Journal of Chromatography B最新文献

{"title":"Development and validation of a high-performance liquid chromatography method with fluorescence detection for the quantification of the resistance protein P-gp in cancer cells.","authors":"Elodie Gay, Maxime Dubois, Manon Roux, Antoine Goisnard, Marie Depresle, Mahchid Bamdad, Pierre Daumar, Emmanuelle Mounetou","doi":"10.1016/j.jchromb.2025.124475","DOIUrl":"https://doi.org/10.1016/j.jchromb.2025.124475","url":null,"abstract":"<p><p>A method using high-performance liquid chromatography coupled with fluorescence detection (HPLC-FLD) was developed and validated to quantify the innovative tool LightSpot®-FL-1, a selective permeability-glycoprotein (P-gp)-targeted fluorescent conjugate used to measure P-gp expression in cell samples. Quantifying P-gp is a major challenge in oncology as its overexpression in many cancer cells results in Multidrug Resistance (MDR) associated with chemotherapy failure. To develop the method reported herein, both sample preparation and analysis parameters were investigated. Optimal chromatographic conditions were achieved with 5 µL injections at a 1 mL/min flow rate on a reversed-phase Zorbax® Eclipse Plus 3.5 µm C18 column (150 × 4.6 mm) with isocratic acetonitrile/water (85/15, by volume) elution. Detection was performed with 505 nm excitation and 510 nm emission wavelengths. Validation studies were designed and performed according to the International Council for Harmonization (ICH) guidelines for bioanalytical method validation. The limit of quantification (LOQ) and limit of detection (LOD) were determined to be 0.5 and 0.2 nmol/L, respectively. The linearity range was demonstrated between 10 and 500 nmol/L, and the trueness and precision of the method were validated. Good stability was shown in three relevant analytical conditions. The greenness of the developed method was also demonstrated with the AGREE, AGREEprep and MoGAPI tools. Finally, the rapid, precise and sensitive validated analytical method was successfully applied to determine the difference in P-gp expression in three cancer cell lines: DU4475, CCRF-CEM and KG-1a.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1253 ","pages":"124475"},"PeriodicalIF":2.8,"publicationDate":"2025-01-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143035739","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":"Analysis of glipizide and pravastatin sodium drug molecules at trace level by using magnetic solid phase extraction and HPLC-DAD system.","authors":"Ümmügülsüm Polat, Halil İbrahim Ulusoy, İsmail Murat Palabıyık","doi":"10.1016/j.jchromb.2025.124477","DOIUrl":"https://doi.org/10.1016/j.jchromb.2025.124477","url":null,"abstract":"<p><p>An easy applicable and selective sample preparation technique has been developed for trace and simultaneously analysis of Glipizide (GLP) and Pravastatin (PST) molecules in biological matrices based on magnetic solid phase extraction (MSPE) and high-performance liquid chromatography (HPLC). A new magnetic adsorbent including Fe₃O₄@TEOS-Melamine has been synthetized and characterized for extraction studies. Experimental variables of MSPE were examined and optimized step by step such as pH, adsorption and desorption conditions, time effect, etc. Simultaneous HPLC analysis of GLP and PST molecules was performed by isocratic elution of a mixture of acetonitrile: phosphate buffer (pH:3.0, 0.02 M) (35:65) with flow rate 1.0 mL min^-1. Analytical signals obtained from DAD detector were recorder in 238 and 226 nm for PST and GLP, respectively. The limit of detections (LOD) for proposed method were 3.17 ng mL^-1 for PST and 3.03 ng mL^-1 for GLP molecules. Consequently, accuracy and precision of developed method were tested by means of recovery tests in synthetic urine and saliva samples. RSD % values were lower than 6.1 % and recovery values were in the range of 98.5-103.3 % for both molecules.