Journal of Chromatography B最新文献

{"title":"Development and validation of an LC-MS/MS method for quantifying total and unbound doravirine in human plasma","authors":"Rizqah Bernard,&nbsp;Sydwell P. Maputla,&nbsp;Phiwe Zuma,&nbsp;Anton Joubert,&nbsp;Sandra Castel,&nbsp;Marthinus van der Merwe,&nbsp;Edda Zangenberg,&nbsp;Lubbe Wiesner","doi":"10.1016/j.jchromb.2024.124439","DOIUrl":"10.1016/j.jchromb.2024.124439","url":null,"abstract":"<div><div>A robust LC-MS/MS method was developed to quantify total and unbound doravirine in plasma samples from patients receiving daily doses of 100 mg doravirine, in combination with lamivudine and tenofovir disoproxil fumarate, in a phase 3 clinical trial. The trial is ongoing, and sample analysis is planned to commence once all samples have been collected. The method was validated to quantify both total and unbound doravirine using a single calibration curve. Protein precipitation was used to obtain the total doravirine from plasma and ultrafiltration was used to obtain the unbound doravirine. A Kinetex 1.7 µm EVO C18 100 Å column was used for chromatography using a gradient mobile phase (0.1 % formic acid in water and 0.1 % formic acid acetonitrile) at a flow rate of 250 µL/min during a five minute runtime. The analyte was ionized by positive electrospray ionization and detection was by multiple reaction monitoring on a Sciex API3200 triple quadrupole mass spectrometer. Using calibration standards prepared in whole plasma, the calibration curve fitted a quadratic regression (weighted by 1/x) over a calibration range of 7.00–2000 ng/mL and was applied successfully for the measurement of both total and unbound doravirine. Validation experiments, conducted according to international guidelines, proved the accuracy and precision of the method over three consecutive days. The method demonstrated robustness in the presence of matrix components, different anticoagulants, hemolyzed blood (2 %), and concomitant medications, showing the necessary sensitivity and selectivity for the quantification of both total and unbound doravirine concentrations expected in the study samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124439"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142926115","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":"Evaluation of the effect of Ela tablets in the treatment of diabetic nephropathy based on rat experiments and screening strategy for quality markers of Ela tablets targeting aldose reductase","authors":"Shunan Guo ,&nbsp;Aizaiti Keremu ,&nbsp;Miao Hu ,&nbsp;Fei He ,&nbsp;Maitinuer Maiwulanjiang ,&nbsp;Haji Akber Aisa ,&nbsp;Xuelei Xin","doi":"10.1016/j.jchromb.2025.124450","DOIUrl":"10.1016/j.jchromb.2025.124450","url":null,"abstract":"<div><div>Ela tablets (ALP) is a traditional Uyghur medicinal formulation comprising 9 herbs. Clinical applications have demonstrated its potential in treating diabetic nephropathy (DN). However, its specific medicinal effects and pharmacodynamic components have not been elucidated. This research aims to investigate the efficacy of ALP in treating DN and to explore the quality markers (Q-markers) for its exertion of efficacy. Using the UHPLC-Q-Orbitrap HRMS technique, a total of 60 compounds were identified within ALP. Animal experiments were conducted to investigate the effect of ALP intervention at doses of 80, 160, and 320 mg/kg in Sprague-Dawley rats. Then, fingerprints of ten batches of ALP extracts were established using UPLC-DAD. Spectrum-effect relationship analysis of these fingerprints and aldose reductase (AR) activity was conducted by chemometric analysis methods. The results were further validated by molecular docking and cellular experiments. The animal experiments indicated that ALP had a therapeutic effect on DN. Specifically, ALP reduced biochemical indexes such as serum creatinine (SCr), 24-hour urinary total protein (24 h UTP), uric acid (UA), blood urea nitrogen (BUN), triglycerides (TG), and total cholesterol (TC). ALP stabilized body weight and fasting blood glucose, enhanced the antioxidant capacity of kidneys, and improved renal pathology. Comprehensive analysis indicated that crocin-I and gallic acid may be used as Q-markers for ALP. In summary, ALP has been identified as a treatment for DN, and gallic acid and crocin-I can be used as its Q-markers.