Journal of Chromatography A最新文献

{"title":"Accurate quantification of quinolones in marine sediment by UPLC-MS/MS after ultrasonic extraction and automated SPE clean-up","authors":"Zhenhua Li ,&nbsp;Qiaoling Zhao ,&nbsp;Haoji Zhao ,&nbsp;Tiejun Li ,&nbsp;Hongmei Hu ,&nbsp;Yuanming Guo ,&nbsp;Heyong Cheng","doi":"10.1016/j.chroma.2026.466752","DOIUrl":"10.1016/j.chroma.2026.466752","url":null,"abstract":"<div><div>As a class of the most prevalent broad-spectrum antibiotics, quinolones (QNs) are ubiquitous in various environmental matrices (in particular marine sediment). However, determination of multiple QNs in marine sediment is a challengeable task due to matrix complexity and strong QNs-sediment adsorption. Herein we presented an efficient quantification strategy for accurate measurement of 15 QNs in marine sediment based on ultrasonic extraction with 0.2 M Na₂HPO₄ in 50 v/v % acetonitrile, followed by automated solid-phase clean-up and ultra-performance liquid chromatography−tandem mass spectrometry with isotope dilution calibration. The method demonstrated negligible matrix effect, satisfactory recoveries (85 %–119 %), and low limits of detection (2–15 pg/g). Five QNs were detected in marine sediment from Yueqing Bay and Daiquyang with total concentrations of 5.6–12.1 μg/kg and 0.2–1.0 μg/kg, respectively, where four QNs including norfloxacin (NOR), enrofloxacin, ciprofloxacin, and ofloxacin were found in all samples, and NOR was the predominant compound both in Yueqing Bay and Daiquyang. Overall, the presented method is highly sensitive and reliable for routine quinolone analysis in marine sediment.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466752"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146099778","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":"Efficient solid-phase extraction of quaternary ammonium alkaloids from traditional Chinese medicines on a novel sulfonic acid group functionalized microporous organic network coated SiO2 composite","authors":"Wen-Jing Zhao,&nbsp;Xin-Yue Wang,&nbsp;Jin-Shuang Wang,&nbsp;Yuan-Yuan Cui,&nbsp;Cheng-Xiong Yang","doi":"10.1016/j.chroma.2026.466756","DOIUrl":"10.1016/j.chroma.2026.466756","url":null,"abstract":"<div><div>In this work, a novel sulfonic acid-functionalized microporous organic network-coated SiO₂ composite (SiO₂@MON-SO₃H-2) was synthesized for efficient solid-phase extraction (SPE) of quaternary ammonium alkaloids (QAAs) from complex traditional Chinese medicine (TCM) samples. The material exhibits a high specific surface area (381.4 m² g⁻¹), superhydrophilicity, and excellent stability. These properties, combined with synergistic interactions such as electrostatic attraction, hydrophobic effects, and π-π stacking, enabled the adsorbent to demonstrate outstanding extraction performance toward four typical QAAs. The developed method owns wide linear ranges (0.88–1000 μg L⁻¹) with good linearity (R² &gt; 0.999), high sensitivity (limits of detection: 0.26–1.02 μg L⁻¹), satisfactory precision (intra- and inter-day RSDs &lt; 6.3%), high enhancement factors (&gt; 91), and insignificant matrix effects (86.6–115.3%). The material maintained excellent reusability, with recoveries remaining above 89% after 50 extraction-desorption cycles. When applied to spiked herbal matrices, the method provided recoveries of 92.7–112.0%. SiO₂@MON-SO₃H-2 also gave higher recovery than commercial C18, activated carbon, macroporous adsorption resin AB-8, and the cation-exchange resin Amberlite 732. The present work demonstrates the prospect of SiO₂@MON-SO₃H-2 for trace QAAs extraction from complex samples and provides a reliable approach for TCM analysis and quality control.