Journal of Chromatography A最新文献

{"title":"Chain-Length dependent IL@MWCNTs adsorbents for solid-phase extraction of aflatoxin B1: Enhancing oil-matrix compatibility and extraction efficiency","authors":"Xin Li ,&nbsp;Jing Zhou ,&nbsp;Juan Xia,&nbsp;Tao Liu,&nbsp;Hongyu Zhi,&nbsp;Ruijin Li,&nbsp;Limin Lu,&nbsp;Hui Chen","doi":"10.1016/j.chroma.2025.466251","DOIUrl":"10.1016/j.chroma.2025.466251","url":null,"abstract":"<div><div>Edible oils are prone to contamination by aflatoxin B₁ (AFB₁), posing significant food safety risks. In this study, a series of imidazolium ionic liquids (ILs) with varying alkyl chain lengths (C₂, C₄, C₆, C₈) were covalently grafted onto multi-walled carbon nanotubes (MWCNTs) via a free-radical method to develop IL@MWCNT adsorbents (EMIM@MWCNT, BMIM@MWCNT, HMIM@MWCNT, OMIM@MWCNT) for solid-phase extraction (SPE) of AFB₁, followed by HPLC-fluorescence detection. Comprehensive characterization revealed that chain length critically influenced material properties: SEM and BET analysis demonstrated that HMIM@MWCNT (C₆) exhibited the highest specific surface area (101.6 m²/g) and optimal pore diameter (35.64 nm), while contact angle measurements and dispersion tests in non-polar solvents highlighted its superior hydrophobicity and oil-matrix compatibility. FTIR and XPS confirmed covalent IL grafting and the presence of oxygenated groups (hydroxyl, epoxy), which facilitated π-π stacking, hydrogen bonding, and electrostatic interactions with AFB₁. Adsorption studies indicated that HMIM@MWCNT achieved the fastest kinetics (equilibrium within 20 min) and highest capacity (45.2 mg/g), following pseudo-second-order kinetics and Freundlich isotherm models. The C₆ chain length balanced hydrophobicity and steric effects, enhancing AFB₁ affinity compared to shorter chains (C₂, C₄) and mitigating aggregation observed with longer chains (C₈). The optimized SPE-HPLC method demonstrated a wide linear range (0.5 μg/L–500 μg/L, R² = 0.9997), ultra-low detection limit (0.1 μg/L), and satisfactory recoveries (88.0–104%) in spiked corn oil with RSD ≤6.0%. The adsorbent retained &gt;98% efficiency over five cycles, underscoring its reusability. This work elucidates the role of IL alkyl chain length in tailoring adsorbent properties for efficient AFB₁ extraction, offering a robust strategy for mycotoxin monitoring in lipid-rich matrices.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1759 ","pages":"Article 466251"},"PeriodicalIF":3.8,"publicationDate":"2025-07-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144713641","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A methylation-assisted gas chromatography-mass spectrometry strategy for comprehensive monosaccharide profiling in Polygonatum polysaccharides: Overcoming limitations of conventional chromatographic techniques","authors":"Liang Xu ,&nbsp;Jinjian Yao ,&nbsp;Zhen Wang ,&nbsp;Songzi Xie ,&nbsp;Jinmei Ou ,&nbsp;Bin Wang","doi":"10.1016/j.chroma.2025.466253","DOIUrl":"10.1016/j.chroma.2025.466253","url":null,"abstract":"<div><div>Conventional methods for analyzing monosaccharides, such as 1-Phenyl-3-methyl-5-pyrazolone (PMP) derivatization coupled with high-performance liquid chromatography (HPLC), struggle to detect ketoses and acidic sugars. This limitation hinders the precise structural analysis of polysaccharides in traditional Chinese medicine (TCM). A methylation-assisted Gas Chromatography-Mass Spectrometry (GC–MS) approach was developed to address this issue in the current study. By optimizing the methylation process and using GC–MS with a BR-17 column and an Electron Ionization (EI) source, simultaneous detection of ten different monosaccharides was achieved within 20 min. GC–MS profiling of monosaccharides generally gives two peaks per analyte, except in the cases of fructose and galacturonic acid. Notably, fructose (Fru) was identified for the first time in the polysaccharides of <em>Polygonatum</em> species: <em>P. sibiricum</em> at 18.55 μg/mg, <em>P. cyrtonema</em> at 16.90 μg/mg, and <em>P. kingianum</em> at 14.35 μg/mg, overcoming the limitations of the inability to detect ketoses in the PMP-HPLC method. Data analysis revealed distinct species-specific markers: <em>P. kingianum</em> polysaccharides (PKP) uniquely contained <em>α</em>-galacturonic acid (α-Gal: 19.95 μg/mg), whereas <em>P. sibiricum</em> polysaccharides (PSP) featured six monosaccharides, including glucose (Glc: 135.45 μg/mg), mannose (Man: 78.95 μg/mg), and ribose (Rib: 26.90 μg/mg), with a total of 299.50 μg/mg. <em>P. cyrtonema</em> polysaccharides (PCP) showed elevated levels of glucuronic acid (GlcA, 38.40 μg/mg). This derivatization-enhanced GC–MS method effectively fingerprints TCM polysaccharides, enabling clear differentiation of <em>Polygonatum</em> species through analysis of monosaccharide composition and total sugar content. This approach establishes clear structural distinctions, overcoming the limitations of conventional chromatographic techniques and enhancing the quality control and authentication of TCM polysaccharides.