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1253 ","pages":"124477"},"PeriodicalIF":2.8,"publicationDate":"2025-01-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143051215","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":"Enrichment and purification of trace substances from yew extracum by twin-column recycling chromatography with a step solvent gradient.","authors":"Wei Xie, Yuxue Wu, Guangxia Jin, Jiarong Sang, Feng Wei","doi":"10.1016/j.jchromb.2025.124467","DOIUrl":"https://doi.org/10.1016/j.jchromb.2025.124467","url":null,"abstract":"<p><p>The concentration and purification of trace substances from natural products represent a bottleneck in current chromatographic separations. In this study, a twin-column recycling chromatography with a step solvent gradient method was proposed and successfully applied in the purification of unknown substances with tiny content in yew extracum. The method consists of two steps. Initially, the target substances were enriched from the yew extracum stock solution, followed by further separation and purification of the enriched substances in the second step. Ultimately, the target substances A and B were obtained with a purity of 99.7 % and 96.6 %, respectively. The proposed method has the potential to be applied in the preparation of trace substances for toxicological evaluation in natural product studies.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"124467"},"PeriodicalIF":2.8,"publicationDate":"2025-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997700","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 of a novel HPLC-HRMS method for quantitative analysis of resorcinol in urine: Application to hairdressers' occupational exposure.","authors":"Amandine Cambrai-Erb, Flavien Denis, Romain Pons, Anca Radauceanu, Sophie Ndaw, Nathalie Grova","doi":"10.1016/j.jchromb.2025.124472","DOIUrl":"https://doi.org/10.1016/j.jchromb.2025.124472","url":null,"abstract":"<p><p>Resorcinol is a widespread substance used in a large variety of manufacturing industries, including cosmetics, with endocrine-disrupting activity on the thyroid function. The aim of the present study was to develop and validate a sensitive, selective and robust method to quantify resorcinol in urine and thereby assess hairdressers' occupational exposure. As resorcinol is mainly excreted in urine as glucuronide or sulfate forms, the first step consisted in hydrolyzing urine samples with a β-glucuronidase-arylsulfatase enzyme for 16 h. Then, after cleaning with a supported-liquid extraction cartridge, the samples were derivatized with dansyl chloride to improve signal and signal-to-noise ratio. Analysis was carried out using an accurate high-resolution liquid chromatography-mass spectrometry instrument on a Kinetex Biphenyl analytical column. Particular attention was paid to the chromatographic separation of resorcinol from its two isomers, catechol and hydroquinone, also present in urine. Acquisition was performed in positive ESI mode, at m/z 577.14615 for dansylated resorcinol and m/z 581.17126 for dansylated resorcinol-d₄, with respective retention times of 8.63 and 8.60 min. The method passed all the performance tests included in the validation process. The lowest limit of quantification (LLOQ) was 0.3 µg/L resorcinol, which was sufficient to quantify resorcinol in all samples tested. The calibration curves were linear from LLOQ to 2000 µg/L, with coefficients of determination R² ranging from 99.82 % to 100 %. The method was accurate, reaching 95.6 to 101.7 % of target intraday and 99.8 to 105.0 % interday, and precise with RSDs between 0.88 and 1.99 % intraday and with RSDs between 1.75 and 8.65 % in interday assessments. It also proved robust, with a matrix effect of 8.25 %. Resorcinol stability was determined by studying long-term stability at -20 °C for sample storage up to 6 months, short-term stability (at + 20 °C and + 4°C for possible short-term storage), freeze-thaw cycles, and post derivatization stability. This method was successfully applied on samples from 17 women working as hairdressers. Urinary resorcinol concentrations ranged from 2 µg/L to 1824 µg/L (6 to 4475 µg/g creatinine) and were in line with those reported in the literature.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1253 ","pages":"124472"},"PeriodicalIF":2.8,"publicationDate":"2025-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143035742","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":"Preparation of halloysite nanotube-based monolithic column for small molecules and protein analysis.","authors":"Qian Zhao, Huixuan Li, Yuanyuan Guo, Moqiong Duan, Mu Li, Tao Li, Hongya Li, Shuna Li, Shuxiang Wang, Quan Wang","doi":"10.1016/j.jchromb.2025.124476","DOIUrl":"https://doi.org/10.1016/j.jchromb.2025.124476","url":null,"abstract":"<p><p>s: This study aimed to prepare a new separation medium, silane coupling agent KH570- modified halloysite nanotube (MPS-HNT) monolithic column, with excellent separation performance for small molecular compounds and macromolecular proteins. This was prepared using the principle of redox polymerization with modified HNTs as monomers. The