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124450"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142963255","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":"Extraction and quantitation of fentanyl in exhaled breath condensate using a magnetic dispersive solid phase based on graphene oxide and covalent organic framework composite and LC-MS/MS analysis","authors":"Sedigeh Mohamadzadeh ,&nbsp;Ali Akbar Fathi ,&nbsp;Abolghasem Jouyban ,&nbsp;Afshin Gharekhani ,&nbsp;Mohamadbagher Hosseini ,&nbsp;Maryam Khoubnasabjafari ,&nbsp;Vahid Jouyban-Gharamaleki ,&nbsp;Mir Ali Farajzadeh ,&nbsp;Mohammad Reza Afshar Mogaddam","doi":"10.1016/j.jchromb.2024.124447","DOIUrl":"10.1016/j.jchromb.2024.124447","url":null,"abstract":"<div><div>Free fentanyl is responsible for its pharmacological effects, but its total concentration is typically determined for therapeutic drug monitoring purposes. Determination of fentanyl concentration can help reduce the prescribed doses, leading to fewer side effects and increased effectiveness. Therefore, predicting free drug concentration in pharmaceutical research is crucial. The aim of this study was to determine free fentanyl in exhaled breath condensate. These samples were extracted using a dispersive micro solid phase extraction method with a new adsorbent made of graphene oxide, magnetic iron oxide nanoparticles, and covalent organic framework. 10 mg of the adsorbent was added to the sample solution adjusted to pH 10. After sonication for 5 min, the sorbent was separated using an external magnet. The adsorbed analyte was then eluted from the sorbent surface using a mixture of acetonitrile, methanol, and deionized water in a ratio of 42.5:42.5:15 (v/v/v) and analyzed using liquid chromatography-tandem mass spectrometry system. The calibration curve showed high linearity in the range of 0.17–10000 μg L⁻¹ with a coefficient of determination of 0.9998 and good repeatability with a relative standard deviation of 4.1 %. Additionally, this method provided a low detection limit of 0.05 μg L⁻¹ and quantification limit of 0.17 μg L⁻¹.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124447"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997757","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A novel LC-MS/MS assay for low concentrations of creatinine in sweat and saliva to validate biosensors for continuous monitoring of renal function","authors":"Sophie Adelaars ,&nbsp;Chyara S.M. Lapré ,&nbsp;Patricia Raaijmakers ,&nbsp;Constantijn J.A.M. Konings ,&nbsp;Massimo Mischi ,&nbsp;R. Arthur Bouwman ,&nbsp;Daan van de Kerkhof","doi":"10.1016/j.jchromb.2024.124444","DOIUrl":"10.1016/j.jchromb.2024.124444","url":null,"abstract":"<div><div>Monitoring of kidney function traditionally relies on plasma creatinine concentrations, necessitating invasive blood draws. Non-invasively obtainable biofluids, such as sweat and saliva, present a patient-friendly alternative with potential for continuous monitoring. This study focusses on developing and validating a novel Liquid Chromatography- tandem Mass Spectrometry (LC-MS/MS) assay as a reference test for measuring low creatinine concentrations in sweat and saliva. We explore the correlation between these biofluids and plasma creatinine concentrations during haemodialysis to support future biosensor applications. Creatinine concentrations were measured in sweat, saliva, and plasma obtained from forty patients undergoing haemodialysis. A novel LC-MS/MS assay was developed to quantify low creatinine concentrations in sweat and saliva. Correlation analyses were performed to compare the creatinine concentrations across biofluids. The novel LC-MS assay demonstrated high accuracy (93.9–97.8%) and low imprecision (3.4–8%) in measuring very low creatinine concentrations with a limit of quantitation of 1.26 µmol/L. Significant correlations ware found between creatinine concentrations in sweat and saliva with those in plasma (ρ: 0.68 and 0.80, respectively). During haemodialysis, creatinine concentrations decreased concurrently in all three biofluids. The strong correlations observed imply that these non-invasive biofluids could serve as reliable alternatives to traditional blood tests for kidney function assessment. This study enhances our understanding of creatinine excretion pathways of creatinine and provides a foundation for developing innovative, patient-friendly approaches for continuous kidney function monitoring, such as wearable biosensors.