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466756"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146099735","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":"Multiresidual analysis of pesticides in white table grapes using hyphenated chromatographic techniques: Compliance and risk assessment","authors":"Giorgia Rinaldi ,&nbsp;Danilo Donnarumma ,&nbsp;Antonio Ferracane ,&nbsp;Romana Rigger ,&nbsp;Markus Obkircher ,&nbsp;Mariosimone Zoccali ,&nbsp;Luigi Mondello","doi":"10.1016/j.chroma.2026.466799","DOIUrl":"10.1016/j.chroma.2026.466799","url":null,"abstract":"<div><div>Grapes are widely cultivated and consumed, requiring pesticide control to ensure consumer safety. Herein we report a simplified workflow for detecting 236 pesticides in white table grapes within the EU multi-annual control programme, along with chronic, acute and cumulative risk assessments. The method involved two complementary analytical platforms: low-pressure gas chromatography (LP-GC) for volatile/semi-volatile pesticides and ultra-high-performance liquid chromatography (UHPLC) for polar/thermally labile pesticides, both coupled to triple quadrupole mass spectrometry (QqQMS). The methods were validated in terms of linearity (correlation coefficients ≥0.998 for all analytes), extraction recovery (mean recoveries of 70–120 % for &gt;90 % of pesticides), precision (intra- and inter-day relative standard deviations ≤20 % for all validated concentrations), trueness (in the range 63–135 %), and limit of quantification (ranging from 0.002 to 0.01 mg Kg^-1 for LP-GC-QqQMS and from 0.002 to 0.05 mg Kg^-1 for UHPLC-QqQMS). Analysis of 20 samples detected 23 pesticides, five of which exceeded MRLs. Risk assessment showed that parathion-methyl poses unacceptable chronic and acute risks (exceedance up to 234 % and 193 % respectively), especially for children under &lt;10 years old and toddlers due to their high consumption and low body weight. This highlights the need for stricter monitoring and regulatory measures to minimize pesticide exposure to widely consumed fruits.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466799"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146218177","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":"Silver-decorated boron carbon nitride nanocomposite for ultra-fast dispersive micro-solid-phase extraction and preconcentration of mercury (II) in environmental waters","authors":"Sedigheh Makaremnia ,&nbsp;Kamal Ghanemi","doi":"10.1016/j.chroma.2026.466795","DOIUrl":"10.1016/j.chroma.2026.466795","url":null,"abstract":"<div><div>This study presents a silver-decorated boron-carbon-nitride (Ag@BCN) nanocomposite for ultra-rapid dispersive micro-solid-phase extraction (d-µ-SPE) of Hg(II) in diverse water samples, followed by detection using cold-vapor atomic absorption spectrometry (CVAAS). The material integrates the high surface area of a mesoporous BCN support with the high selectivity of Ag nanoparticles (60–75 nm) for Hg(II) through spontaneous amalgamation, addressing the kinetic and environmental limitations of traditional organic chelating agents. The developed D-µ-SPE method reached quantitative extraction equilibrium in just one minute, offering a substantial improvement over most existing D-µ-SPE techniques. The developed method demonstrated excellent analytical performance, with a low LOD (0.067 ng/mL), a high adsorption capacity (54.5 mg/g), and good precision (RSD &lt; 4.6 %) under optimal conditions (pH 4.0, 70 mg of adsorbent). Additionally, the Ag@BCN adsorbent showed recoveries from 94.8 % to 100.0 % even in complex matrices of up to 5 % NaCl, demonstrating its stability in high-ionic-strength matrices like seawater and river water. By combining ultrafast kinetics monitoring, high sensitivity, and a user-friendly interface in a D-µ-SPE format, this work presents an efficient alternative to traditional methods for routine screening and monitoring of mercury in environmental waters.