Pranav S Bang, Vishnu P Choudhari, Vikram S Gharge
{"title":"AQbD-guided development of a robust and green SI-RP-HPLC method for impurity profiling of an efonidipine hydrochloride ethanolate and chlorthalidone combination, with LC-MS and NMR-based identification of degradation product in efonidipine.","authors":"Pranav S Bang, Vishnu P Choudhari, Vikram S Gharge","doi":"10.1016/j.chroma.2026.467321","DOIUrl":"10.1016/j.chroma.2026.467321","url":null,"abstract":"<p><p>Efonidipine Hydrochloride Ethanolate (EHE) and Chlorthalidone (CTD) are co-formulated for the management of hypertension owing to their complementary pharmacological actions. Ensuring accurate impurity profiling in such combination formulations is vital for maintaining drug stability, safety and regulatory compliance. However, conventional analytical techniques often face challenges related to sustainability and robustness. Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) remains a key analytical approach for impurity determination, yet the integration of Quality by Design (QbD) principles into its development is still evolving. The present study focuses on developing a novel, sustainable RP-HPLC method for impurity profiling of EHE and CTD tablets using a QbD approach and green chemistry. Chromatographic separation was achieved on a Zorbax SB C8 column (150 mm × 4.6 mm, 5 µm). Critical method parameters such as mobile phase composition and pH were systematically optimized through QbD to enhance method robustness. A photolytic degradation product of EHE was identified as Efonidipine Related Compound A, and a plausible photolytic degradation pathway was proposed. A photolytic degradation product was identified in the LC-MS and its structure was confirmed through NMR spectroscopy. The developed green method exhibited excellent resolution, precision and reproducibility across multiple batches, allowing for effective separation and quantification of impurities. This green QbD-optimized, environmentally sustainable RP-HPLC method provides a reliable and scalable solution for impurity profiling in complex pharmaceutical formulations, aligning with modern quality control and regulatory expectations.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1785 ","pages":"467321"},"PeriodicalIF":4.0,"publicationDate":"2026-09-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148696805","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":"Comparison of ultrahigh- and low-pressure packing methods for preparation of 50 cm long capillary UHPLC columns.","authors":"Tate A Hancock, Robert T Kennedy","doi":"10.1016/j.chroma.2026.467400","DOIUrl":"https://doi.org/10.1016/j.chroma.2026.467400","url":null,"abstract":"<p><p>Interdependent variables including pressure, slurry concentration, and slurry solvent contribute to producing high-efficiency liquid chromatography columns by slurry packing. Most commonly, ultrahigh-pressure (over 2000 bar) slurry packing methods have been observed to generate the highest performing column packed beds. However, low-pressure packing (<200 bar) methods are also commonly used but have not been examined in depth or compared to ultrahigh-pressure packed columns for kinetic performance. In this work, we compare methods that employed low- (100 bar) or ultrahigh-pressures (2070 bar) to slurry pack 50 cm long × 75 µm inner diameter (i.d.) capillaries with 1.7 µm diameter ethylene-bridged hybrid (BEH) C18 particles. Both packing methods utilized a high slurry concentration, with low-pressure packing using a settled slurry (3 mm tall layer of particles in the bottom of a tube with slow stirring) and ultrahigh-pressure packing using a suspended (fast stirring to prevent settling) 200 mg/mL slurry. Columns were evaluated with isocratic separations of small molecules and gradient separations of a peptide standard mixture. Low-pressure packed columns saw an improvement in performance when sonication was used during packing. Low-pressure packed columns achieved a minimum reduced plate height as low as 1.18 and a peak capacity of 534 in <2 h, thus generating comparable separation performance to columns packed at ultrahigh-pressures. Similar column-to-column and run-to-run performance repeatability was also observed for both packing methods. The low-pressure packing technique provides a less technically demanding and more cost-effective approach for preparing high-efficiency capillary columns.