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124444"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143078301","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 and High Throughput HPTLC Method for Simultaneous Estimation of Celecoxib and Tramadol Hydrochloride in their Newly Approved Analgesic Combination and Spiked Plasma with Dichromic Green and Blue Assessments","authors":"Mona M. Abdel Moneim,&nbsp;Mohamed M.A. Hamdy","doi":"10.1016/j.jchromb.2024.124434","DOIUrl":"10.1016/j.jchromb.2024.124434","url":null,"abstract":"<div><div>The FDA “Food and Drug Administration” recently approved a novel co-crystal formulation of Celecoxib (CEX) and Tramadol (TRM) for the treatment of adults suffering from moderate to severe pain in several conditions. This novel combination has advantages over co-administration of the two drugs individually as better patient compliance, synergism and lower therapeutic cost. This work presents the first “High performance Thin Layer Chromatographic” (HPTLC) quantitative analytical technique for CEX and TRM simultaneous assay in bulk, their new dosage form and plasma.<!--> <!-->The proposed HPTLC assay is based on separation of CEX and TRM on silica gel 60 F254 sheets followed by densitometric scanning at 270 nm. The plates’ development was carried out using a mobile phase of ethyl acetate–methanol–ammonia (5:5:0.05, v/v). The two drugs showed linearity of 0.025–1 μg.band⁻¹ <!-->&amp; for plasma analysis linearity range was 0.2–10 μg.mL⁻¹ <!-->plasma. The proposed chromatographic technique was validated and showed satisfying validation characteristics of linearity, selectivity, precision and accuracy. In addition, the assay was evaluated by AGREE, AGREEprep, ComplexMoGAPI and BAGI for greenness and blueness to ensure the method’s environmental sustainability and its safety for routine quality control assay of this novel combination.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124434"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142891001","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":"“On-off” elution mechanism facilitates the rapid LC/MS/MS-based analysis of peptide antibiotics in human plasma","authors":"Huan Tong ,&nbsp;Yong Qiao ,&nbsp;Yang Deng,&nbsp;Fang Yuan,&nbsp;Debiao Xiang,&nbsp;Siwei Guo,&nbsp;Bing Xu,&nbsp;Xin Li","doi":"10.1016/j.jchromb.2024.124438","DOIUrl":"10.1016/j.jchromb.2024.124438","url":null,"abstract":"<div><div>Individualized medication with peptide antibiotics, guided by therapeutic drug monitoring, is essential to treat infections caused by multidrug-resistant bacteria. Peptide antibiotics exhibit an “on-off” elution mechanism on a C18 column, leading to adsorption at the column inlet in all-aqueous conditions. Unlike small molecules, column length minimally influences their retention, with longer columns simply broadening peptide antibiotic peaks due to unnecessary post-column volume. Our theory suggests short columns can achieve comparable separation quality and enable faster analysis. Consequently, we developed a rapid LC-MS/MS method using an ultra-short (4 × 2.0 mm) column to quantify five peptide antibiotics in human plasma simultaneously. Calibration curves demonstrated strong linear regression (R2 &gt; 0.996). The inter- and intra-accuracy at the three QC levels ranged from 86.7 % to 109.1 %, and at the LLOQ, it was between 87.6 % and 116.0 %. The precision for QCs and LLOQ was consistently below 11.7 % and 18.5 %, respectively. This method, characterized by simplicity and universality, was undoubtedly useful in clinically tailoring peptide antibiotic medication for individual patients.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124438"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142926110","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 UHPLC-MS/MS method for the quantitative analysis of trans-ISRIB in human plasma","authors":"Weizhuan He,&nbsp;Akshay Suresh Patil,&nbsp;Yan Xu","doi":"10.1016/j.jchromb.2025.124469","DOIUrl":"10.1016/j.jchromb.2025.124469","url":null,"abstract":"<div><div>The integrated stress response (ISR) is a cellular defense mechanism activated under stress conditions. When the ISR is activated, it slows the production of proteins, the building blocks that cells need to function. <em>Trans</em>-integrated stress response inhibitor (<em>trans</em>-ISRIB) is a compound that can reverse the effects of ISR activation, showing promise for treating neurodegenerative diseases. The preclinical and clinical evaluation of <em>trans</em>-ISRIB necessitates a reliable analytical method. This study presents the development and validation of an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for the quantitative analysis of <em>trans</em>-ISRIB in human plasma, conforming to the U.S. FDA’s guidelines for bioanalytical method validation. The method developed utilizes a liquid–liquid extraction procedure to prepare plasma samples with a spiked internal standard (IS). The extracts containing <em>trans</em>-ISRIB