Journal of Chromatography A最新文献

{"title":"Nontarget screening and suspect identification of organic chlorinated compounds in cosmetics and personal care products using UHPLC-Q-Orbitrap-HRMS","authors":"Tao Yang ,&nbsp;Xinling Li ,&nbsp;Jianhua Tan ,&nbsp;Wenyao Liang ,&nbsp;Xianzhi Peng","doi":"10.1016/j.chroma.2026.466681","DOIUrl":"10.1016/j.chroma.2026.466681","url":null,"abstract":"<div><div>Organic chlorinated compounds have been extensively incorporated into cosmetics and personal care products (CPCPs) as germicides, surfactants, and oil-controlling agents, leading to potential human exposure and associated health risks. However, available research has mostly been limited to several chlorinated compounds in CPCPs, e.g., triclosan and triclocarban. In this study, an integrated analytical framework was established combining isotope-pattern–based nontarget screening with database-assisted suspect identification to comprehensively characterize organic chlorinated compounds in CPCPs. The framework was successfully validated by screening and identification of chlorinated compounds in children’s skincare products for sale in China. A total of 227 chlorinated compounds were tentatively identified, including 3 confidence level (CL)1, 9 CL2, 93 CL3, and 122 CL4 compounds with RDBE values of 0 - 29 and molecular masses of 128 - 931 Da. Heterocyclics and ethers were predominant among the CL1–CL3 compounds. Chlorhexidine was quantified maximally at 0.456 %. Triclosan, elubiol, and 4-chloroaniline were also detected in at least one product although they have been banned in skincare products. Overall, the results demonstrated robustness of the comprehensive analytical framework in identifying and characterizing chlorinated compounds in CPCPs. In addition, this research shed light on potential exposure of young children to a cocktail of chlorinated compounds, underscoring urgent need for strict regulations of chemical addition and transparent ingredient labeling to ensure safe use of CPCPs.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466681"},"PeriodicalIF":4.0,"publicationDate":"2026-01-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145941913","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 metabolite profiling of herbal products using an integrated 4-in-1 analysis system and the MetaboTarget algorithm","authors":"Mengyuan Wang,&nbsp;Yunuo Fan,&nbsp;Ye Zhang,&nbsp;Ling Chen,&nbsp;Bin Li,&nbsp;Ping Li","doi":"10.1016/j.chroma.2026.466671","DOIUrl":"10.1016/j.chroma.2026.466671","url":null,"abstract":"<div><div>The inherent chemodiversity and complexity of herbal products make their quality control extremely challenging. In this work, a comprehensive analysis strategy through combining a polarity-extended liquid chromatography-mass spectrometry system (4-in-1 analysis system) and a metabolite-oriented targeted screening algorithm (MetaboTarget) for herbal products was proposed. The 4-in-1 analytical technique significantly expanded detection coverage of analytes through polarity extension. The Python-based MetaboTarget algorithm constructs a predictive database of potential metabolites by integrating Phase I/II metabolic reaction rules with parent drug components absorbed into the blood. Using precursor ions for targeted DDA scanning of plasma samples enables comprehensive metabolite characterization through integration with feature-based molecular networking (FBMN). The developed strategy was successfully applied to the deep <em>in vitro</em> and <em>in vivo</em> analysis of chemical components of Gegen Qinlian Decoction (GQD). As a result, 303 components in GQD and 181 metabolites in plasma were annotated. This integrated strategy enables simultaneous detection of compounds across the full polarity spectrum (high/medium/low) while overcoming key challenges in metabolite identification through the MetaboTarget algorithm, which effectively addresses issues arising from strong endogenous interference and low target abundance, thereby providing a powerful tool for comprehensive characterization of complex herbal products.