Journal of Chromatography A最新文献

{"title":"An optimized LC–Q–Orbitrap HRMS method for the DIA-based suspected-target analysis of multi-class pesticide residues and mycotoxins in alkaloid-rich herbal medicines","authors":"Yimin Cao,&nbsp;Lan Lan,&nbsp;Wenting Li,&nbsp;Shen Ji,&nbsp;Ke Wang,&nbsp;Qing Hu,&nbsp;Heng Zhou","doi":"10.1016/j.chroma.2026.466679","DOIUrl":"10.1016/j.chroma.2026.466679","url":null,"abstract":"<div><div>With the growing variety of exogenous hazardous residues, there is a need to develop broad screening and quantification methods beyond triple quadrupole MS. This study adopted an optimized non-targeted acquisition mode. It enabled suspected-target screening and quantification of pesticide residues, while also providing retrospective capability for non-targeted analysis through data-independent acquisition. Orbitrap high-resolution mass spectrometry enables non-targeted screening and trace-level detection, yet its acquisition modes often struggle to simultaneously meet demands for sensitivity, specificity, and repeatability under complex matrix interference. This study employed LC–Q–Orbitrap HRMS for non-targeted analysis of multi-class pesticides and mycotoxins in four alkaloid-rich herbal matrices. Five data-independent acquisition modes were optimized, including the newly introduced Multi-Full MS/vDIA mode. This approach achieved approximately 0.372–0.384 s per full-scan interval, allowing 20–56 full scans per chromatographic peak to improve repeatability. Specific mass-range isolation windows enabled 3–5 MS² scans per cycle, balancing specificity and acquisition efficiency. After optimizing QuEChERS sample preparation and the Multi-Full MS/vDIA mode, a method for 653 pesticides was validated. Recoveries of 82–92% of pesticides fell within 70–120% across matrices, and over 90% had quantitation limits below 0.01 mg/kg, demonstrating high accuracy and sensitivity suitable for qualitative and quantitative analysis. In 62 real samples, 36 pesticides were detected in 43 batches, including highly toxic compounds and paclobutrazol. Mycotoxin screening detected 14 compounds, including aflatoxin B1. Statistical analysis indicated a weak-to-moderate negative correlation trend between pesticide and mycotoxin contamination, with mycotoxin incidence linked to climatic conditions of sample origins.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466679"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145941932","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":"Integrated dual adaptive control of continuous chromatographic separation processes via reinforcement learning","authors":"Foteini Michalopoulou ,&nbsp;Maria M. Papathanasiou","doi":"10.1016/j.chroma.2025.466638","DOIUrl":"10.1016/j.chroma.2025.466638","url":null,"abstract":"<div><div>Continuous chromatographic processes involve nonlinear dynamics, cyclic operation, and strong interactions between operating variables, which make real-time control inherently complex. As process variability and integration increase, there is a growing need for adaptive control frameworks that can maintain performance under changing conditions. In this work, a reinforcement learning (RL) control framework is developed for adaptive operation of continuous chromatographic systems. The controller is trained based on a mechanistic simulation environment and learns to coordinate multiple process inputs based on observed system states. A phase-dependent reward formulation captures the trade-offs between product purity, yield, and operational efficiency, guiding the agent toward stable, high-performance operation from process start-up. The RL controller maintains the target purity under feed variations, flowrate disturbances, and measurement noise, achieves cyclic steady state (CSS) within 10 process cycles, improves process yield from 86 % to 91 %, and increases product recovery by 79 % compared to nominal operation. These results demonstrate that RL can deliver robust and adaptive control for complex multivariable chromatographic systems, providing a framework for intelligent and adaptive process operation.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466638"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145831905","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 and validation of an analytical method for determining triflumezopyrim residues in multiple paddy field matrices (Paddy Water, Paddy Soil, Brown Rice, Rice Husk, and Rice Straw) using GC-ECD and GC-MS","authors":"Xinhong Deng ,&nbsp;Wenxing Wang ,&nbsp;Bin Yang ,&nbsp;Xuguo Zhou ,&nbsp;Lihua Yang","doi":"10.1016/j.chroma.2026.466714","DOIUrl":"10.1016/j.chroma.2026.466714","url":null,"abstract":"<div><div>Triflumezopyrim (TFM), a neonicotinoid insecticide for rice planthopper control, poses potential risks to rice safety and paddy ecosystems via residues. Herein, gas chromatography-electron capture detector (GC-ECD) and GC-mass spectrometry (GC-MS, selected ion monitoring: <em>m/z</em> 206.0, 116.0, 131.0) methods were developed and validated for TFM residue analysis in paddy