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1787 ","pages":"467400"},"PeriodicalIF":4.0,"publicationDate":"2026-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148890552","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":"Emulsive liquid-liquid microextraction using deep eutectic solvents for the determination of sulfonamide antibiotics in urine samples by high-performance liquid chromatography.","authors":"Ying Li, Shuang Feng, Shaojie Chang, Shaofei Shen, Mai Luo, Xu Jing","doi":"10.1016/j.chroma.2026.467423","DOIUrl":"https://doi.org/10.1016/j.chroma.2026.467423","url":null,"abstract":"<p><p>An emulsive liquid‑liquid microextraction (ELLME) technique based on deep eutectic solvents (DES) was developed for the extraction of three sulfonamide antibiotics (SAs) in canine and feline urine, followed by their determination using high‑performance liquid chromatography (HPLC) with a diode array detector (DAD). The DES synthesized from thymol and hexanoic acid was used as an extractant to form an emulsion with water for the efficient extraction of SAs. Without using auxiliary instruments or chemical reagents, the emulsion undergoes spontaneous demulsification upon static standing. No auxiliary equipment, such as vortex mixers, ultrasonic baths, or centrifuges, is required for sample pretreatment. This simplifies operational procedures and shortens the extraction time. The linear range is 0.005-0.5 mg L<sup>-1</sup>, with detection and quantitation limits of 0.002 and 0.005 mg L<sup>-1</sup>, respectively. The extraction recovery ranges from 85.3 % to 97.2 %, with a relative standard deviation <2.7 %. Seven evaluation tools were employed to assess the greenness and practical applicability of the analytical procedure. This simple and eco-friendly DES-ELLME-HPLC-DAD method provides a novel and reliable technical strategy for rapid screening and accurate quantification of veterinary drugs in urine samples.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1787 ","pages":"467423"},"PeriodicalIF":4.0,"publicationDate":"2026-09-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148896146","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}
Kazhal Khazaei, Shahram Seidi, Mahsa Shirkhodaie, Sara Bakhshmaleki
{"title":"A magnetic copper-based metal-organic gel-derived aerogel for spin-assisted dispersive micro-solid phase extraction of trace organophosphorus pesticide residues in plant-based milk alternatives followed by LC-MS/MS.","authors":"Kazhal Khazaei, Shahram Seidi, Mahsa Shirkhodaie, Sara Bakhshmaleki","doi":"10.1016/j.chroma.2026.467418","DOIUrl":"https://doi.org/10.1016/j.chroma.2026.467418","url":null,"abstract":"<p><p>A novel, and efficient spin-assisted dispersive micro-solid phase extraction (SA-DµSPE) method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for quantifying trace levels of organophosphorus pesticide (OPP) residues in plant-based milk alternatives (PBMAs). To fabricate the extraction sorbent, silica-coated magnetite nanoparticles were incorporated into a copper-based metal-organic gel (MOG) network, followed by freeze-drying, yielding a porous magnetic aerogel with excellent adsorption properties. A custom-built electrical device was employed to promote sorbent dispersion and expedite its magnetic separation. Adsorption and desorption parameters were optimized using a rotatable central composite design (RCCD) and one-variable-at-a-time (OVAT) approach. Matrix effect (ME%) values ranged from 15.0% to 34.9%; therefore, a matrix-matched calibration method was employed for OPP quantification. Under the optimal conditions, calibration curves in various matrices were linear within the range of 0.05-200.0 ng mL<sup>-1</sup>, with coefficients of determination (R²) ≥ 0.9978. Limits of detection (LODs) and quantification (LOQs) ranged from 0.03 to 0.08 ng mL<sup>-1</sup> and 0.05 to 0.25 ng mL⁻¹, respectively. Preconcentration factors (PFs) were calculated in the range of 16.3 to 24.3 for different matrices, corresponding to absolute extraction recoveries (ER%) between 40.8% and 60.8%. The method provided relative recoveries (RR%s) of 90.0%-111.3% and relative standard deviations (RSD%) of 3.5-6.8% for the determination of OPPs in almond, soy, and hazelnut milks. The newly prepared aerogel combined with LC-MS/MS provided efficient retention of the target analytes, which, together with the other analytical figures of merit, confirms the proposed method as a suitable alternative for OPP determination in PBMAs.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1787 ","pages":"467418"},"PeriodicalIF":4.0,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148890545","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}
Shuping Qiang, Mahima Seeborun, Albert L Juhasz, Peter Hoffmann
