Journal of Chromatography B最新文献

{"title":"Analysis of eicosanoids by quadrupole gas chromatography-negative ion chemical ionization-tandem mass spectrometry as pentafluorobenzyl trimethylsilyl derivatives: Naming the Murphy rearrangement","authors":"Dimitrios Tsikas","doi":"10.1016/j.jchromb.2025.124794","DOIUrl":"10.1016/j.jchromb.2025.124794","url":null,"abstract":"<div><div>Eicosatetraenoic acid (arachidonic acid) is the precursor of the eicosanoids, which include the prostaglandins (PGs), the leukotrienes (LTs), and the endocannabinoids (ECs). Methods based on GC–MS/MS are the <em>Gold Standard</em> for the quantitative analysis of eicosanoids in biological samples. After extraction and derivatization, biological eicosanoids are analyzed on quadrupole GC–MS/MS apparatus as pentafluorobenzyl (PFB) ester trimethylsilyl (TMS) ether derivatives, i.e., PFB-TMS. Negative-ion chemical ionization (NICI) generates in the ion-source abundant anions due to [M–PFB]<sup>−</sup>. Collision-induced dissociation (CID) of [M–PFB]<sup>−</sup> in the collision cell generates product ions, which are suitable candidates for specific quantitative analyses in the selected-reaction monitoring (SRM) mode. In this article, we review CID gas-phase reactions of PFB-TMS derivatives of PGs and LTs. The specific CID negative charge-driven intramolecular rearrangement of TMS groups from ether moieties (OTMS) to carboxylate anions [M–PFB]<sup>−</sup> of PFB-TMS derivatives to form a –COO-TMS ester has been reported for the first time by Robert C. Murphy on PFB-TMS derivatives of 5-hydroxy-eicosanoic acid (HEA) from hydrogenated and desulfurized LTE<sub>4</sub>, and saturated LTB<sub>4</sub>. We propose to name this specific CID gas-phase reaction the <em>Murphy Rearrangement</em> in honour of R.C. Murphy. The <em>Murphy Rearrangement</em> generates the product ions <em>m/z</em> 253 and <em>m/z</em> 89 from the precursor ion <em>m/z</em> 399 of the PFB-TMS derivative of HEA and neutral loss of 146 Da. We propose to name <em>Murphy-type Rearrangements</em> that were observed for the eicosanoids 8-<em>iso</em>PGF<sub>2α</sub>, its 2,3-dinor- and 2,3-dinor-5,6-dihydro-metabolites, the major urinary metabolites (MUM) of F and E prostaglandins, i.e., PGF-MUM and PGE-MUM, respectively, as well as for the CID of <em>m/z</em> 179 [M–PFB]<sup>−</sup> of the PFB ester of the drug acetylsalicylic acid (aspirin). The <em>Murphy Rearrangement</em> and <em>Murphy-type Rearrangements</em> differ with respect to the rearrangement ion and the subsequent neutral losses and fragmentations. The <em>Murphy-type Rearrangements</em> of PGF-MUM and PGE-MUM includes a specific neutral loss of 198 Da PFBOH due to intramolecular attack of 1- or ω-COO<sup>−</sup> anions to ω- or 1-COO-PFB esters. <em>Murphy Rearrangements</em> and <em>Murphy-type Rearrangements</em> are best identified by performing CID studies on PFB-TMS derivatives of [1,1-<sup>18</sup>O<sub>2</sub>]- and [1,ω-<sup>18</sup>O<sub>2</sub>]-eicosanoids in the NICI mode. Neutral loss of TMS<sup>18</sup>OH (92 Da) and PFB<sup>18</sup>OH (200 Da) (in dicarboxy-eicosanoids), and formation of a product ion with <em>m/z</em> 91 [TMS<sup>18</sup>O]<sup>−</sup> will indicate <em>Murphy Rearrangements</em> and <em>Murphy-type Rearrangements.</em> Formation of a product ion with <em>m/z</em> 59 (acetate) from ","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1267 ","pages":"Article 124794"},"PeriodicalIF":2.8,"publicationDate":"2025-09-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145106567","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":"Eco-friendly microextraction technique using SFO-DLLME coupled with HPTLC for plasma analysis of metformin and imeglimin","authors":"Venkata Suresh Ponnuru ,&nbsp;D. Renuka ,&nbsp;M. Siva Prasad ,&nbsp;R. Hari Prasad Reddy ,&nbsp;M. Bhargava Reddy ,&nbsp;K.N. Rajani Kanth ,&nbsp;G. Naga Raju ,&nbsp;N. Rama Rao ,&nbsp;M. Hemanth Kumar","doi":"10.1016/j.jchromb.2025.124791","DOIUrl":"10.1016/j.jchromb.2025.124791","url":null,"abstract":"<div><div>This study aimed to develop and validate a green, sensitive, and high-throughput analytical method for the simultaneous determination of metformin and imeglimin in plasma samples using gliclazide as an internal standard. A novel microextraction