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466671"},"PeriodicalIF":4.0,"publicationDate":"2026-01-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145916404","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":"Development of a chiral mass spectrometry derivatization reagent for amino acid enantiomer analysis: Metabolic investigation of DL-amino acids in the serum of nephritis patients","authors":"Xinxin Kong ,&nbsp;Zongshuo Sun ,&nbsp;Xinyi Xu,&nbsp;Xi-Ling Li,&nbsp;Jin Ji Li,&nbsp;Jun Zhe Min","doi":"10.1016/j.chroma.2026.466677","DOIUrl":"10.1016/j.chroma.2026.466677","url":null,"abstract":"<div><div>A chiral mass spectrometry derivatization reagent, <em>(R)</em>/<em>(S)</em>-(5-(2-(((1-(p-toluenesulfonylmethylamino)vinyl)oxy)carbonyl)pyrrolidin-1-yl)-5-oxopentyl) triphenylphosphonium bromide (TPP-<em>(R)</em>/<em>(S)</em>-BSA), was developed in this study. The derivatization reagent carries a permanent positive charge and incorporates an α-acyloxy acetylenamide moiety, enabling highly sensitive detection and stereochemical resolution of amino-containing enantiomers. Exposure of DL-amino acids to TPP<em>-(R)</em>/<em>(S)</em>-BSA under heating at 70 °C for 60 min resulted in formation of the corresponding diastereomers. Fine-tuning of the separation conditions enabled clear resolution of fifteen enantiomeric amino acid pairs on a BEH C18 column, with Rs values spanning 1.02–14.49. Except for Pro, Gln, and His, all DL-amino acid pairs showed Rs values above 1.5, indicating effective enantiomeric separation under standardized conditions. Based on the TPP-<em>(S)</em>-BSA derivatization strategy, we developed a UHPLC<img>HRMS assay with excellent sensitivity and selectivity, enabling concurrent resolution and determination of 13 DL-amino acid enantiomeric pairs together with glycine in human serum. The method provided excellent linearity within 0.05–1000 μM (R² ≥ 0.9914), with limits of detection (LOD) between 0.2 and 4.5 fmol. For both intra-day and inter-day evaluations, the observed precision fell within the range of 0.92%–14.00%, while recovery rates averaged 97.88%–111.78%, and matrix effects were within 3.82%–14.58%. Furthermore, statistical analysis of DL-amino acid metabolic concentrations in serum from healthy volunteers and nephritis patients enabled the construction of a diagnostic model integrating differentially expressed enantiomers, providing a potential screening tool for nephritis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466677"},"PeriodicalIF":4.0,"publicationDate":"2026-01-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145941930","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 nucleosides in serum by two-dimensional magnetic solid-phase extraction microfluidic chip/liquid chromatography-mass spectrometry","authors":"Yongzhe Cheng ,&nbsp;Yangkun Sun ,&nbsp;Ningning Wang ,&nbsp;Qiangqiang Jia ,&nbsp;Linghao Zhao ,&nbsp;Zeyu Wu ,&nbsp;Yuerong Wang ,&nbsp;Hongyang Zhang ,&nbsp;Min Zhang ,&nbsp;Ping Hu","doi":"10.1016/j.chroma.2026.466678","DOIUrl":"10.1016/j.chroma.2026.466678","url":null,"abstract":"<div><div>A two-dimensional magnetic solid-phase extraction microfluidic chip (2D-MSPE-chip) was designed in this paper. A microcolumn array was integrated before two serially connected extraction chambers to filter particles in the sample. The two magnetic nanomaterials with orthogonal separation mechanism of Fe₃O₄@UiO-66-C18 and Fe₃O₄@MOF@COF-B(OH)₂ were filled into the extraction chamber, respectively, and were used to effectively eliminate matrix effects and enrich the targets. The 2D-MSPE-chip was combined with liquid chromatography-mass spectrometry (LC-MS) for the determination of eight nucleosides in serum samples. The validation results showed that the 2D-MSPE-chip/LC-MS method had excellent linear range (2–1000 ng/mL), high sensitivity (detection limit of 0.02–0.22 ng/mL), good repeatability (intra-day precision ≤5.2%, inter-day precision ≤7.2%) and a negligible absolute matrix effect (93.1%-101.9%). The recovery rate of the spiked serum samples of prostate cancer patients and healthy person was 90.8%-109.1%, indicating a high accuracy. The inosine level decreased and adenosine level increased in the serum of prostate cancer patients (<em>p</em> &lt; 0.01), suggesting the correlation between nucleosides and the cancer.