{"title":"An integrated LC-MS/MS workflow for multi-matrix determination of glyphosate and aminomethylphosphonic acid for occupational exposure assessment.","authors":"Shuping Qiang, Mahima Seeborun, Albert L Juhasz, Peter Hoffmann","doi":"10.1016/j.chroma.2026.467417","DOIUrl":"https://doi.org/10.1016/j.chroma.2026.467417","url":null,"abstract":"<p><p>Glyphosate, a widely used herbicide in agricultural and forestry settings, raises significant concerns regarding potential occupational exposure. However, comprehensive exposure assessment integrating biological and environmental monitoring remains limited, partly due to the lack of analytical workflows capable of supporting multiple sample matrices on a single platform. Here, we developed and validated a high-throughput derivatization-free LC-MS/MS workflow for the determination of glyphosate and aminomethylphosphonic acid (AMPA) in urine, surface wipes, patches and breath zone air monitoring samples collected using Occupational Safety and Health Administration (OSHA) versatile sampler (OVS) tubes. The workflow combines selective solid-phase extraction (SPE) using AFFINIMIP molecularly imprinted polymer cartridges for urine with a simplified universal aqueous extraction workflow for environmental matrices, enabling efficient analysis of diverse matrices using a single analytical platform. Chromatographic separation was achieved on a mixed-mode Obelisc N column within 6 minutes, with the in-sample addition of 0.1 mmol L<sup>-1</sup> methylenediphosphonic acid (MA) significantly improved peak shape and sensitivity. The method demonstrated excellent specificity, accuracy and precision across all matrices. The limits of detection (LODs) for glyphosate and AMPA were 0.1 and 0.2 ng mL<sup>-1</sup> in urine, respectively; and 1.6 ng in surface wipes and patches, and 0.4 ng in OVS air samples for both analytes. The method was successfully applied to 1121 biological and environmental samples collected from forestry workers in Australia, confirming its suitability for real-world exposure assessment. By integrating biomonitoring and environmental monitoring within a single analytical platform, this approach provides a practical and high-throughput tool for comprehensive assessment of occupational glyphosate exposure.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1787 ","pages":"467417"},"PeriodicalIF":4.0,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148896156","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}
Anna Constantinou, Maria Kousi, Abuzar Kabir, Kenneth Furton, Natasa P Kalogiouri, Victoria F Samanidou
{"title":"First report of molecularly imprinted polymer-enhanced fabric phase sorptive extraction for highly selective isolation of bisphenol A from environmental waters prior to high-performance liquid chromatography analysis with diode array detection.","authors":"Anna Constantinou, Maria Kousi, Abuzar Kabir, Kenneth Furton, Natasa P Kalogiouri, Victoria F Samanidou","doi":"10.1016/j.chroma.2026.467406","DOIUrl":"https://doi.org/10.1016/j.chroma.2026.467406","url":null,"abstract":"<p><p>Bisphenol A (BPA) is among the most extensively utilized and widespreadendocrine-disrupting compounds present in consumer products. In this study, a Fabric Phase Sorptive Extraction (FPSE) membrane functionalized with molecularly imprinted polymers (MIPs), in conjunction with high-performance liquid chromatography coupled with a diode array detector (HPLC-DAD), was employed for the quantification of BPA in environmental water samples. The MIP-FPSE-HPLC-DAD method was systematically optimized by evaluating key parameters influencing analytical performance, including sample matrix pH, duration and ratio of magnetic stirring, type and volume of the extraction solvent, vortex-assisted extraction time, and the addition of salt. The MIP-FPSE membranes exhibited reusability for up to ten extraction cycles. The imprinting factor (IF) was determined to be 6.78 ± 0.19 (n = 3), indicating a high degree of selectivity and binding affinity toward BPA. Method validation was performed to assess linearity, sensitivity, accuracy, and precision. The analytical method demonstrated excellent linearity (R² = 0.9990) over the concentration range of 0.025-5.0 mg/L. Recovery rates ranged from 92.7% to 97.1%, with relative standard deviations (RSDs%) below 6.8%, confirming satisfactory repeatability and precision. The limits of detection (LOD) and quantification (LOQ) were calculated as low as 0.008 mg/L and 0.025 mg/L, respectively, underscoring the method's high sensitivity for trace-level BPA detection.