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1759 ","pages":"Article 466253"},"PeriodicalIF":4.0,"publicationDate":"2025-07-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144721454","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Preparation of a phenylcarbamoylethylenediureido-β-cyclodextrin-bonded phase for enantioseparation and determination of cyproconazole, metconazole and other triazole fungicides in fruits and vegetables by high-performance liquid chromatography","authors":"Jing Lin,&nbsp;Dan Li,&nbsp;Peiyuan Luo,&nbsp;Laisheng Li","doi":"10.1016/j.chroma.2025.466258","DOIUrl":"10.1016/j.chroma.2025.466258","url":null,"abstract":"<div><div>we reported a new phenylcarbamoylethylenediureido-β-cyclodextrin CSP (PUCDP) for HPLC, which was conveniently prepared by immobilizing the addition product of diethylenetriamino-β-CD with 3,5-dichlorophenyl isocyanate onto silica gel. After structural characterization, the chromatographic performance of PUCDP was preliminarily evaluated by using common 11 triazole pesticides as probes. The results showed that PUCDP had strong chiral separation abilities for all triazoles (<em>R</em>s=1.44–3.70). Especially, it could first completely separate triazoles with two chiral centers such as cyproconazole, triadimenol, metconazole, paclobutrazol and bitertanol, into four peaks, respectively. Some effects on the separation and detection were investigated, including the composition of mobile phase, pH value, column temperature, and absorption wavelength. Based on comprehensive optimization of chromatographic conditions and a homemade PUCDP column, we established a new method for the simultaneous separation and determination of twelve triazole pesticide enantiomeric residues (flutriafol, cyproconazole, tebuconazole, and metconazole) in nine kinds of fruits and vegetables (apple, banana, orange, pear, cucumber, green pepper, tomato, wax gourd, cabbage). After simple QuEChERS pretreatment, samples were analyzed under the optimized conditions of a gradient elution program with acetonitrile-water (ACN<img>H₂O) containing 0.5 % triethylammonium acetate (TEAA) buffer (pH=6.30) as the mobile phase at a flow rate of 0.5 mL min^-1, a photo-diode array (PDA) detector at 220 nm, column temperature at 20 °C and an injection volume of 20 μL. The method exhibited good linear relationship (<em>R</em>²=0.9941–0.9999) in the range of 0.5–60 mg l^-1 for all triazole enantiomers. The limits of detection (LODs) and limits of quantification (LOQs) ranged from 0.05 to 0.10 mg kg^-1 and 0.15 to 0.30 mg kg^-1, respectively. The average recoveries of all enantiomers were 81.60 %-104.08 % with <em>intra</em>-day and <em>inter</em>-day relative standard deviations (RSDs) of 1.91 %-3.50 % (<em>n</em> = 5) and 2.05 %-4.49 % (<em>n</em> = 15), respectively. The determination of 54 actual samples indicated the practicality of the method. This simultaneous determination method could save analysis time, and reduce solvent consumption with high analysis efficiency. The excellent performance of PUCDP was mainly related to the rich hydrogen bonds (donors and acceptors), the large π-π stacking and the extended cavity derived from the diphenylurea groups, which was consistent with the results of AutoDock molecular docking.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1759 ","pages":"Article 466258"},"PeriodicalIF":4.0,"publicationDate":"2025-07-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144724198","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Cationic separation of medium strong bases by electrophoretic focusing on inverse electromigration dispersion profile. Sensitive analysis of beta-blockers in blood and water with ESI-MS detection","authors":"Zdena Malá,&nbsp;Petr Gebauer","doi":"10.1016/j.chroma.2025.466250","DOIUrl":"10.1016/j.chroma.2025.466250","url":null,"abstract":"<div><div>Electrophoretic focusing on an inverse electromigration dispersion profile is a method where the migrating profile focuses and separates the analytes and transports them to the detector. Although so far only a few anionic and cationic electrolyte systems have been reported for this technique, it has proved its separation and concentration