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466795"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146225140","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":"Transmembrane proteome analysis of frozen mouse lung tissues by LC-MS using metal organic framework-based protein extraction","authors":"Li Zhu ,&nbsp;Miao Guo ,&nbsp;Yingjia Liu ,&nbsp;Lu Zhang ,&nbsp;Suntao Li ,&nbsp;Jiaqi Zhao ,&nbsp;Jianzheng Zhu ,&nbsp;Meihui Sang ,&nbsp;Liqiang Qian ,&nbsp;Yan Zhang ,&nbsp;Hua Xiao","doi":"10.1016/j.chroma.2026.466733","DOIUrl":"10.1016/j.chroma.2026.466733","url":null,"abstract":"<div><div>Membrane proteins (MPs) play crucial roles in cellular functions and are key targets for drug discovery and cancer research. However, due to their poor solubility, high hydrophobicity, and low abundance, MPs present significant analytical challenges, particularly with regard to their dissolution, isolation, and characterization. Efficiently extracting MPs from frozen tissue samples remains challenging, which limits our ability to study their functions in pathological processes. In this study, we developed a metal-organic frameworks (MOFs)-assisted bio-separation strategy using Zeolitic Imidazolate Framework-67 (ZIF-67) for efficient membrane proteome isolation from frozen mouse lung tissue. We optimized key parameters for MPs extraction, including protein extraction approaches (tissue grinding versus enzymolysis), material-to-protein ratio, and SDS concentration. Our results demonstrated that ZIF-67 strategy with enzymolysis dramatically improved the enrichment efficiency of MPs with multi-transmembrane domains (TMs≥2) than the commercial kit method. In particular, among the 500 most abundant MPs isolated by the optimized ZIF-67 strategy, 133 were MPs with TMs≥2, which was 2.18 times that of the kit method. We further applied this strategy to analyze two distinct types of clinical lung cancer tissue samples (ground glass opacity nodules and solid nodules). Quantitative proteomics analysis revealed distinct membrane protein profiles and dysregulated pathways in the two lung cancer nodules. The enhanced capability of the ZIF-67 strategy for analyzing multi-transmembrane proteome provided valuable biological information for investigating the underlying molecular mechanisms underlying distinct nodule types. The strategy’s compatibility with frozen tissues underscores its broad applicability in translational and biomedical studies, paving the way for in-depth exploration of MPs in disease mechanisms and therapeutic development.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466733"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146071101","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":"Tribute for Professor Peter W. Carr","authors":"Dwight Stoll ,&nbsp;Mark Vitha","doi":"10.1016/j.chroma.2026.466779","DOIUrl":"10.1016/j.chroma.2026.466779","url":null,"abstract":"","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466779"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147385901","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":"Mobile-phase selection for isomer selectivity in reversed-phase liquid chromatography: Evaluation of conventional and green, binary and ternary mobile phases for the separation of carvacrol and thymol","authors":"Robin Simon Beers,&nbsp;Alexandra Höltzel,&nbsp;Ulrich Tallarek","doi":"10.1016/j.chroma.2026.466808","DOIUrl":"10.1016/j.chroma.2026.466808","url":null,"abstract":"<div><div>To map out the mobile-phase parameter space for the separation of the positional isomers carvacrol and thymol, naturally occurring monoterpenoid phenols of astonishingly wide biological activity, by reversed-phase liquid chromatography, we tested conventional and green candidates for the organic solvent (OS) in the mobile phase. Binary and ternary compositions were evaluated at different solvent ratios regarding resolution, selectivity, and analysis time of the isomer separation on a C₁₈ column. Baseline separation with binary compositions was obtained with ethanol (EtOH), acetonitrile (ACN), or tetrahydrofuran (THF) as OS, but not with water‒methanol (W‒MeOH) mobile phases. The sensitivity of the isomer selectivity to the OS volume fraction in the mobile phase strongly depended on the OS candidate, yielding a narrower or wider range of OS volume fractions over which the isomer separation succeeded. Among the binary compositions, W‒ACN mobile phases performed best, but W‒EtOH mobile phases were an acceptable green alternative. The addition of THF or MeOH as third solvent to W‒ACN mobiles phase offered little or no selectivity enhancement, whereas the addition of THF or ethyl acetate (EtOAc) to W‒MeOH or W‒EtOH mobile