matrices. Samples were extracted with dichloromethane and purified by dispersive solid-phase extraction. For five matrices, calibration curves showed good linearity (0.01–1 mg L⁻¹, R² ≥ 0.9912). At 0.01, 0.1, 1 mg kg⁻¹ spiking levels, mean recoveries were 81.04%-109.66% (GC-MS) and 89.45%-106.41% (GC-ECD), with relative standard deviations (RSDs) of 3.55%-13.08% and 0.59%-9.30%, respectively. Limits of quantitation (LOQ) were 0.01 mg kg⁻¹ for both techniques; limits of detection (LOD) were 0.001 mg L⁻¹ (GC-ECD) and 0.0005 mg L⁻¹ (GC-MS). These parameters met current residue limits and analytical criteria. Robustness tests revealed minimal impacts of pretreatment and most chromatographic parameters, except carrier gas flow rate (critical, RSD &gt; 10% when varied). The validated method was applied to real paddy field samples from Hunan Province, China, and 20 batches of five types of substrates were screened, with trace TFM in soil (below LOQ). This is the first validated GC-ECD/GC-MS method for TFM trace analysis covering the entire paddy ecosystem (paddy water, paddy soil, brown rice, rice husk, and rice straw), suitable for routine monitoring and supporting TFM environmental/food safety evaluation.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466714"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146034305","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 and validation of a multi-class solid-phase extraction and liquid chromatography tandem mass spectrometry method for emerging contaminants in water","authors":"Madara Weerasooriyagedara ,&nbsp;Jordan M. Partington ,&nbsp;Wejdan Alghamdi ,&nbsp;Mulugeta Legesse Akele ,&nbsp;Stefano Freguia ,&nbsp;Bradley O. Clarke","doi":"10.1016/j.chroma.2025.466655","DOIUrl":"10.1016/j.chroma.2025.466655","url":null,"abstract":"<div><div>A robust and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous quantification of 39 multi-class emerging contaminants (ECs), encompassing diverse groups including industrial chemicals (<em>n</em> = 6), pharmaceuticals (<em>n</em> = 19), personal care products (<em>n</em> = 4), and pesticides (<em>n</em> = 10). LC-MS/MS parameters were systematically optimized, including compound-specific transitions, source conditions, mobile phase composition, injection volumes, and chromatographic flow rates, to maximize signal intensity and ensure reproducible detection. Solid-phase extraction (SPE) was further optimized through evaluation of reconstitution solvent composition, evaporation settings, washing solvents, and elution strategies to improve recoveries and minimize matrix effects. The final method achieved instrument detection limits as low as 0.01 fg on-column, with method detection and quantitation limits of 0.01–1.32 ng/L and 0.03–3.96 ng/L, respectively. Calibration linearity (R² &gt;0.99), recoveries within 70–130%, and intra-/inter-day precision (RSD ≤20%) confirmed the robustness and reproducibility of the protocol. Application to six real water matrices, bottled water, tap water, surface water, seawater, wastewater effluent, and influent, revealed the highest concentrations and widest range of analytes in influent, lower but quantifiable levels of persistent compounds in effluent, and predominantly trace-level detections or non-detects in natural and potable waters. Complementary greenness and applicability assessments using AGREE, MoGAPI, and BAGI highlighted moderate environmental sustainability and strong practical utility, reinforcing the suitability of the method for routine monitoring, source tracking, regulatory compliance, and risk assessment applications requiring ultra-trace sensitivity, high selectivity, and broad chemical coverage.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466655"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145931598","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":"Post-synthetic click chemistry-mediated surface engineering of fluorinated COFs for ultrahigh PFASs uptake","authors":"Chenchen Lin ,&nbsp;Yan Wu ,&nbsp;Tuo Zhen ,&nbsp;Jinxin Chi ,&nbsp;Xucong Lin","doi":"10.1016/j.chroma.2026.466680","DOIUrl":"10.1016/j.chroma.2026.466680","url":null,"abstract":"<div><div>Fluorinated covalent organic frameworks (F-COFs) have attracted widespread attention, owing to their capacity to enhance the adsorption of per- and polyfluoroalkyl substances (PFASs) through F-F affinity and the intrinsic adsorption properties of COFs. F-COFs were usually synthesized based on “de novo synthesis” with commercial fluorinated monomers. However, challenges still remain due to the limited availability of fluorinated monomers, harsh control of crystal growth, and difficult adjustment of surface fluorination. Post-synthetic surface engineering offers great potential for flexibly fabricating F-COFs with tailored functions by modifying functional moieties into the predefined frameworks. Herein, a post-synthetic strategy was pioneered for the fabrication of novel F-COFs with tunable fluorination degrees (noted as COF-V-x-F, x=0-1.0). The approach integrates two synergistic processes: aniline-modulated room-temperature synthesis of the COF-V precursor, and the flexible surface engineering on COF-V via click chemistry to realize controllable fluorination. Using this method, the optimal COF-V-0.33-F was achieved, which contains sufficient fluorinated groups for F-F affinity, high hydrophobicity, and strong molecular adsorption, thus enabling ultra-high PFAS uptake by solid-phase microextraction (SPME). A highly sensitive detection was achieved with limits of detection at 0.2–1.4 ng·L⁻¹ using COF-V-0.33-F fiber coupled with LC-MS/MS. Compared to the commercial PDMS, COF-V and amorphous COP-V-0.33-F, the designed COF-V-0.33-F fiber exhibited rather high extraction capacity with 2.7-65.8, 2.1-10.8, and 2.8-367.1 fold enhancement, respectively. The proposed method was successfully used for PFASs determination in tap, pond and river water. Seven trace PFASs were detected with satisfactory recoveries of 71.0%-117.9%, 75.7%-109.1% and 82.8%-118.2% at spiked concentrations of 20 ng/L, 200 ng/L and 2000 ng/L, respectively. This work posed a simple but powerful access to efficient synthesis of F-COFs with good crystallinity and flexible adjustment of fluorination.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466680"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145948240","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":"Decoding diastereomeric and impurity profiles of phosphorothioated siRNAs via 2D anion-exchange chromatography coupled with ion-pair reversed phase liquid chromatography mass spectrometry","authors":"Quang-Dong Bui ,&nbsp;Willy Verluyten ,&nbsp;Bart Noten ,&nbsp;Tiny Deschrijver ,&nbsp;Sebastiaan Eeltink","doi":"10.1016/j.chroma.2025.466639","DOIUrl":"10.1016/j.chroma.2025.466639","url":null,"abstract":"<div><div>Phosphorothioate (PS) modifications are widely used in RNA-based therapeutic oligonucleotides (ONs), forming diastereomers that enhance ON stability, bioavailability, and cellular uptake. This study presents a strategy for profiling PS-ONs, including both duplexes and the respective single sense and antisense-strand components using anion-exchange chromatography (AEX). The impact of varying PS number and position, ribose modifications, and base compositions in PS-modified pentamer ONs was demonstrated by AEX analysis. Retention behavior was thoroughly characterized using the Boardman and Patrick model. Diastereomers displayed consistent conformations with a similar number of charges involved in adsorption-desorption, though each could be distinguished by unique surface-charged areas. Parameters, including pH, column temperature, counter- and displacing ions, and particle size, were systematically evaluated to optimize diastereomer separations. The optimized method programming a multistep negative gradient led to a baseline separation of 8 diastereomers from a 21-mer ON with 3 PS modifications. Diastereomer profiling of a N-acetylgalactosamine-conjugated duplex ON and palmitoyl-amide-modified small interfering RNA was performed via multiple heart-cut AEX-IP-RPLC-MS 2D analysis. Unlike non-conjugated ONs, the presence of non-ionic conjugates leads to suppression into only two diastereomer peaks during the ¹D AEX chromatograms. Each small-interfering RNA diastereomer fraction was denatured during the ²D IP-RPLC analysis leading to the separation of the antisense and sense strands, allowing qualitative impurity profiling for each strand in subsequent MS coupling.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466639"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145941906","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":"Characterization of biomimetic chromatography columns based on plasma proteins through the Abraham solvation parameter model","authors":"A.L. Valdez-Micheo ,&nbsp;M. Rosés ,&nbsp;S. Amézqueta ,&nbsp;E. Fuguet","doi":"10.1016/j.chroma.2025.466631","DOIUrl":"10.1016/j.chroma.2025.466631","url":null,"abstract":"<div><div>Biomimetic chromatography is a valuable tool for studying drug interactions by mimicking biological environments. In this work, two liquid chromatography systems with stationary phases based on plasma proteins, human serum albumin (HSA) and α₁-acid glycoprotein (AGP), will be evaluated regarding the interactions that these stationary phases establish with neutral and ionized compounds.</div><div>The Abraham solvation parameter model has been used to characterize the chromatographic systems. The models obtained demonstrate that both columns present almost identical selectivity for neutral compounds, with very similar retention mechanisms. The volume of the compounds increases the retention, whereas a high hydrogen bond basicity reduces it. Contrarily, the columns show different selectivity for ionic compounds, especially for anions, which are specifically retained in the HSA column, whereas no or low retention is observed in the AGP column.