densitometric and RP-HPLC assays for concurrently measuring VNB and its degradation product for the first time. TLC-densitometric assay was carried out on silica gel 60 F₂₅₄ TLC plates and a developing system of ethyl acetate: methanol: triethylamine (6:4:0.05, by volume) and detection at 230 nm. RP-HPLC method depended on a C8 column and a mixture of methanol: water (95:5, v/v). The rate of flow was 1 mL/min and UV detection at 230 nm. The proposed assays were used for prediction of the degradation behavior of VNB under the mentioned conditions and then applied for quantitation of VNB in its commercially available capsules. Four distinct metric approaches; National Environmental Method Index (NEMI), Analytical Eco-Scale, Green Analytical Procedure Index (GAPI), and Blue Applicability Grade Index (BAGI) were utilized to assess the chromatographic method’s ecological effect. Findings obtained from the provided methodologies were contrasted statistically with the stated HPLC method using Student’s t and F-tests. The analysis revealed that there were no significant differences between them. The established methods were verified in accordance with the recommendations of the International Council for Harmonization (ICH), and all the outcomes were deemed to fall within the permissible limit.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1249 ","pages":"Article 124371"},"PeriodicalIF":2.8,"publicationDate":"2024-11-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142680342","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 validation of a robust RP-HPLC method to quantitate residual 2–mercaptoethylamine in drug product formulations containing amino acid additives","authors":"Delaney Doran,&nbsp;Geoffrey Struble,&nbsp;Katarina Moravcevic,&nbsp;Pinger Wang,&nbsp;Shelly Ji","doi":"10.1016/j.jchromb.2024.124379","DOIUrl":"10.1016/j.jchromb.2024.124379","url":null,"abstract":"<div><div>Bispecific antibodies have a wide range of applications in cancer immunotherapy, some of which are manufactured by controlled Fab-arm exchange requiring the reductant 2-mercaptoethylamine (2-MEA). As a process impurity, monitoring the residual 2-MEA in bispecific antibody drug product process development is needed. A novel reversed phase-high performance liquid chromatography (RP-HPLC) method for measurement of residual 2-MEA that uses 7–fluorobenzofurazan-4-sulfonic acid ammonium salt (SBD-F) as a fluorescent-detection tag in drug product formulations containing high concentrations of arginine has been developed. Using a thiol tag for residual 2–MEA eliminates any potential interference from conventional tag binding to amine groups of the formulation arginine, and potentially resulting in overestimation of the amount of impurity in a given sample. The new method has been fully validated for specificity, linearity, accuracy, range, limit of quantitation, limit of detection, and robustness. This method therefore has potential to aid in detecting residual 2-MEA content for any process that utilizes 2-MEA for bispecific antibody manufacturing.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1249 ","pages":"Article 124379"},"PeriodicalIF":2.8,"publicationDate":"2024-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142674862","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simple and rapid analytical method for the determination of methylmercury in fish and shellfish using solid-phase extraction and gas chromatography–mass spectrometry","authors":"Sachiko Kakimoto,&nbsp;Masato Yoshimitsu,&nbsp;Naoya Kakutani","doi":"10.1016/j.jchromb.2024.124383","DOIUrl":"10.1016/j.jchromb.2024.124383","url":null,"abstract":"<div><div>Herein, we devise a method to detect methylmercury (MeHg) in fish and shellfish food samples using solid-phase extraction. We draw from the principles of the “QuEChERS” method, eliminating the need for hazardous organic solvents and employing general-purpose gas chromatography–mass spectrometry (GC–MS) equipment. The use of acetonitrile during extraction prevents emulsion formation, which could otherwise disrupt MeHg recovery. Additionally, the introduction of sulfuric acid solution during extraction dissolves sample lipids. The purification process involves solid-phase extraction instead of liquid–liquid extraction, ensuring rapid and straightforward analysis. The MeHg recovery, analyzed using reference samples and MeHg-loaded blank samples, is 86.1 %–98.3 %, and the limit of quantification is 0.02 mg/kg. The calibration curves for phenyl-derivatized MeHg exhibit exceptional linearity at 1–50 ng/mL. The intra- and inter-assay coefficients of variation validate the repeatability and intermediate precision of our method. This analytical approach is simple, and it offers high precision and accuracy, making it valuable for quantifying MeHg in fish and