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466678"},"PeriodicalIF":4.0,"publicationDate":"2026-01-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145941867","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 green and practical strategy for therapeutic drug monitoring of teicoplanin A2 components in human plasma using functionalized liquid film solvent bar microextraction coupled with high-performance liquid chromatography–ultraviolet detection","authors":"Jie Tian ,&nbsp;Yi-fang Zhang ,&nbsp;Yu-feng Sun ,&nbsp;Dou Yan ,&nbsp;Shuang Hu ,&nbsp;Rong-rong Xing ,&nbsp;Run-qin Wang ,&nbsp;Li Yang ,&nbsp;Xuan Chen","doi":"10.1016/j.chroma.2026.466673","DOIUrl":"10.1016/j.chroma.2026.466673","url":null,"abstract":"<div><div>A novel functionalized liquid film solvent bar microextraction (FLF-SBME) method coupled with high-performance liquid chromatography–ultraviolet detection (HPLC/UV) was developed for the extraction and subsequent determination of five A₂-components of teicoplanin, TA_2-1, TA_2-2, TA_2-3, TA_2-4 and TA_2-5, simultaneously in human plasma. The microextraction mechanism of FLF-SBME was systematically elucidated, in which tri-<em>n</em>-octyl methyl ammonium chloride (TOMAC) was employed to modify polypropylene hollow fibers (PP-HFs), enabling efficient enrichment and separation of the target analytes from plasma. The key extraction parameters influencing efficiency were thoroughly optimized. Under optimal conditions, the method provided high enrichment factors (36–59) for all five A₂ components, along with good linearity (1.0–110 µg/mL; <em>r</em> &gt; 0.99), limits of detection of 0.5–3.0 µg/mL, and lower limits of quantification of 1.0–5.0 µg/mL. The intra- and inter-day precision (RSD &lt; 12.2 %) and accuracy (recoveries: 91.5–110.3 %) were satisfactory. With its notable enrichment capability, high selectivity, sensitivity, and reliability, the proposed FLF-SBME–HPLC/UV method is well-suited for the monitoring of teicoplanin in human plasma.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466673"},"PeriodicalIF":4.0,"publicationDate":"2026-01-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145931630","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":"Ultrasensitive detection of triazine herbicides in food via dispersive solid-phase extraction with nanoconfined task-specific ionic liquids in tunable hollow porous carbon spheres","authors":"Xu Xu,&nbsp;Yuanjun Liao,&nbsp;Yuhan Guo,&nbsp;Yi Jiang,&nbsp;Lei Zhang","doi":"10.1016/j.chroma.2026.466672","DOIUrl":"10.1016/j.chroma.2026.466672","url":null,"abstract":"<div><div>Triazine herbicides are widely detected in food and pose significant hazards to ecosystems and human health. In this study, a nanoconfined composite of task-specific ionic liquids (TSILs) within hollow porous carbon spheres (HPCS), denoted TSILs@HPCS, was synthesized via post-impregnation for selective enrichment and efficient extraction of triazine herbicides. Hydrophobic TSILs incorporating [NTf₂^-] anion were systematically prepared. Confinement within HPCS tunable pores yielded a 6.0-fold increase in triazine herbicide adsorption capacity relative to pristine HPCS. The TSILs@HPCS composite serves as a multifunctional adsorbent, enabling the simultaneous sorptive removal, highly sensitive detection, and sieving of analytes. A dispersive solid-phase extraction method coupled with high-performance liquid chromatography was developed to quantify trace triazine herbicides in complex food matrices. This approach demonstrated low detection limits (0.06–0.12 μg kg^-1) and high enrichment factors (124–192), confirming its suitability for residue analysis. These results establish TSILs@HPCS as a promising adsorbent for preconcentrating triazine herbicides in food samples.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466672"},"PeriodicalIF":4.0,"publicationDate":"2026-01-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145916529","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":"Structure-guided design of a minimal epitope tag and nanobody affinity system","authors":"Jiayi Tan ,&nbsp;Limin Zhao ,&nbsp;Mu Li ,&nbsp;Kanglong Yang ,&nbsp;Yue Li ,&nbsp;Yuqing Ding ,&nbsp;Heng Liu ,&nbsp;Houjun Xia ,&nbsp;Chongyuan Wang ,&nbsp;Jiawei Li","doi":"10.1016/j.chroma.2026.466675","DOIUrl":"10.1016/j.chroma.2026.466675","url":null,"abstract":"<div><div>The isolation of recombinant proteins commonly relies on affinity-based methods. Nevertheless, widely used tags and solid supports are frequently constrained by insufficient specificity, harsh elution requirements, and cost inefficiency. Here, we developed a robust purification system based on a nanobody that specifically recognizes a short peptide epitope. The nanobody is produced at high yield in a prokaryotic expression system, and the corresponding peptide tag, comprising only 6–7 amino acids, can be fused to either the N- or C-terminus of target proteins. We demonstrate that this system enables one-step purification of diverse soluble and membrane proteins from cell lysates, with high purity and yield. Bound proteins are gently eluted under non-denaturing conditions using a competitive synthetic peptide, achieving a recovery yield of over 90%. Furthermore, the nanobody-conjugated resin maintains consistent binding capacity over at least 10 reuse cycles. Given its high specificity, mild elution, reusability, and simplicity, we propose this system as a versatile and efficient platform for high-quality protein purification, with broad applicability in proteomics, structural biology, and biotherapeutic development.