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1787 ","pages":"467406"},"PeriodicalIF":4.0,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148890548","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":"Method validation of non-targeted analysis of mainstream smoke constituents from the 1R6F reference cigarette.","authors":"Masahiro Mizuno, Norimichi Orikata, Yoshifumi Mori, So Kikuchi, Yohei Miyashita, Mami Okumura, Akiyoshi Ota, Ryota Kawanishi, Shiori Kido, Yoji Uwano","doi":"10.1016/j.chroma.2026.467409","DOIUrl":"https://doi.org/10.1016/j.chroma.2026.467409","url":null,"abstract":"<p><p>In this study, we developed a systematic validation framework for non-targeted analysis (NTA) and applied it to complementary analytical workflows using comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-TOFMS) and liquid chromatography-trapped ion mobility spectrometry-quadrupole time-of-flight mass spectrometry (LC-TIMS-QTOFMS) for broad profiling of cigarette mainstream smoke constituents. The validation framework evaluated instrumental detection and annotation performance, method-specific library-search thresholds, the accuracy of semi-quantitative concentration estimates, repeatability and intermediate precision, and analytical coverage across two GC × GC-TOFMS methods and three LC-TIMS-QTOFMS methods. An operational reporting threshold of 100 ng per cigarette was selected as the lowest evaluated level at which the mean true-positive rate across the analytical methods was at least 90% and no individual method showed a true-positive rate below 80%. The method-specific library-similarity-score thresholds used to define high-confidence annotations ranged from 700 to 800. For the GC × GC-TOFMS methods, the accuracy of semi-quantitative concentration estimates for the quality control (QC) compounds ranged from 41% to 128%. In the LC-TIMS-QTOFMS methods, the initial semi-quantitative concentration estimates showed substantial compound-dependent positive bias; application of predicted relative response factors reduced this bias, although the accuracy of the adjusted semi-quantitative estimates still ranged from 67% to 428%. The coefficients of variation for repeatability and intermediate precision were below 30% for all evaluated QC compounds across all analytical methods. The summed semi-quantitative concentration estimates obtained using the NTA workflows, together with separately determined amounts of major constituents, including nicotine, water, propylene glycol, glycerin, and triacetin, represented 39.6 mg/cig. This amount corresponded to an apparent mass ratio of 91.0% relative to the gravimetrically determined total particulate matter (TPM) yield. The annotated constituents also demonstrated broad and complementary chemical space coverage in terms of molecular weight and calculated log P. Application of the evaluated workflows to mainstream smoke from the Kentucky reference cigarette (1R6F) resulted in 3590 reported analytical features after consolidation of duplicate \"Confirmed\" identifications across analytical methods. These results demonstrate that the proposed framework provides a systematic basis for evaluating and further developing NTA workflows for cigarette smoke and other complex chemical mixtures.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1787 ","pages":"467409"},"PeriodicalIF":4.0,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148900016","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}
Dominique Hurtaud-Pessel, Pierrick Couedor, Khaled El Hawari, Eric Verdon
{"title":"High resolution mass spectrometry screening method for routine surveillance of pharmacologically active substance residues in meat and milk.","authors":"Dominique Hurtaud-Pessel, Pierrick Couedor, Khaled El Hawari, Eric Verdon","doi":"10.1016/j.chroma.2026.467411","DOIUrl":"https://doi.org/10.1016/j.chroma.2026.467411","url":null,"abstract":"<p><p>This study presents the development and validation of a multi-residue screening method for the determination of 196 analytes in meat and milk using LC-Q-Orbitrap mass spectrometer in accordance with Commission Implementing Regulation (CIR) (EU) 2021/808. Four different multi-residue extraction methods from the literature were compared, and a double extraction combining an acetonitrile/water mixture followed by pure acetonitrile was selected as the most effective approach. The performance of the method showed good specificity for 87% of the target analytes. False negative results remained limited, affecting 6% of analytes in muscle and 8% in milk, and highlighting a few problematic compounds. The detection capability (CCβ) ranged from 5 to 10 µg/kg for 80% of the analytes in both matrices, whereas for the other substances CCβ values were found in the range of 50 to 100 µg/kg. In addition, the method fulfilled the quantification criteria of the CIR (EU) 2021/808 for 106 analytes in muscle and 115 analytes in milk at concentrations ranging from 5 µg/kg to 100 µg/kg. The method was further subjected to external evaluation through participation in different proficiency testing schemes for the determination of multi-class of VMPs. The results showed no false negatives and all obtained z-scores entered within the satisfactory range of ±2, proving that the method is suitable for both qualitative and quantitative screening of veterinary drug residues in animal-derived products and could be envisaged for somehow confirmatory status.