shellfish food samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1250 ","pages":"Article 124383"},"PeriodicalIF":2.8,"publicationDate":"2024-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142692294","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":"Unraveling the molecular mechanism of aqueous extract of Sargentodoxa cuneata against ulcerative colitis from serum metabolomics and bioinformatics perspectives","authors":"Dengli Wu ,&nbsp;Hongmei Wu ,&nbsp;Piao Yu ,&nbsp;Hongyun Liu ,&nbsp;Mei Liu ,&nbsp;Junyi Wang ,&nbsp;Xiangpei Wang ,&nbsp;Feng Xu","doi":"10.1016/j.jchromb.2024.124372","DOIUrl":"10.1016/j.jchromb.2024.124372","url":null,"abstract":"<div><div>Symptoms of ulcerative colitis (UC) are like “intestinal carbuncle” in Chinese medicine. The aqueous extract of <em>Sargentodoxa cuneata</em> (AESc) has good therapeutic effects on UC, but the underlying mechanism needs to be further elucidated. The mechanism of AESc against UC was studied based on metabolomics and bioinformatics in mice with UC. Dextran sodium sulfate was applied to induce a mouse model of UC. After the intervention of AESc, the general condition of the animals was recorded, and efficacy-related indicators were measured. Information on serum metabolites was determined. Multivariate analysis combined with bioinformatics methods were used to identify the differential metabolites. Furthermore, “metabolite-target-disease” network was obtained, and differential metabolites of UC were screened, and further analysis of the metabolites were performed. Molecular docking validation was also carried out. AESc improved general conditions such as blood in stool, hair of animals, and weight loss, reduced disease activity index scores and shortening of colon length in mice with UC. A total of 3445 serum metabolites were obtained, and 64 differentiated metabolites of AESc against UC were screened. Enrichment analysis showed that arachidonic acid metabolism, bile secretion, drug metabolism-other enzymes, and tyrosine metabolism were associated with AESc in the treatment of UC. In addition, based on “metabolite-target-disease” network, the serum metabolites cholylleucine, 9,10,13-TriHOME, birabresib, anthramycin methyl ether, <em>trans</em>-hexadec-2-enoyl carnitine, and lucidumol A were found to have the therapeutic potential for UC. Further, 14 core targets were obtained, and lipids and atherosclerosis, rheumatoid arthritis and multiple immune-inflammatory pathways were associated with AESc for the treatment of UC. AESc corrects serum metabolic disturbances in UC mice, and multiple serum metabolites have therapeutic potential for UC. AESc may treat UC by regulating biological processes such as lipid metabolism, amino acid metabolism, thereby restoring normal physiological function of the intestine.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1249 ","pages":"Article 124372"},"PeriodicalIF":2.8,"publicationDate":"2024-11-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142674863","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 validation of ultra-performance liquid chromatography tandem mass spectrometry methods for the quantitative analysis of the antiparasitic drug DNDI-6148 in human plasma and various mouse biomatrices","authors":"Wietse M. Schouten ,&nbsp;Katrien Van Bocxlaer ,&nbsp;Hilde Rosing ,&nbsp;Alwin D.R. Huitema ,&nbsp;Jos H. Beijnen ,&nbsp;Jadel M. Kratz ,&nbsp;Charles E. Mowbray ,&nbsp;Thomas P.C. Dorlo","doi":"10.1016/j.jchromb.2024.124377","DOIUrl":"10.1016/j.jchromb.2024.124377","url":null,"abstract":"<div><div>DNDI-6148 is a promising new oral drug for the treatment of cutaneous leishmaniasis (CL), a parasitic neglected tropical disease that affects impoverished populations worldwide. Preclinical target site pharmacokinetics (PK) studies are necessary to evaluate the actual exposure to DNDI-6148 of <em>Leishmania</em> parasites in the skin. To facilitate these investigations, we have developed and validated a reversed phase ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) method to quantify DNDI-6148 in relevant target site PK samples, adhering to the relevant International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) M10 guideline on bioanalytical method validation. Full validation was performed for the surrogate biomatrices human K₂EDTA plasma, enzymatic digestion buffer and skin microdialysate. Partial validation was conducted for mouse K₂EDTA plasma and tissues. The tissue samples, including mouse skin, liver and spleen, were homogenized using a collagenase A-based enzymatic homogenization workflow. This method was found to be 2.9-fold more effective in extracting DNDI-6148 from skin than the commonly used mechanical homogenization. Protein precipitation was subsequently carried out for all biomatrices. A surrogate biomatrix was used for