optimal monomer proportion was obtained by optimizing the ratio of monomer, cross-linker, and pore-forming agent, which was evaluated using scanning electron microscopy, nitrogen adsorption, and mercury intrusion. The monolithic column exhibited a relatively homogeneous pore structure and good separation performance and permeability. As a high-performance liquid chromatography stationary phase, six small aromatic molecules were successfully separated in 6 min with a theoretical plate count of 35, 640 plates m^-1 for benzene. Twenty-one peaks were separated from the fermentation mattress extract containing lipopeptide antibiotics on the MPS-HNT column. The separated chromatographic peaks further identified three lipopeptide antibiotics using matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) analysis. Twelve chromatographic peaks were isolated from chicken egg whites, and the eighth peak was identified as the lysozyme. The methodological validation of the lysozyme in chicken egg white showed that the linear correlation coefficient was 0.9996. The intraday and inter-day relative standard deviations were 3.1-4.0 % and 1.9-3.4 %, respectively. The spike recovery rate of lysozyme was 94.20-103.31 %. The overall column displayed good stability: the relative standard deviations of the peak area of six aromatic compounds and retention time were < 3.28 %.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1253 ","pages":"124476"},"PeriodicalIF":2.8,"publicationDate":"2025-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143035438","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":"Analytical quality by design guided white analytical chemistry driven green in the development of LC-ICP-MS method for arsenic speciation analysis in HEK-293 cells.","authors":"Pothuraju Naresh, Salona Devnath Roy, Prashant Vilas Pawaskar, Puja Shamrao Lokhande, Rahul Laxman Gajbhiye, Ramalingam Peraman","doi":"10.1016/j.jchromb.2025.124474","DOIUrl":"https://doi.org/10.1016/j.jchromb.2025.124474","url":null,"abstract":"<p><p>An analytical quality by design-guided LC-ICP-MS method for simultaneous arsenic speciation analysis in HEK-293 cells was optimized and validated. Initially, critical method variables (CMVs) were identified to achieve the targeted critical quality attribute (CQA) of the analytical target profile (ATP). Based on knowledge and risk assessments, formic acid (X₁), citric acid (X₂), and pH (X₃) were studied for their effect on method responses such as resolutions (Y1, Y2) and retention time of As(V), As(III) and DMA (Y3, Y4, and Y5) using central composite design (CCD). ANOVA analysis indicated that variable interaction was significant in method responses with curvature effect on resolution (Y1 and Y2). The method operable design region (MODR) afforded a 0.1% formic acid, citric acid strength of 20-30 mM, and pH 5.6-6.8 as a robust region for the appropriate method performance. Hence, the final method was optimized on the ZORBAX RRHD SB-Aq column using a mobile phase consisting of 0.1% Formic acid: Citric acid (22.5 mM) (50:50 % v/v; pH 5.6). The optimized method eluted As(V), As(III), and DMA at 2.5 ± 0.1, 2.7 ± 0.1, and 3.1 ± 0.1 min, respectively, with an acceptable resolution. The LOD of the method was 4.78, 3.39, 5.35 ppb respectively for As(V), As(III), and DMA whilst the linearity was established at 30-1000 ppb for all species with respective r²-value of 0.9967, 0.9996, and 0.9972, respectively. The % recovery (77.11-99.64 %) and precision (0.25-1.95 %) were acceptable. The method has proven robust for method variables. Notably, we conducted the Green-white analytical chemistry assessment for the developed method by three different assessment tools viz., AGREES, GAPI, and RGB of 12 algorithms. The developed method demonstrated robustness, environmental friendliness, and user-friendliness.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"124474"},"PeriodicalIF":2.8,"publicationDate":"2025-01-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143021697","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 an LC-MS/MS multiplex assay for the quantification of bedaquiline, n-desmethyl bedaquiline, linezolid, levofloxacin, and clofazimine in dried blood spots.","authors":"Gerard Aime Kenfack Teponnou, Anton Joubert, Saskia Spaltman, Marthinus van der Merwe, Edda Zangenberg, Sharon Sawe, Paolo Denti, Sandra Castel, Francesca Conradie, Richard Court, Gary Maartens, Lubbe Wiesner","doi":"10.1016/j.jchromb.2025.124470","DOIUrl":"https://doi.org/10.1016/j.jchromb.2025.124470","url":null,"abstract":"<p><p>Dried