power and potential for sensitive and selective analyses of samples with complex matrices, typically without any pretreatment. To extend its applicability, there is need for the design of electrolyte systems covering other pH ranges and potential analyte groups. This work describes the first functional cationic system for electrophoretic focusing on inverse electromigration dispersion profile in the alkaline region, based on pentamethylenediamine and acetohydroxamic acid. Computer simulation and experiments have shown that the designed electromigration dispersion profile can be split into smaller sub-profiles to reach increased performance and selectivity. The practical applicability of the system is demonstrated on the analysis of beta-blockers in capillary blood via the dried blood spot technique in combination with electrospray-ionization mass-spectrometric detection. The method allows direct injection of aqueous dried blood spot extracts and sensitive determination of metoprolol and betaxolol in real samples with limits of detection at the 2 nM (500 ngL^-1) level. Experiments with direct injection of spiked water samples show that the method can be used also for analysis of beta-blockers in waters with almost the same sensitivity.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1759 ","pages":"Article 466250"},"PeriodicalIF":4.0,"publicationDate":"2025-07-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144721455","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Extraction of aloe polysaccharides by recoverable aqueous biphasic system composed of thermo-sensitive magnetic ionic liquid and pH-sensitive copolymer","authors":"Tian Yao,&nbsp;Jialin Liu,&nbsp;Meilin Feng,&nbsp;Cailing Feng","doi":"10.1016/j.chroma.2025.466249","DOIUrl":"10.1016/j.chroma.2025.466249","url":null,"abstract":"<div><div>In this work, thermo-sensitive magnetic ionic liquids were applied to construct aqueous biphasic systems with pH-sensitive copolymers. These triple-responsive aqueous biphasic systems have been developed for the purification of aloe polysaccharides from crude extract of aloe pulp. These systems are responsive to external magnetic field and can accelerate phase separation applying only a magnet. Thermo-sensitive magnetic ionic liquid and pH-sensitive copolymer as phase-forming reagents can be effortlessly recovered through heating and pH adjustment without any use of organic solvents. The developed system presents several benefits, including expeditious extraction, magnet-assisted phase separation, efficient recovery induced by temperature and pH changes, especially without utilization of any organic solvent throughout the entire extraction and recovery procedures. Comprehensive studies on phase behaviors were carried out, providing valuable insights for extraction applications. The process of extraction, purification and recovery of aloe polysaccharides were thoroughly examined and optimized. Under optimal conditions, a near-total extraction of aloe polysaccharides was observed in the copolymer-rich phase, while the majority of the primary impurity, protein, was partitioned into the magnetic ionic liquid phase. Subsequent analyses of monosaccharide constituents confirmed high purity of the aloe polysaccharides product, with no impurities found. The recycled magnetic ionic liquid and copolymer have been demonstrated to possess recyclability for a minimum of seven cycles, exhibiting steadily good performance. This simple and green aqueous biphasic system exhibits considerable potential for extraction and purification of aloe polysaccharides, as well as other natural products.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1759 ","pages":"Article 466249"},"PeriodicalIF":3.8,"publicationDate":"2025-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144713398","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Quantitative analysis of hydrogen mass fraction in catalytically reacted 1,4-bis(phenylethynyl)benzene by gas chromatography-mass spectrometry","authors":"Lei Yu ,&nbsp;Bo Liu ,&nbsp;Pucheng Wang ,&nbsp;Shuai Liu ,&nbsp;Junjie Sheng ,&nbsp;Yinyong Ao","doi":"10.1016/j.chroma.2025.466247","DOIUrl":"10.1016/j.chroma.2025.466247","url":null,"abstract":"<div><div>1,4-Bis(phenylethynyl)benzene blended with an activated carbon-supported palladium catalyst has been demonstrated as an effective hydrogen scavenger in reducing hydrogen gas accumulation within vacuum-sealed and hermetically closed systems. Accurate determination of the hydrogen mass fraction in reacted 1,4-bis(phenylethynyl)benzene (DEB) is essential for guiding the replacement of