and the IS were dried under nitrogen, reconstituted in the mobile phase, and separated on a Waters XSelect HSS T3 column under isocratic conditions with a mobile phase containing 0.1 % acetic acid in 70 % methanol aqueous solution at a flow rate of 0.500 mL/min. Detection and quantification were accomplished using a positive electrospray ionization tandem mass spectrometer (ESI⁺-MS/MS) operated in multiple-reaction-monitoring (MRM) mode. The method demonstrated a linear calibration range for <em>trans</em>-ISRIB concentrations from 0.500 to 1.00 x 10³ nM, with high specificity, precision, accuracy, and recovery. This method addresses a significant analytical gap, offering a robust tool for quantifying <em>trans</em>-ISRIB in human plasma.</div><div><strong>Chemical compounds studied in this article:</strong> 2-(4-chlorophenoxy)-<em>N</em>-[4-[[2-(4-chlorophenoxy)acetyl]amino]cyclohexyl]acetamide (<em>trans</em>-ISRIB) (CAS # 1597403–47-8); 2-(4-chlorophenoxy)-N-(2-{[(4-chlorophenoxy)acetyl]amino}ethyl)acetamide (CAS # 327071–30-7).</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124469"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997689","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":"An integrated approach using molecular docking, network pharmacology, and UPLC-Q-TOF-MS analysis to investigate the chemical makeup and mechanism of Xiaoqinglong decoction against asthma","authors":"Shuang Wei ,&nbsp;Xueting Li ,&nbsp;Xinyu Li,&nbsp;Rui Wang,&nbsp;Yuming Wang,&nbsp;Yubo Li","doi":"10.1016/j.jchromb.2025.124490","DOIUrl":"10.1016/j.jchromb.2025.124490","url":null,"abstract":"<div><div>Objective: This study aims to investigate the potential mechanisms by which Xiaoqinglong decoction (XQLD) exerts its therapeutic effects on asthma. This will be achieved through the application of the UPLC-Q-TOF-MS coupling technique, integrated with network pharmacology and molecular docking methodologies. Methods: The UPLC-Q-TOF-MS technique was employed to perform a qualitative analysis of both the aqueous extract of XQLD and the drug-containing serum. The Swiss TargetPrediction, OMIM, and GeneCards databases were utilized to identify blood-derived components and disease-associated targets. Subsequently, a protein-protein interaction (PPI) network was constructed by intersecting these datasets to identify key targets, which were then subjected to Gene Ontology (GO) functional analysis and Kyoto Encyclopedia of Genes and Genomes (KEGG) pathway enrichment analysis. Cytoscape software facilitated the construction of a ‘drug-component-disease-target’ network to enable visualization and analysis, thereby aiding in the prediction of targets and signaling pathways of XQLD in the treatment of asthma. Finally, molecular docking of the pertinent incoming components to the central target was conducted utilizing AutoDock Vina and PyMol software. Results: A comprehensive analysis identified 102 components within the aqueous extract of XQLD, alongside 93 components in the drug-containing serum. Additionally, 90 compound-disease shared targets and 45 key targets were identified through PPI network analysis. Notably, compounds such as apigenin, l-asarinin, 6-shogaol, ellagic acid, kaempferol, and naringenin are pivotal in mediating the therapeutic effects of XQLD in asthma treatment. The primary molecular targets of XQLD for asthma include SRC, AKT1, EGFR, ESR1, HIF1A, and PIK3CA. The results of the molecular docking analysis indicated that the binding energies between the core target and the active ingredient were ≤ −5.5 kcal/mol, demonstrating a strong affinity. Conclusion: This study elucidated the chemical composition, potential targets, and action pathways of the aqueous extract of XQLD and its drug-containing serum. It preliminarily identified the material basis and mechanism of action, thereby providing a foundation for further in-depth research into the mechanisms underlying XQLD and its clinical applications.