technique was proposed, combining salt-induced dispersive liquid–liquid microextraction based on solidified floating organic droplet (SI-DLLME-SFOD) with high-performance thin-layer chromatography HPTLC-densitometric detection. This approach significantly improves greenness, sensitivity, and simplicity compared to conventional extraction and chromatographic techniques. The method was optimized for maximum resolution using silica gel 60 F254 pre-coated TLC plates as the stationary phase and a mobile phase comprising methanol: chloroform: 0.5 % <em>w</em>/<em>v</em> ammonium acetate (8:1:1, <em>v</em>/v/v). Detection was performed at 254 nm. The method was validated following US FDA bioanalytical guidelines. The R_f values were observed at 0.45 ± 0.04 for imeglimin, 0.63 ± 0.04 for metformin, and 0.84 ± 0.04 for gliclazide. The method exhibited excellent linearity in the range of 100–1000 ng/band, with correlation coefficients (r²) exceeding 0.998. The average recoveries were 90.91 % for imeglimin and 92.61 % for metformin, with RSD values of 0.42 and 0.39, respectively, confirming high precision and accuracy. The SI-DLLME-SFOD protocol enables efficient extraction, lower solvent consumption, and improved analyte enrichment. The developed method was evaluated using green analytical chemistry metrics and its eco-friendliness was confirmed. It demonstrated reduced solvent usage, minimal waste generation, and a lower environmental burden, establishing its superiority over previously reported sample preparation techniques. Furthermore, the validated method was successfully applied to real samples (human plasma) to assess the concentration, thereby demonstrating the potential value of the method for routine use. This method provides a green, efficient, and validated strategy for the bioanalysis of antidiabetic drugs in human plasma, supporting its potential application in routine clinical diagnostics and therapeutic drug monitoring.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1267 ","pages":"Article 124791"},"PeriodicalIF":2.8,"publicationDate":"2025-09-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145060844","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":"GC–MS metabolomics coupled with multi-biomarker analysis reveal toxic effects of functionalized nanoplastics in Paphia undulata","authors":"Pingping Li ,&nbsp;Zixin Kang ,&nbsp;Jianhui Lin ,&nbsp;Min Liu ,&nbsp;Xi Deng ,&nbsp;Yuangao Qu ,&nbsp;Yingxu Zeng","doi":"10.1016/j.jchromb.2025.124790","DOIUrl":"10.1016/j.jchromb.2025.124790","url":null,"abstract":"<div><div>Despite the widespread occurrence of nanoplastics (NPs) in marine ecosystems, a knowledge gap persists regarding their bioaccumulation and toxic effects in marine bivalves, particularly for NPs with surface modifications. This study employed combined metabolomics and multi-biomarker analyses to investigate the bioaccumulation, elimination, and toxicity of pristine polystyrene (PS), carboxylated PS (PS-COOH), and aminated PS (PS-NH₂) NPs in marine clam <em>Paphia undulata</em>. Results revealed distinct tissue-specific accumulation patterns, showing highest NP uptake in intestines (109.34 μg/g), followed by digestive glands (30.36 μg/g), with minimal uptake in gills (7.47 μg/g). Following a 4-day exposure, NPs triggered tissue-specific antioxidant responses, inducing significant oxidative damage (elevated malondialdehyde) in digestive glands. PS-NH₂ activated the superoxide dismutase (SOD) and glutathione (GSH) systems, while PS and PS-COOH elicited synergistic upregulation of SOD and catalase (CAT) activities, indicating surface chemistry-dependent detoxification pathways. GC–MS-based metabolomics revealed that NPs markedly disrupted metabolic homeostasis in digestive glands. Significant alterations occurred in carbohydrates, amino acids, lipids, and organic acids, with PS-COOH exposure yielding the most differential metabolites (PS-COOH: 27, PS: 21, PS-NH₂: 20). Pathway enrichment analysis showed all NPs interfered galactose metabolism and starch/sucrose metabolism, disrupting energy homeostasis. Additionally, PS dysregulated phenylalanine, tyrosine and tryptophan biosynthesis, whereas PS-COOH perturbed cysteine and methionine metabolism, demonstrating surface chemistry-specific dysregulation of distinct amino acid pathways. This work provides mechanistic insights into how NP surface chemistry modulates toxicity in marine bivalves. The integration of biomarker responses with metabolome perturbations offers a systematic framework for evaluating NP ecotoxicity, informing ecological risk assessments for marine benthic ecosystems.