hydrogen-absorbing materials. In this study, a novel method for determining the hydrogen mass fraction in reacted DEB was developed. First, the reaction products of DEB with hydrogen gas were isolated and characterized using gas chromatography-mass spectrometry (GC–MS). A correlation between the peak areas of the reaction products and the saturation level of DEB was established. The hydrogen mass fraction in the reacted DEB was precisely determined based on the relationship between DEB saturation and hydrogen content. Furthermore, the effect of O₂ on the hydrogen uptake of DEB was investigated using the developed method. The results demonstrate that this method exhibits high detection sensitivity and accuracy for determining the hydrogen mass fraction in reacted DEB, offering a reliable approach for monitoring hydrogen absorption in such systems.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1759 ","pages":"Article 466247"},"PeriodicalIF":3.8,"publicationDate":"2025-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144713687","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of volatile fluorotelomer alcohols in water by stir bar sorptive extraction–liquid desorption and gas chromatography–chemical ionization tandem mass spectrometry","authors":"Peter Tölgyessy,&nbsp;Milan Laurenčík,&nbsp;Tamara Vranová,&nbsp;Michal Kirchner","doi":"10.1016/j.chroma.2025.466246","DOIUrl":"10.1016/j.chroma.2025.466246","url":null,"abstract":"<div><div>We developed a simple, environmentally friendly method for determining seven fluorotelomer alcohols (FTOHs) in water, including EU Water Framework Directive priority substances 6:2 and 8:2 FTOH. The method combines stir bar sorptive extraction with liquid desorption (SBSE–LD) and gas chromatography–tandem mass spectrometry using positive chemical ionization (GC–PCI-MS/MS) analysis, while addressing FTOH volatility issues during sample preparation. Detection and quantification limits ranged from 0.068 to 0.60 ng L^–1 and 0.23–2.0 ng L^–1, respectively, with a linear range of 0.5–80 ng L^–1. Intra-day precision (RSDs) was 2.3–12 %, and trueness was generally 81–114 %, except for 12:2 FTOH (58–124 %). Strong matrix effects (up to 78 %) were observed for some FTOHs, requiring matrix-matched calibration. The method showed good environmental compatibility, receiving an AGREEprep score of 0.63, which reflects the absence of hazardous chemicals, the use of reusable materials, zero waste generation, and enhanced operator safety. Its practical applicability, as evaluated using the Blue Applicability Grade Index (BAGI), yielded a score of 60.0. The method was successfully applied to river, groundwater, and tap water samples, confirming its suitability for routine environmental monitoring of volatile FTOHs.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1759 ","pages":"Article 466246"},"PeriodicalIF":3.8,"publicationDate":"2025-07-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144713686","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Machine learning enhanced process design in protein a chromatography","authors":"Andrea Galeazzi ,&nbsp;Steven Sachio ,&nbsp;Elizabeth Edwards ,&nbsp;David Hilton ,&nbsp;Maria M. Papathanasiou","doi":"10.1016/j.chroma.2025.466193","DOIUrl":"10.1016/j.chroma.2025.466193","url":null,"abstract":"<div><div>Quality by Digital Design (QbDD) employs in-silico experimentation to reduce wet-lab reliance and accelerate development. Design space identification is critical for QbDD to overcome bottlenecks and streamline process design. Traditional design space identification methods require costly, high-fidelity models. This work introduces a machine learning-enhanced design space identification approach that utilises wet-lab data. A transfer learning framework is developed under limited data availability by leveraging synthetic datasets created using off-the-shelf mechanistic models. An artificial neural network is constructed and used to classify feasible design regions under high, moderate, and low data availability (HDA, MDA, LDA). Results show strong performance in HDA for the data-driven method, with transfer learning improving accuracy in MDA and being essential in LDA. This approach demonstrates machine learning’s potential to enable cost- and time-efficient process design in early-stage biopharmaceutical development.