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1254 ","pages":"Article 124490"},"PeriodicalIF":2.8,"publicationDate":"2025-01-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143372032","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 of full and empty adeno-associated virus particles using a novel multi-modal anion exchange membrane","authors":"Xiaolei Hao ,&nbsp;Ronny Horax ,&nbsp;S. Ranil Wickramasinghe ,&nbsp;Xianghong Qian","doi":"10.1016/j.jchromb.2025.124499","DOIUrl":"10.1016/j.jchromb.2025.124499","url":null,"abstract":"<div><div>A novel multi-modal anion exchange (MMAEX) membrane with both electrostatic and hydrophobic interaction moieties was developed for the separation of full and empty AAV2 capsids with only slight differences in surface charge and hydrophobicity. Both gradient and two-step elution have been able to separate the full and empty capsids effectively. During gradient elution with slight increase in conductivity coupled with weakening electrostatic and enhanced hydrophobic interactions between the ligand and the capsids, two distinctive elution peaks representing empty and full capsids were resolved. Full capsid recovery of 94 % at 89 % purity has been achieved with a loading density of ∼10¹² virus particles per milliliter of membrane volume. During the two-step elution process, the functionalized membrane can achieve 88 % full capsid recovery at 75 % purity, or 67 % recovery at 89 % purity, or 59 % recovery at 93 % purity at first-step conductivity of 7.0, 7.5 and 8.0 mS/cm respectively and a loading density of ∼10¹³ particles per milliliter of membrane volume. Our results indicate that our MMAEX membrane coupled with careful modulation of capsid-ligand interaction has superior performance for separating the full and empty AAV capsids.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1255 ","pages":"Article 124499"},"PeriodicalIF":2.8,"publicationDate":"2025-01-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143403499","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A new indirect method for the quantification of total organic iodine (TOI) in environmental waters by inductively coupled plasma with mass spectrometry and liquid chromatography with tandem mass spectrometry","authors":"Jinbo Chen ,&nbsp;Shinya Echigo ,&nbsp;Yuto Tada ,&nbsp;Klon D.C. Hinneh ,&nbsp;Sadahiko Itoh","doi":"10.1016/j.jchromb.2025.124489","DOIUrl":"10.1016/j.jchromb.2025.124489","url":null,"abstract":"<div><div>The formation of emerging iodinated disinfection by-products (I-DBPs) is associated with iodine sources including organic compounds. Total organic iodine (TOI) was used as a bulk index of organic iodinated compounds because of the difficulty in identifying and quantifying individual organic iodinated compounds in environmental waters. Conventional methods for the direct quantification of TOI require complicated pretreatments, which has promoted many studies to attempt to simplify the quantification of TOI by an indirect measurement. In current indirect methods, TOI is mainly calculated as the differences between the concentration of total iodine (TI) and inorganic iodine (<span><math><msup><mi>I</mi><mo>−</mo></msup></math></span> and <span><math><msup><msub><mtext>IO</mtext><mn>3</mn></msub><mo>-</mo></msup></math></span>) by liquid chromatography-inductively coupled plasma with mass spectrometry (LC-ICP-MS). However, without accurate identification and discrimination by LC-ICP-MS, possible co-eluting iodinated compounds may be detected as <span><math><msup><mi>I</mi><mo>−</mo></msup></math></span> and <span><math><msup><msub><mtext>IO</mtext><mn>3</mn></msub><mo>-</mo></msup></math></span>. To measure TOI more accurately, a simple method was developed by ICP-MS and liquid chromatography-tandem mass spectrometry (LC-MSMS). TI was measured by ICP-MS, and the spiked recoveries of tested iodinated compounds showed acceptable accuracy and repeatability in Milli-Q water and environmental waters, respectively. <span><math><msup><mi>I</mi><mo>−</mo></msup></math></span> and <span><math><msup><msub><mtext>IO</mtext><mn>3</mn></msub><mo>-</mo></msup></math></span> were first simultaneously measured by LC-MSMS without redox pretreatments. The limits of quantification of <span><math><msup><mi>I</mi><mo>−</mo></msup></math></span> and <span><math><msup><msub><mtext>IO</mtext><mn>3</mn></msub><mo>-</mo></msup></math></span> in this method were 0.05 <span><math><mi>μ</mi></math></span>g I/L and 0.4 <span><math><mi>μ</mi></math></span>g/L (0.3 <span><math><mi>μ</mi></math></span>g I/L), respectively. The method is highly sensitive, and the actual concentration of <span><math><msup><mi>I</mi><mo>−</mo></msup></math></span> and <span><math><msup><msub><mtext>IO</mtext><mn>3</mn></msub><mo>-</mo></msup></math></span> can be calculated by the spiked recovery. The method was successfully applied by measuring TOI concentration (2.2 to 17 <span><math><mi>μ</mi></math></span>g I/L) in various types of environmental waters.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1254 ","pages":"Article 124489"},"PeriodicalIF":2.8,"publicationDate":"2025-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143272982","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}