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1267 ","pages":"Article 124790"},"PeriodicalIF":2.8,"publicationDate":"2025-09-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145103235","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 general urine screening method for performance enhancing drugs in racehorses utilizing liquid chromatography-high resolution mass spectrometry (LC-HRMS)","authors":"Saurabh Dubey ,&nbsp;Izabela Lomnicka ,&nbsp;Pamela Waller ,&nbsp;Dharmikkumar Vora ,&nbsp;Levent Dirikolu","doi":"10.1016/j.jchromb.2025.124786","DOIUrl":"10.1016/j.jchromb.2025.124786","url":null,"abstract":"<div><div>The complexity of the drug market and the constant updating of drugs have been challenging issues for drug regulatory authorities. In this manuscript, a high-throughput automated assay based on Liquid Chromatography High Resolution Mass Spectrometry (LC-HRMS) suitable for use as an initial testing procedure covering multiple classes of compounds prohibited in horse racing is described. The assay requires a 250-μL urine aliquot, which is subjected to enzymatic hydrolysis followed by Biotage Isolute supported liquid extraction plates using Biotage Extrahera system, evaporation, and reconstitution in a 96-well collection plate. LC–HRMS analyses were carried out on a Thermo Fisher Q-Exactive Mass spectrometer (equipped with HESI source interface) coupled with Vanquish UHPLC system linked to ACE Excel column. Drug targets were identified by retention time and accurate mass, with a mass tolerance window of +/− 5 ppm. The screening method was validated for over 250 drug targets and/or their metabolites in a 7-min run. Validation data including sensitivity, specificity, extraction recovery and precision are presented. As the method employs full-scan mass spectrometry, an unlimited number of drug targets can theoretically be incorporated.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1267 ","pages":"Article 124786"},"PeriodicalIF":2.8,"publicationDate":"2025-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145077172","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":"DNA-protective and antioxidant potentials of thym samples: Chemometric and bioactive profiling from Iraq's Kurdish highlands and Siirt, Türkiye","authors":"İbrahim Teğin ,&nbsp;Karwan Mohammed Amin Mahmood Khoshnaw ,&nbsp;Mehmet Fidan ,&nbsp;Gurbet Canpolat ,&nbsp;Behcet İnal ,&nbsp;Erdal Yabalak","doi":"10.1016/j.jchromb.2025.124789","DOIUrl":"10.1016/j.jchromb.2025.124789","url":null,"abstract":"<div><div>Thyme, a fragrant herb from the Lamiaceae family, is highly valued for its essential oil content, making it a key ingredient in perfumery, aromatherapy, phytotherapy, and pharmacology. This study investigates the chemical composition and biological activity of thyme samples collected from Iraq's Kurdish Region (Qandil, Asos, Balambo, Karokh) and Siirt, Türkiye (Eruh, Şirvan, Kezer, Tillo, and other regions). Comprehensive analyses were conducted to assess micro- and macro-element levels, total phenolic and flavonoid content, and antioxidant properties using methanolic extracts. The highest phenolic and flavonoid contents were 226.83 ± 0.21 mg/mL gallic acid equivalent (GAE) and 2.59 ± 0.02 mg/mL of routine equivalents (RE). Antioxidant activity, evaluated via FRAP and DPPH assays, demonstrated IC₅₀ values of 1.32 mg/mL and 2.05 mg/mL. Maximum metal chelation was 22.92 %. LC-MS/MS identified 29 out of 37 phenolic compounds, including abundant levels of hesperidin (62.37 ± 0.02 μg/kg), rosmarinic acid (19.90 ± 0.01 μg/kg), and Ferulic acid (2.23 ± 0.01 μg/kg). Chemometric analyses, including PCA and cluster analysis, highlighted regional differences. Hydroxyl radicals (•OH) produced through the Fenton reaction involving H₂O₂ and Fe(II) cause damage to the pBR322 plasmid DNA. This damage is evidenced by a reduction in the supercoiled form and an increase in relaxed or linear DNA forms following oxidative stress. DNA damage assays demonstrated that thyme extracts provided partial protection against Fenton reaction-induced damage without compromising DNA integrity. These findings emphasize thyme's potential for pharmaceutical, nutritional, and industrial applications.