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1787 ","pages":"467411"},"PeriodicalIF":4.0,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148890567","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":"Integrating GC-MS profiling and portable mass spectrometry with machine learning for comprehensive chemical characterization and rapid authentication of nine Curcuma species.","authors":"Xuemei Wei, Yixuan Xie, Jianqing Zhang, Yun Li, Yang Yang, Cuicui Wang, Qinhua Chen, De-An Guo","doi":"10.1016/j.chroma.2026.467410","DOIUrl":"https://doi.org/10.1016/j.chroma.2026.467410","url":null,"abstract":"<p><p>Plants of the genus Curcuma are vital medicinal resources; however, their highly similar chemical profiles and morphological features present substantial challenges for accurate species authentication. Here, we established a comprehensive analytical strategy for the precise differentiation of eight medicinal Curcuma species and one counterfeit by integrating untargeted gas chromatography-mass spectrometry (GC-MS) profiling with rapid in situ portable mass spectrometry (PMS) and machine learning. GC-MS analysis tentatively identified ten predominant volatile components, whose potential biological targets and signaling pathways were elucidated via network pharmacology. Chemometric analysis of GC-MS metabolic profiles further enabled the screening of core differential markers driving species discrimination. For rapid on-site detection, in situ PMS fingerprints were acquired and processed using a characteristic ion-based binarization strategy following base peak normalization. When coupled with advanced machine learning algorithms, particularly Ensemble and Efficient Linear classifiers, the system achieved 100% classification accuracy with high computational efficiency. Together, this dual-platform approach provides an effective, and broadly applicable method for quality control and rapid authentication of multi-origin traditional medicines.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1787 ","pages":"467410"},"PeriodicalIF":4.0,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148885842","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}
Yue Yang, Yan Tang, Jing Zhang, Fei He, La Chen, Huanhuan Hong, Luhong Wen
{"title":"Rapid determination of triazine herbicides in environmental and biological fluids by hydroxyl COF-based SBSE combined with dielectric barrier discharge ionization-mass spectrometry.","authors":"Yue Yang, Yan Tang, Jing Zhang, Fei He, La Chen, Huanhuan Hong, Luhong Wen","doi":"10.1016/j.chroma.2026.467414","DOIUrl":"https://doi.org/10.1016/j.chroma.2026.467414","url":null,"abstract":"<p><p>Triazine herbicides are widely used in agricultural production. However, their environmental persistence and mobility pose potential threats to ecological safety and human health. Herein, a novel analytical method integrating stir bar sorptive extraction (SBSE) with airflow-assisted thermal desorption dielectric barrier discharge ionization mass spectrometry (AFA-TD-DBDI-MS), an ambient ionization mass spectrometry (AMS), was developed for the sensitive determination of triazine herbicides. A hydroxyl-functionalized covalent organic framework (COF-HF) was synthesized and used to fabricate COF-HF-coated stir bars via physical adhesion. The as-prepared stir bars exhibited outstanding extraction performance toward triazine herbicides, and the underlying adsorption mechanism was systematically investigated. The established COF-HF-based SBSE-AFA-TD-DBDI-MS method demonstrated good linearity (R² ≥ 0.9957), satisfactory recoveries (91.31%-98.81%), good repeatability (RSD ≤ 8.49%), and low limits of detection (0.0061-0.0312 ng/mL). This study provides a rapid and efficient strategy for monitoring trace triazine pollutants in environmental water and serum matrices.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1787 ","pages":"467414"},"PeriodicalIF":4.0,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148885840","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}