</div><div>When the obtained models are compared to the models corresponding to other biomimetic chromatography systems, it has been observed that, despite the nature of the stationary phase, all them provide similar selectivity for neutral compounds. In concrete, the two evaluated systems present great similarity to other systems based on liquid chromatography or electrokinetic chromatography that use phosphatidylcholine as stationary phase.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466631"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145802126","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":"Computer-aided fabrication of molecularly imprinted COFs for enantioselective extraction of dihydroquercetin from vine tea","authors":"Yanlong Chen ,&nbsp;Xingyuan Zhang ,&nbsp;Juanqiong Ma ,&nbsp;Na Yang ,&nbsp;Jincheng Su ,&nbsp;Zhiyong Xie ,&nbsp;Fenglian Chen ,&nbsp;Xiao Lin ,&nbsp;Jing Gong ,&nbsp;Qiongfeng Liao","doi":"10.1016/j.chroma.2025.466637","DOIUrl":"10.1016/j.chroma.2025.466637","url":null,"abstract":"<div><div>Efficient separation and enrichment of bioactive flavonoid enantiomers from complex natural matrices remain a major challenge in analytical and life sciences. However, the enantioselectivity of adsorbents for flavonoid extraction remains limited because they lack complementary recognition sites. Herein, molecularly imprinted covalent organic frameworks (MI-COFs) were constructed based on a computer-aided design, which formed well-defined imprinting cavities serving as high-affinity recognition sites. These cavities impart precise and selective recognition toward flavonoid enantiomers, enabling efficient extraction of (2<em>R</em>,3<em>R</em>)-dihydroquercetin (DMY) from vine tea. The MI-COFs exhibited a high adsorption capacity (105 mg/g), excellent selectivity (imprinting factor, 2.7), and rapid adsorption kinetics. The MI-COFs were successfully applied as adsorbents for the targeted extraction of DMY from real vine tea samples, achieving high recoveries (86.8–89.2 %) and an enantiomeric excess of 98 %, with excellent reproducibility. This work demonstrates that rational chiral functionalization of MI-COFs enables precise and selective recognition of target enantiomers. Moreover, it provides a robust and versatile platform for the enantioselective separation and purification of chiral natural products, with broad applicability in food and pharmaceutical analysis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466637"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145831902","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":"2026-02-08","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":"Trends of microextraction methods for opioids in complex samples","authors":"Mei-di Wang ,&nbsp;Yuan Zhang ,&nbsp;Ping-yuan Zhang ,&nbsp;Yun-yang Zhang ,&nbsp;Li Yu ,&nbsp;Xue-song Feng ,&nbsp;Xiao-dan Liu","doi":"10.1016/j.chroma.2026.466713","DOIUrl":"10.1016/j.chroma.2026.466713","url":null,"abstract":"<div><div>The growing global opioid crisis, evidenced by a 90% surge in overdose deaths between 2013 and 2017 and &gt;130 fatalities reported daily in the U.S., underscores the pressing need for advanced detection methods. Opioids, including natural alkaloids (e.g., morphine), semi-synthetic derivatives (e.g., oxycodone), and synthetic analogs (e.g., fentanyl), pose significant public health risks due to their rampant misuse. This review highlights cutting-edge microextraction technologies, specifically liquid-phase microextraction (LPME) and solid-phase microextraction (SPME), which aim to effectively address these limitations. Recent innovations in LPME include surfactant-assisted single-drop microextraction and hollow fiber LPME with amine-functionalized mesoporous foam. These techniques achieve high recovery rates while significantly minimizing solvent use. Furthermore, deep eutectic solvents and ionic liquids (e.g., [C₈MIM][PF₆]) have emerged as environmentally friendly alternatives, enhancing selectivity and enrichment factors. For SPME, advancements such as molecularly imprinted polymers and graphene oxide nanosheets offer exceptional specificity and reusability, with high recoveries. Novel materials, such as electrochemically co-deposited sol-gel/Cu nanocomposite fibers and magnetic materials, further enhance operational efficiency and reduce processing time. These developments enhance analytical precision and adhere to the principles of green chemistry, facilitating scalable and high-throughput detection of opioids in complex matrices. Future research should focus on integrating these technologies with portable analytical platforms for practical applications. Thin-film microextraction devices can be directly coupled with handheld mass spectrometers or miniaturized GC–MS systems. This integration enables rapid, on-site detection of opioids in forensic or clinical settings. Moreover, microextraction sorbents could be incorporated into paper-based lateral flow assay devices, allowing simple, cost-effective, and disposable field testing for opioid residues.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466713"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146008333","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}