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1267 ","pages":"Article 124789"},"PeriodicalIF":2.8,"publicationDate":"2025-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145057111","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":"Discrimination of isomeric dihydroflavone and chalcone by the boosting optimal collision energy-liquid chromatography-tandem mass spectrometry: A case study of pharmacokinetics in honey-fried licorice","authors":"Yueting Li ,&nbsp;Yan Cao ,&nbsp;Tengteng Wang ,&nbsp;Shengnan Cai ,&nbsp;Yun Qiao ,&nbsp;Chao Cheng ,&nbsp;Jiale Gao ,&nbsp;Jie Liu ,&nbsp;Hongbin Xiao","doi":"10.1016/j.jchromb.2025.124785","DOIUrl":"10.1016/j.jchromb.2025.124785","url":null,"abstract":"<div><div>The occurrence of isomeric dihydroflavone and chalcone, two important subfamilies of flavonoid class, extensively happens in herbal medicines. However, identical MS/MS spectra make the identity confirmation a tough job, the complexity will be further boosted in biological samples. Inspired by that isomers possess distinct inherent physicochemical parameters, optimal collision energy (OCE), which is positively correlated with the bond dissociation energies (BDEs), was evaluated towards differentiating isomeric dihydroflavone and chalcone. It was achieved by plotting their relative response-collision energy curves (RRCECs) and comparing the unique OCEs obtained. As a result, difference were observed for either OCE of bond dissociations involving Retro Diels-Alder (RDA) reaction as well as glycosidic cleavage when comparing two pairs of isomers, which were liquiritin <em>vs.</em> isoliquiritin and liquiritigenin <em>vs.</em> isoliquiritigenin, because the energies required for bond dissociation to produce identical fragment ions varies among isomers. Furthermore, OCEs consistently ranked dihydroflavone higher than chalcone, aligning with their BDEs determined through quantum calculation. These results suggested great potential for OCEs in distinguishing between dihydroflavone and chalcone. By applying the discriminating criterion, successful identity recognition was achieved for the two pairs of isomers among the many signals sharing identical MRM transitions in honey-fried licorice treated plasma. Thereafter, the confidence-enhanced OCE-LC-MS/MS method was applied to characterize and determine these 4 isomers along with 3 components of honey-fried licorice in rat plasma, the definite determination as well as the pharmacokinetic courses were subsequently accomplished and discussed. Overall, this study boosted the application of OCE-LC-MS/MS in isomers discrimination of isomeric dihydroflavone and chalcone.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1267 ","pages":"Article 124785"},"PeriodicalIF":2.8,"publicationDate":"2025-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144989788","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":"Comprehensive LC-MS/MS and HPLC-based profiling of secondary metabolites in Aster incisus from diverse cultivation regions","authors":"Shi-Heon Kang ,&nbsp;Neil Patrick Uy ,&nbsp;Yunji Lee ,&nbsp;Hoon Kim ,&nbsp;Sanghyun Lee","doi":"10.1016/j.jchromb.2025.124787","DOIUrl":"10.1016/j.jchromb.2025.124787","url":null,"abstract":"<div><div><em>Aster incisus</em> is a perennial herbaceous plant belonging to the Asteraceae family, known for its pharmacologically active secondary metabolites. In this study, we conducted a comparative profiling and quantification of secondary metabolites in <em>A. incisus</em> extracts cultivated in two regions, Eumseong (AIE) and Inje (AII), using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and high-performance liquid chromatography with a variable wavelength detector (HPLC/VW). LC-MS/MS analysis conducted in negative ion mode enabled the identification of 13 secondary metabolites, including key flavonoids and phenolic acids such as chlorogenic acid, narcissoside, isorhamnetin, and rutin. HPLC quantification revealed distinct compositional differences between the AIE and AII samples. The AII