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466675"},"PeriodicalIF":4.0,"publicationDate":"2026-01-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145941883","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":"Enrichment of pyrethroid insecticides using effervescent-assisted ionic liquid functionalized in melamine sponge for pipette tip micro solid-phase extraction","authors":"Dararat Saenkam ,&nbsp;Pirom Suwannasom ,&nbsp;Jitlada Vichapong","doi":"10.1016/j.chroma.2026.466674","DOIUrl":"10.1016/j.chroma.2026.466674","url":null,"abstract":"<div><div>A preconcentration and detection method using ionic liquid for embedded in melamine sponge for pipette tip micro solid-phase extraction of pyrethroid insecticides coupled to HPLC was developed for trace amount of pyrethroids residue detection. The synthesis of ionic liquid was accomplished by using tributylhexadecylphosphonium bromide ([P₄₄₄₁₂]Br) and potassium hexafluorophosphate (KPF₆), after that effervescent process was carried out by adding sodium carbonate into a centrifuge tube. The as-prepared ionic liquid was then embedded into melamine sponge, and used for pipette tip micro solid-phase extraction of insecticides in fruit juice matrices. After impregnation, the morphological and structural properties of the sorbents were characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. Under the selected conditions, the method exhibited wide linear range (2 – 100 μg <span>l</span>^-1) with a coefficient for determination (R²) greater than 0.99. The limit of quantification (LOQ) and limit of detection (LOD) were in the range of 2 – 3 μg <span>l</span>^-1 and 0.7 – 1 μg <span>l</span>^-1, respectively. Good reproducibility (RSD &lt; 4.65%, <em>n</em> = 5) were achieved. Moreover, the proposed method provided high enrichment factors (EF) ranging from 36.50 to 45.52 folds. The sorbent was then applied to extract pyrethroids in fruit juice. Accuracy was excellent and acceptable recoveries were attained. The greenness profiles were evaluated utilizing multiple assessment metrics including the Analytical Eco-Scale, AGREE Assessment, and BAGI.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466674"},"PeriodicalIF":4.0,"publicationDate":"2026-01-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145909697","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":"Developing 2D mzCompare for single comprehensive two-dimensional chromatography time-of-flight mass spectrometry chromatograms: Substantial resolution enhancement in the context of statistical overlap theory","authors":"Wenjing Ma,&nbsp;Caitlin N. Cain,&nbsp;Robert E. Synovec","doi":"10.1016/j.chroma.2025.466669","DOIUrl":"10.1016/j.chroma.2025.466669","url":null,"abstract":"<div><div>Accurate identification of all detectable analyte components in a single comprehensive two-dimensional (2D) gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS) chromatogram is a fundamental interest in the field. While commercial software tools intended for this purpose are available, the performance of these tools to generate an accurate peak table has generally not been validated. To address this, we developed a new algorithmic software approach called 2D mzCompare to generate accurate peak tables for GC × GC-TOFMS. Extending from our original method for one-dimensional GC–MS data, the 2D mzCompare algorithm discovers selective mass channels (<em>m/z</em>) for each analyte to resolve overlapping peaks and improve analyte identification, by leveraging the similarity in retention time and peak shape across <em>m/z</em> of the same analyte. The 2D mzCompare algorithm calculates the peak shape similarity between <em>m/z</em> at every modulation, followed by clustering and focusing steps, to generate a final peak table. To evaluate