each method and the range was specifically developed for its intended application, resulting in a linear concentration range of 5.00–2000 ng/mL, 2.00–1000 ng/mL, and 3.00–600 ng/mL for human K₂EDTA plasma, enzymatic digestion buffer and microdialysate, respectively. Each biomatrix had intra- and inter-run accuracy and precision within 15 % for all concentration levels. Matrix effects did not affect the determination of DNDI-6148, since the stable isotopically-labelled internal standard for DNDI-6148 effectively compensated for these matrix effects. Total recovery across all methods was between 73.5 % and 81.3 % (CV ≤4.5 %). DNDI-6148 was stable under various conditions in all the tested biomatrices. However, a decrease in its concentration was observed during homogenization, for which the internal standard corrected adequately. The suitability of the method for use in future preclinical research involving DNDI-6148 was demonstrated in a preclinical target site PK study using a CL-infected murine model.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1250 ","pages":"Article 124377"},"PeriodicalIF":2.8,"publicationDate":"2024-11-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142692293","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Green RP-HPLC method for the estimation of carfilzomib in bulk, protein nanocarriers and human plasma: Application of chemometrics and Monte-Carlo simulations","authors":"Drishti Panjwani ,&nbsp;Asha Patel ,&nbsp;Deepak Mishra ,&nbsp;Shruti Patel ,&nbsp;Viral Patel ,&nbsp;Mange Ram Yadav ,&nbsp;Bhupinder Singh","doi":"10.1016/j.jchromb.2024.124350","DOIUrl":"10.1016/j.jchromb.2024.124350","url":null,"abstract":"<div><div>Carfilzomib is a tetrapeptide epoxyketone that has shown potential clinical outcomes in the treatment of multiple myeloma. However, inaccuracies in quantifying such peptide drug products have arisen due to poor stability, low solubility, time-consuming techniques, complex physicochemical properties, and use of non-green solvents with less recyclability. This provides a substantial urge to develop an ecological and sensitive analytical method for quantifying peptide drugs from matrix formulation and biological samples in early as well as lateral stages of product development in pharma industries. As a result, the study aimed to develop a robust ecological method for estimation of carfilzomib via Green RP-HPLC using analytical quality by design (AQbD) paradigms with specific application in protein nanoparticles and biological matrix. Initially, an appropriate wavelength for quantification of carfilzomib was chosen using principal component analysis (PCA) as a chemometric tool.Risk assessment followed by factor screening studies using 8-factor Placket-Burman Design aided in earmarking critical method parameters (CMPs) affecting critical analytical attributes (CAAs). Further, Central Composite Design (CCD) was employed for design space optimisation to demarcate optimum chromatographic conditions, which were corroborated for robustness using Monte-Carlo simulations. The method was validated as per ICH Q2 (R2), followed by quantifying the greenness of the method using Green Assessment tools. The method optimisation resulted in the optimal chromatographic conditions using Green RP-HPLC. The chromatographic system was equipped with a Phenomenex Aeris Peptide-XC C₁₈ column (150 × 4.6 mm × 5 µm), and the mobile phase was composed of isopropanol:methanol:0.1 M PBS (pH 5.5 adjusted using 0.1 % formic acid) (35:45:20v/v), with a 1 ml/min flow rate at a 210 nm ʎmax. The optimised chromatographic conditions resulted in a short retention time (RT) of 4.95 mins, 0.87 tailing factor (TF), 4,875,122 peak area (PA), and 8995 theoretical plate count (TPC). The method demonstrated linearity in a wide range of concentrations (0.1–20 µg/ml) with a correlational coefficient of 0.997 and &lt; 2 % RSD. The method unearthed a high precision rate with more than 95 % of drug recovery in protein nanoparticles and human plasma, thereby confirming the accuracy and sensitivity of the developed method. Chemometrics and Monte-Carlo simulations ratified the robustness and sensitivity of the developed analytical method of Carfilzomib with established greenness and a high degree of practical utility in protein-based nano formulations and human plasma matrix for life cycle product development.