extract contained significantly higher levels of chlorogenic acid (35.97 mg/g extract), narcissoside (8.08 mg/g extract), and isorhamnetin 3-galactoside (23.79 mg/g extract), while the AIE extract exhibited greater concentrations of protocatechuic acid (0.77 mg/g extract), rutin (2.08 mg/g extract), and hirsutrin (2.05 mg/g extract). Isorhamnetin was detected exclusively in AII (0.24 mg/g extract), and a number of other compounds were present only in trace amounts in both samples. These results suggest that environmental and geographical factors play a significant role in the biosynthesis of phenolic and flavonoid compounds in <em>A. incisus</em>. These findings provide critical chemotaxonomic and pharmacological insights into the region-dependent accumulation of bioactive metabolites, highlighting their potential relevance in drug discovery and therapeutic formulation based on natural products.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1267 ","pages":"Article 124787"},"PeriodicalIF":2.8,"publicationDate":"2025-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145005251","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":"Integrated network pharmacology, metabolomics and experimental validation to reveal the pharmacological substances and mechanism of Wendan decoction on chronic obstructive pulmonary disease","authors":"Fang Wang ,&nbsp;Guoan Zhao ,&nbsp;Qi Yu ,&nbsp;Ruinan Ren ,&nbsp;Wenbao Wang ,&nbsp;Tianyang Wang ,&nbsp;Song Lin ,&nbsp;Yan Lin","doi":"10.1016/j.jchromb.2025.124788","DOIUrl":"10.1016/j.jchromb.2025.124788","url":null,"abstract":"<div><div>Wendan Decoction (WDD), a classic formula for the expectoration of phlegm, has been acknowledged for the management of chronic obstructive pulmonary disease (COPD). Nevertheless, the therapeutic components and mechanism of WDD in COPD remain elusive. Hence, an analytical strategy for extensive investigation of the constituents in WDD combining UFLC-ESI-Q/TOF-MS and subsequent network pharmacology was conducted, and the appropriate preparation of bio-samples was involved with mechanistic bioanalysis including multi-technique metabolomics and molecular biological means, that pivotal factors such as PTGS2, arachidonic acid (AA) metabolism, and PI3K-AKT signaling pathway were recommended as potential central elements for the anti-COPD effects. Subsequently, based on the rat model of COPD, a dose-dependent manner for the significant attenuation effect of WDD on pulmonary injury, inflammation, and oxidative stress was observed. Metabolomics analysis revealed the restoration of 65 COPD biomarkers by WDD intervention. A comprehensive analysis highlighted AA metabolism as the predominant metabolic pathway. The significance of vital targets within the AA metabolism pathway, including PTGS2 and PLA2, and their robust binding affinities with key constituents of WDD such as naringenin and baicalin were characterized and verified from the aspects of docking fitting and thermal stability. Notably, the upregulation levels of protein and mRNA of key targets within the AA metabolism pathway caused by COPD was significantly reversed by WDD. Hence, the efficacy of WDD against COPD was uncovered from the aspects of components and mechanism in this research, implying the effective treatment of COPD and the clinical application of WDD.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1267 ","pages":"Article 124788"},"PeriodicalIF":2.8,"publicationDate":"2025-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145005250","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":"Chromatographic determination of antidepressants in plasma and saliva: Towards non-invasive therapeutic monitoring","authors":"Sofia Soares ,&nbsp;Luana Rosendo ,&nbsp;Suzana Fonseca ,&nbsp;Nuno Gonçalves ,&nbsp;João M. Franco ,&nbsp;Tiago Rosado ,&nbsp;Mário Barroso ,&nbsp;Vítor Hugo Santos ,&nbsp;Cristina Rei ,&nbsp;Patricia Amantegui ,&nbsp;António Pissarra da Costa ,&nbsp;Telma Chaves ,&nbsp;Rita Valente ,&nbsp;Fábio Duarte ,&nbsp;Susana Pacheco ,&nbsp;Marco Martins ,&nbsp;Kátia Dias ,&nbsp;Patricia Costa ,&nbsp;Rui Costa ,&nbsp;Sílvia Castro ,&nbsp;Eugenia Gallardo","doi":"10.1016/j.jchromb.2025.124782","DOIUrl":"10.1016/j.jchromb.2025.124782","url":null,"abstract":"<div><div>Drug monitoring of antidepressants in plasma and oral fluid represents a valuable tool in clinical practice, enabling the optimisation of treatment efficacy and the reduction of adverse effects. Given the significant interindividual variability in antidepressant response—driven by factors such as metabolism, drug-drug interactions, and adherence to therapy—drug monitoring facilitates dose adjustment based on measured drug concentrations, ensuring levels remain within the therapeutic window.