blood spot (DBS) assays to quantify novel and repurposed drugs for the treatment of rifampicin-resistant tuberculosis (RR-TB) would facilitate pharmacokinetic studies and therapeutic drug monitoring in low-middle income settings, considering their ease of application and simple sample storage requirements. We describe a DBS method for the simultaneous quantification of bedaquiline and metabolite N-desmethyl bedaquiline, linezolid, levofloxacin, and clofazimine. The analytes were extracted from the matrix and isolated by solid-phase extraction. Two LC-MS/MS systems were used, optimized for the separate analysis of the more polar compounds (linezolid and levofloxacin), and less polar compounds (bedaquiline, N-desmethyl bedaquiline, and clofazimine), employing gradient elution. Electrospray ionization and multiple reaction monitoring were used to quantify the analytes on a Sciex API3200 and an API5500 triple quadrupole mass spectrometer, for the more polar and less polar analytes, respectively. Isotopically labelled internal standards were used to compensate for variability in the quantification of each analyte. The method was validated according to international guidelines and applied to samples from a clinical trial. We performed correlation and agreement analysis of the DBS assay and in-house plasma methods using Deming regressions and Bland-Altman plots. Coefficients of correlation between measured plasma and DBS concentrations ranged from 0.866 (95% CI: 0.817-0.902) to 0.989 (95% CI: 0.985-0.992). More than 67% of the samples showed a difference between the observed and estimated plasma concentrations within 20% of their means, meeting EMA requirements for method reproducibility and demonstrating the interchangeability of our DBS and plasma LC-MS/MS methods.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"124470"},"PeriodicalIF":2.8,"publicationDate":"2025-01-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997732","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":"Comparison of urinary excretion patterns among exposures to cosmetic preservative, herbicide, and nootropic stimulant in anti-doping analysis.","authors":"I-Wen Lu, Mei-Chich Hsu, Yu-Tse Wu, William Chih-Wei Chang","doi":"10.1016/j.jchromb.2024.124430","DOIUrl":"10.1016/j.jchromb.2024.124430","url":null,"abstract":"<p><p>Doping with meclofenoxate, a nootropic stimulant prohibited in-competition by the World Anti-Doping Agency (WADA), is identified through the primary marker of urinary 4-chlorophenoxyacetic acid (4-CPA). However, the presence of 4-CPA can also arise from permissible sources. This study ventured into comparing urinary excretion patterns among exposures to permitted chemicals (chlorphenesin and 4-CPA) and the banned stimulant (meclofenoxate) and interpreting the analytical findings according to the reporting requirements. A validated method, utilising direct injection and ultra-performance liquid chromatography-tandem mass spectrometry, was employed for urine analysis. In the first experiment, participants applied chlorphenesin-containing cosmetics with varied functions, dosages, frequencies, and application sites. Sunscreen usage led to significantly higher urinary 4-CPA concentrations (up to 1049 ng/mL) as compared to others, highlighting the impact of cosmetic formulation composition for chlorphenesin delivery. The diagnostic marker for preservative exposure included 3-(4-chlorophenoxy)-2-hydroxypropanoic acid (4-CPP) and chlorphenesin and its conjugated metabolites, with 4-CPP reaching higher concentrations (C_max of 903-7629 ng/mL) and for a longer period, up to 7-14 days. In the second experiment involving meclofenoxate supplement administration, urinary C_max levels of 4-CPA were observed between 36,287 and 39,769 ng/mL at 3-10 h post-dosing, with the parent meclofenoxate undetected in all participants' samples. The third experiment, focused on occupational herbicide exposure in agricultural environments, detected minimal 4-CPA (< 10 ng/mL) in urine. WADA's current guidance for meclofenoxate aligns with reporting correct analytical results. Investigations, such as the experimental approach herein, offer valuable evidence addressing accuracy concerns in anti-doping tests, contributing insights for future amendments.