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1249 ","pages":"Article 124350"},"PeriodicalIF":2.8,"publicationDate":"2024-11-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142664033","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":"Methylated magnetic covalent organic framework for sample preparation and LC-MS/MS detection of 12 tadalafil analogs in dietary supplements","authors":"Meng Li ,&nbsp;Xiuli Xu ,&nbsp;Xiujuan Wang ,&nbsp;Feng Feng ,&nbsp;Jie Lian ,&nbsp;Feng Zhang","doi":"10.1016/j.jchromb.2024.124341","DOIUrl":"10.1016/j.jchromb.2024.124341","url":null,"abstract":"<div><div>Tadalafil analogs are often illegally added to dietary supplements such as herbal beverages, protein powders and tablet foods. Due to the complexity of the matrices, effective extraction of tadalafil analogs is the key to achieve accurate quantification. Therefore, it is of great significance to establish a rapid and effective method for the analytical determination of tadalafil analogs in complex matrices. In this study, a novel methylated magnetic covalent organic framework, Fe₃O₄@TFPB-OT, was successfully synthesized under mild conditions. Fe₃O₄@TFPB-OT demonstrated robust adsorption capabilities, with capacities ranging from 52.4 to 90.9 mg/g for the tadalafil analogs. Several pre-enrichment parameters were optimized, including adsorbent dosage, extraction time, pH, shaking time, elution solvent, and desorption time. The applicability of Fe₃O₄@TFPB-OT was evaluated as effective adsorbents for the magnetic solid-phase extraction (MSPE) of 12 tadalafil analogs in dietary supplements. Combined with high-performance liquid chromatography-tandem mass spectrometry, the limits of detection (LODs) of this method ranged from 0.005 to 0.05 μg/L in liquid matrices and from 0.005 to 0.05 μg/kg in solid matrices, showing good sensitivity and recoveries ranged from 56.1 % to 90.9 %with relative standard deviations lower than 3.9 %, demonstrating good accuracy and precision. Additionally, the adsorbent retained its effectiveness after at least ten reuse cycles, indicating significant reusability. This study provides an effective method for the analysis and detection of tadalafil analogs in dietary supplements and has great potential for application.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1249 ","pages":"Article 124341"},"PeriodicalIF":2.8,"publicationDate":"2024-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142646700","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":"Metabolomics combined with network pharmacology revealed a paradigm for determining the mechanism underlying the metabolic action of Gegen Qinlian Decoction amelioration of ulcerative colitis in mice","authors":"Ming Zhang ,&nbsp;Yang Jin ,&nbsp;Tiantai Wu ,&nbsp;Qing Zhao ,&nbsp;Herong Li ,&nbsp;Huan Zhang ,&nbsp;Yuan Lu ,&nbsp;Shuaishuai Chen ,&nbsp;Ting Liu ,&nbsp;Zipeng Gong ,&nbsp;Daoping Wang ,&nbsp;Wen Liu","doi":"10.1016/j.jchromb.2024.124352","DOIUrl":"10.1016/j.jchromb.2024.124352","url":null,"abstract":"<div><div>Ulcerative colitis (UC) is a common disease of the digestive system that is challenging to treat. Gegen Qinlian Decoction (GQD), which is an ancient classic formula in Chinese medicine, is effective at alleviating the symptoms of UC, but comprehensive research on its mechanism of action has not been performed. Here, we explored the material basis and potential molecular mechanism underlying GQD-mediated protection against UC by integrated metabolomics and network pharmacology. First, differentially expressed metabolites were screened and identified via a metabolomics approach, and the metabolic pathway was analyzed via MetaboAnalyst. Second, a protein–protein interaction (PPI) network was constructed to identify hub genes that encode metabolic enzymes. Third, the differentially expressed metabolites were used to construct a compound-reaction-enzyme-gene network. Finally, the metabolites were compared with relevant active components for molecular docking, molecular dynamics (MD) simulation, and verification experiment. GQD intervention alleviated UC in mice and significantly inhibited metabolic dysfunction in mice with UC; specifically, GQD reversed the abnormal changes in metabolites in the colon and serum, and regulated the arachidonic acid metabolism, tryptophan metabolism, glycerophospholipid metabolism, and purine metabolism pathways. Further literature review and molecular docking analysis with targeted MD simulation and Poisson-Boltzmann surface area (MM-PBSA) analysis were performed, revealing that GQD may inhibit the disruption of arachidonic acid metabolism and tryptophan metabolism by suppressing PTGS2 and CYP450 protein expression; these results were verified by qRT-PCR, WB, and surface plasmon resonance (SPR) assays<em>.</em> Our experiments indicated that GQD alleviated UC in mice by systematically regulating arachidonic acid metabolism and tryptophan metabolism, supporting further research and the development of GQD as a novel drug for ameliorating UC.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1250 ","pages":"Article 124352"},"PeriodicalIF":2.8,"publicationDate":"2024-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142685651","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}