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1759 ","pages":"Article 466193"},"PeriodicalIF":3.8,"publicationDate":"2025-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144679762","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Enhanced by ionic liquids: Magnetic molecularly imprinted polymers-magnetic solid-phase extraction-UHPLC-UV for sensitive detection of benzimidazoles in multiple food matrices","authors":"Tianyi Xue ,&nbsp;Yue Yuan ,&nbsp;Yiyang Yuan ,&nbsp;Zhexue Song ,&nbsp;Zhili Xiong ,&nbsp;Honggang Wang","doi":"10.1016/j.chroma.2025.466237","DOIUrl":"10.1016/j.chroma.2025.466237","url":null,"abstract":"<div><div>Benzimidazoles (BZDs) as fungicides and veterinary drugs may remain in various food matrices, posing potential risks to human health. It is challenging to detect trace BZDs under complex matrix interferences. In this study, ion liquid magnetic molecularly imprinted polymers (IL-MMIPs) for the selective extraction of six BZDs from complex matrices were synthesized via surface imprinting technology with vinyl-functionalized Fe₃O₄@SiO₂ as magnetic carriers. Importantly, the synthesized 1-vinyl-3-amidomethylimidazolium chloride ([VAFMIM]Cl-IL) was used as the functional monomer, which could form π-π, hydrogen bonds, electrostatic interactions, ion exchange, and hydrophobic interactions with BZDs. A series of adsorption test results demonstrated that IL-MMIPs exhibited superior selectivity, with high imprinting factors (3.77–4.41) and excellent adsorption capacities (18.26 mg/g). Furthermore, coupling with ultra-high performance liquid chromatography (UHPLC) analysis, an effective, sensitive and selective analysis method based on IL-MMIPs-MSPE-UHPLC integrated technology was established and validated for the quantification of 6 BZDs from multiple food matrices. The results showed remarkable sensitivity with limits of quantification 1.5–10.0 μg/kg and expected recoveries (85.1 %-103.6 %). The method satisfied the detection standards of China and the European Union (EU) and had been applied to food matrices including pork, milk, eggs, drinking water, grapes, cucumbers samples. Finally, trace amounts of thiabendazole were detected only in grapes (533 μg/kg) and eggs (79 μg/kg), demonstrating practical significance for detecting trace BZDs in complex matrices.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1759 ","pages":"Article 466237"},"PeriodicalIF":3.8,"publicationDate":"2025-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144695390","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Methodological approach for a simultaneous determination of persistent and non-persistent organic pollutants in human blood (serum/plasma) using gas chromatography and mass spectrometry techniques","authors":"Carolina M. Bustamante ,&nbsp;Paula Ruiz ,&nbsp;Atiya B. Rifat ,&nbsp;Natalia Bravo ,&nbsp;Joan O. Grimalt ,&nbsp;Mercè Garí","doi":"10.1016/j.chroma.2025.466235","DOIUrl":"10.1016/j.chroma.2025.466235","url":null,"abstract":"<div><div>Human biomonitoring of persistent organic pollutants (POPs) remains essential for tracking long-term exposure, evaluating health risks, and assessing the effectiveness of regulatory bans. For this purpose, an experimental and analytical methodology has been optimized allowing the determination of 47 POPs, encompassing chlorinated cyclodienes, chlorobenzenes, cyclohexanes, polychlorodiphenyl derivatives, several congeners of polychlorobiphenyls (PCBs) and polybromodiphenyl ethers (PBDEs, including the deca-BDE), as well as three non-persistent chemicals (namely quintozene, tecnazene and vinclozolin). The method uses a single liquid-liquid extraction procedure with 500 µL of serum/plasma. Instrumental analysis involves gas chromatography (GC) with electron capture detection (ECD) for the analysis of organochlorines, and a subsequent injection into a GC coupled to mass spectrometry in negative chemical ionization mode (MS-NCI) for the determination of PBDEs. The analytical procedure has been successfully validated, demonstrating high sensitivity (limits of detection: 0.0016–0.012 ng/mL; limits of quantification: 0.0029–0.021 ng/mL), acceptable linearity (R² &gt; 0.9962), good precision (coefficients of variation &lt;25%, except for BDE-209), satisfactory accuracy (recoveries within 70–130% for 41 out of 47 compounds) and minimal matrix effects. Proficiency Testing Materials from the AMAP Ring Test for POPs in human serum confirmed the method’s reliability with results within the accepted reference range. This method represents an efficient and practical approach for human biomonitoring studies, with a simplified workflow suitable for routine application.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1759 ","pages":"Article 466235"},"PeriodicalIF":4.0,"publicationDate":"2025-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144724199","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}