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1251 ","pages":"124430"},"PeriodicalIF":2.8,"publicationDate":"2025-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142870611","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":"Dispersive solid phase extraction of apixaban from human plasma samples prior to capillary electrophoresis determination using zirconium-based metal organic frameworks prepared by different modulator and solvent.","authors":"Aysa Abbasalizadeh, Mohammad Reza Afshar Mogaddam, Mir Ali Farajzadeh, Mahboob Nemati, Saeed Mohammad Sorouraddin","doi":"10.1016/j.jchromb.2024.124417","DOIUrl":"10.1016/j.jchromb.2024.124417","url":null,"abstract":"<p><p>Here, a zirconium-based metal organic framework-dispersive solid phase extraction method was established as an efficient, robust, and accurate approach for quantifying apixabanin human plasma samples prior to capillary electrophoresis with diode array detection. Various types of metal organic frameworks based on UiO-66-NH₂ were synthesized by altering modulators and solvents and applied as sorbents in the extraction procedure. Among the tested sorbents, UiO-66-NH₂ prepared in dimethylformamide in the presence of acetic acid was found to be the best sorbent in this method for the extraction of apixaban with high extraction efficiency comparable to other types of UiO-66-NH₂ metal organic frameworks. The extraction and preconcentration of apixaban were carried out by adding 5 mg of synthesized sorbent to a 5 mL sample solution, followed by vortexing for 3 min. After discarding the supernatant, the adsorbed analyte was eluted from the sorbent surface using 60 µL acetonitrile under vortexing for 2 min. The effective parameters of the offered method were optimized and validated using a one-parameter-at-a- time strategy. The detection and quantification limits of the method were 9.9 and 32 ng mL^-1 in plasma and 1.5 and 4.9 ng mL^-1 in deionized water, respectively. The method was linear ranging from 4.9 to 1000 ng mL^-1 in deionized water and from 32 to 500 ng mL^-1 in plasma, respectively. The enrichment factor and extraction recovery values were 44 % and 53 %, respectively. The relative standard deviations were ≤6.2 % for intra- and inter-day precisions. Finally, the proposed method was successfully employed to quantify apixaban in human plasma samples.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1251 ","pages":"124417"},"PeriodicalIF":2.8,"publicationDate":"2025-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142870647","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":"Simultaneous separation and detection of common chiral and achiral metabolites in the urine of human exposed to benzene series by LC-MS/MS.","authors":"Liang Li, Gang Li, Huiying Xie, Zhi Zhang","doi":"10.1016/j.jchromb.2024.124428","DOIUrl":"10.1016/j.jchromb.2024.124428","url":null,"abstract":"<p><p>Benzene, toluene, and xylene (BTX) are priority pollutants known for their hematotoxicity and carcinogenic properties. Benzene is further metabolized to phenyl mercapturic acid (PMA), toluene and xylene also generate benzyl mercapturic acid (BMA) in human urine. To confirm whether the exposure to benzene series comes from the workplace or from the external environment such as smoking is a very meaningful work, so accurate measurement of their biomarkers in biological samples is crucial. This study developed a novel chiral stationary phase using 6-ethylenediamine mono-derivatized-β-cyclodextrin for the simultaneous separation and detection of four chiral and achiral biomarkers PMA, BMA, N-acetyl-S-(3,4-dihydroxybutyl)-L-cysteine (DHBMA), and N-acetyl-S-(1-hydroxymethyl-2-propenyl)-L-cysteine (MHBMA) in human urine. The method demonstrated high sensitivity with detection limits below 0.211 μg/L for PMA, 0.467 μg/L for BMA, 0.246 μg/L for DHBMA, and 0.109 μg/L for MHBMA, excellent recoveries ranging from 78 to 116 % as well as the high resolutions of PMA, BMA and MHBMA-2 enantiomers being up to 1.62, 2.23 and 1.79, respectively, within 50 min under reversed-phase chromatography. Application to 60 urine samples from an automobile manufacturing plant revealed that benzene as a paint solvent has been strictly limited, while toluene and xylene are widely used, potentially posing health risks to occupational groups. The simultaneous detection of PMA, BMA, MHBMA, and DHBMA provides a more accurate assessment of non-smoking populations, enhancing the evaluation of occupational exposure to benzene series compounds.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1251 ","pages":"124428"},"PeriodicalIF":2.8,"publicationDate":"2025-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142870651","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}