this software, we simulated realistic GC × GC-TOFMS data in the context of the statistical overlap theory (SOT), so the exact number and identities of analytes are known <em>a priori</em>. Utilizing an in-house mass spectrum library of similar compounds, GC × GC-TOFMS chromatograms were simulated with varying degrees of 2D chromatographic saturation (<span><math><msub><mi>α</mi><mrow><mn>2</mn><mi>D</mi></mrow></msub></math></span>). At low saturation factors (<span><math><msub><mi>α</mi><mrow><mn>2</mn><mi>D</mi></mrow></msub></math></span> = 0.01, 0.03, and 0.1), over 95% of the simulated components are found to be mathematically resolved singlets (pure analyte components) by 2D mzCompare. Meanwhile, approximately 62% were found at <span><math><msub><mi>α</mi><mrow><mn>2</mn><mi>D</mi></mrow></msub></math></span> = 1, exceeding predictions made by SOT. Application of 2D mzCompare computationally reduces the ²D peak widths, resulting in an ∼12-fold reduction in <span><math><msub><mi>α</mi><mrow><mn>2</mn><mi>D</mi></mrow></msub></math></span>. The results of this research are simultaneously two-fold. First, we provide a new algorithmic approach, 2D mzCompare, to resolve overlapped analytes in GC × GC-TOFMS data, and second, we validate the accuracy of the software performance using SOT.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466669"},"PeriodicalIF":4.0,"publicationDate":"2026-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145909699","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":"Ionic liquid-based aqueous two-phase extraction as a pretreatment strategy for the determination of 38 pharmaceuticals and personal care products in aquatic environments by HPLC-MS/MS","authors":"Shuo Xie ,&nbsp;Wenbin Zhang ,&nbsp;Yike Han ,&nbsp;Xinyan Dong ,&nbsp;Wanning Li ,&nbsp;Penghui Li ,&nbsp;Liyun Kong","doi":"10.1016/j.chroma.2026.466670","DOIUrl":"10.1016/j.chroma.2026.466670","url":null,"abstract":"<div><div>The accurate determination of pharmaceuticals and personal care products (PPCPs) in wastewater is crucial for comprehensive environmental risk assessment and human exposure evaluation. Given the complex matrices of aqueous environmental samples, efficient sample preparation remains a critical challenge in analytical procedures. This study presents an ionic liquid-based aqueous two-phase system (IL-ATPS) extraction methodology used as a pretreatment step prior to high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the simultaneous determination of 38 PPCPs. A mechanistic investigation revealed that target analytes with more hydrogen-bonding sites and higher hydrogen-bond donor (HBD) capacity exhibited enhanced solubility in ILs. In addition, IL anions with stronger hydrogen-bond acceptor (HBA) capacity further improved the solubility of the 38 PPCPs. These findings indicate that hydrogen bonding between analytes and ILs likely played a critical role in the dissolution mechanism. The established IL-salt ATPS extraction method utilized a 15 mL aqueous sample, 0.2 g tetraethylammonium acetate ([N₂₂₂₂][OAc]), and 12 g K₂HPO₄, with a 1-minute vortex mixing. Compared with traditional solid phase extraction (SPE), this approach significantly reduced the sample volume from 1 L to 15 mL, avoided the use of volatile organic solvents, simplified the overall processing, and enabled rapid (&lt;15 minutes) pretreatment. The method demonstrated excellent sensitivity with limits of detection (LODs) ranging from 0.00013 to 0.11 ng/mL. Method validation via standard addition experiments demonstrated satisfactory accuracy, yielding recoveries between 74.3 and 129.8 %. Precision was assessed using both intra-day and inter-day measurements. The intra-day relative standard deviations (RSDs) ranged from 0.7 % to 19.9 %, while the inter-day RSDs ranged from 1.4 % to 18.4 %, demonstrating that the method provides consistent and reproducible results under controlled laboratory conditions. These findings underscore the present IL-based ATPS extraction method, followed by HPLC-MS/MS analysis, as an eco-friendly, robust, and scalable approach for PPCPs monitoring in aqueous environmental samples, offering potential applications in environmental monitoring and risk assessment.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466670"},"PeriodicalIF":4.0,"publicationDate":"2026-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145909693","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}