</div><div>This study aimed at developing and validating a robust, rapid, and sensitive method for the simultaneous quantification of 21 selected antidepressants and their metabolites in only 100 μL of plasma and oral fluid. Sample preparation was performed using a simple protein precipitation protocol, followed by analysis via liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method was validated in accordance with internationally accepted bioanalytical guidelines, demonstrating linearity over the concentration range of 0.98–1000 ng/mL. Limits of quantification were established at 0.98 ng/mL for all analytes across both matrices.</div><div>The extraction procedure yielded high recovery rates, and the method showed excellent selectivity, sensitivity, precision, and accuracy, confirming its suitability for routine toxicological applications. The validated method was successfully applied to 142 paired authentic plasma and oral fluid specimens from patients undergoing antidepressant therapy. Antidepressant concentrations were determined in both matrices, and treatment adherence was considered high, being confirmed in 88.7 % of patients. Correlation analysis between plasma and oral fluid concentrations produced promising results for several of the compounds under investigation, reinforcing the potential utility of oral fluid as a non-invasive alternative matrix in drug monitoring.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1267 ","pages":"Article 124782"},"PeriodicalIF":2.8,"publicationDate":"2025-09-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144933190","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":"Quyu Huazhuo Decoction alleviates non-Alcoholic steatohepatitis via remodeling the gut microbiota and regulating bile acid and short-chain fatty acid metabolism","authors":"Lu Lu ,&nbsp;Chengting Wu ,&nbsp;Juhong Jia ,&nbsp;Yuanqin Du ,&nbsp;Yujiao Peng ,&nbsp;Hongna Huang ,&nbsp;Jingjing Huang ,&nbsp;Yaobin Nong","doi":"10.1016/j.jchromb.2025.124784","DOIUrl":"10.1016/j.jchromb.2025.124784","url":null,"abstract":"<div><div>Non-alcoholic steatohepatitis (NASH), a globally prevalent metabolic disorder, exhibits a complex and incompletely understood pathogenesis with limited clinical treatment options available. Studies have shown that Quyu Huazhuo Decoction (QYHZD) can effectively reduce insulin resistance and improve liver function in NASH patients, though its underlying mechanisms remain unclear. Using a high-fat diet (HFD)-induced NASH rat model, the present study employed 16S rDNA sequencing along with targeted metabolomics of bile acids (BAs) and short-chain fatty acids (SCFAs) to systematically evaluate the therapeutic effects of QYHZD. The results showed that QYHZD significantly alleviated HFD-induced obesity, hepatic steatosis, inflammatory response, and glucose and lipid metabolism dysregulation. The intervention also reshaped the gut microbiota, promoting the growth of beneficial bacteria such as <em>Akkermansia</em> and <em>Roseburia</em>, while suppressing harmful taxa including <em>Klebsiella</em> and Desulfovibrio. Metabolomics analysis indicated that QYHZD intervention upregulated protective BAs (e.g., UDCA, CDCA, and their conjugated forms) and SCFAs (e.g., butyric acid and valeric acid), along with reduced production of toxic BAs such as DCA. In conclusion, this study revealed that QYHZD improves the progression of NASH through multi-axis regulation of “microbiota-BA/SCFA-metabolism”, providing experimental evidence and mechanistic insights for the use of traditional Chinese medicine in treating metabolic liver diseases.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1267 ","pages":"Article 124784"},"PeriodicalIF":2.8,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144933187","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}