phases, respectively, delivered large selectivity improvements compared to all other binary and ternary compositions. The quantification of carvacrol and thymol in oregano leaf extract using a W‒EtOH‒EtOAc mobile phase proved that green methods can easily replace conventional ones in this application. Regarding the physicochemical properties of the OS candidates, the study showed that the absence of hydrogen-bond donor properties favored, but did not create, the isomer selectivity with binary mobile phases, and that ternary mobile phases combining two OS candidates with large differences in molecular volume, solute polarity, and hydrogen-bond capability achieved the best results overall.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466808"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146225192","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 single column multimodal cation exchange process for removal of half antibody, homodimer and light chain mispaired product-related impurities from a bispecific antibody","authors":"Cameron DiSpirito ,&nbsp;Siddharth Parasnavis ,&nbsp;Matthew Aspelund ,&nbsp;Steven M Cramer","doi":"10.1016/j.chroma.2026.466745","DOIUrl":"10.1016/j.chroma.2026.466745","url":null,"abstract":"<div><div>During synthesis of IgG-like bispecific antibodies (bsAbs), product-related impurity formation via the mispairing of heavy chains and light chains (LCs) is common despite protein engineering efforts to mitigate these species. These mispaired impurities have similar biophysical characteristics to the target bsAb and are often difficult to remove with conventional platform processes. In this paper we demonstrate the utility of Capto MMC ImpRes for removing ½ IgG, homodimer and LC-mispair product-related impurities from an asymmetric IgG-like bsAb. Screening experiments from pH 5.0 to 9.5 showed that the ½ IgG and homodimer impurities eluted at pH 9.5, while the LC-mispair could be removed from the bsAb at pH 5.5 using a linear salt gradient. These results were then employed as a guide to propose a single column, multi-pH step gradient process for the removal of all product-related impurities. The final process included loading at pH 7.5 followed by elution of the homodimer and ½ IgG impurities from the column with a pH 9.5 wash. The column pH was then reduced to 5.5 and the LC-mispair impurity was subsequently removed during a 1 M NaCl step. Finally, a pH 8.0 with 1 M NaCl eluent was employed to recover the bound bsAb. This one step MMCEX polishing process resulted in an increased purity of the bsAb from 67.3% to 94.5% with a 72% overall recovery of the bsAb. These results demonstrate the utility of single column multimodal chromatographic processes when operated at multiple pHs for the removal of challenging product-related impurities from bsAbs.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466745"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146099749","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":"New equations of column performance in liquid chromatography","authors":"Leonid M. Blumberg","doi":"10.1016/j.chroma.2026.466754","DOIUrl":"10.1016/j.chroma.2026.466754","url":null,"abstract":"<div><div>New equation expressing the optimal efficiency and optimal dimensionless solvent velocity of LC column of an arbitrary structure are derived. The use of the equations for evaluating and comparing performance of several differently structured columns has been illustrated.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466754"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146111789","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 efficient boronate affinity solid-phase extraction strategy for ginsenosides enrichment based on dendritic mesoporous silica","authors":"Weiman Zhao,&nbsp;Longchan Liu,&nbsp;Wenxiang Fan,&nbsp;Ziwei Li,&nbsp;Haizhen Zhang,&nbsp;Linnan Li,&nbsp;Zhengtao Wang,&nbsp;Li Yang","doi":"10.1016/j.chroma.2026.466737","DOIUrl":"10.1016/j.chroma.2026.466737","url":null,"abstract":"<div><div>Ginsenosides are a class of natural glycosidic compounds characterized by structural diversity and significant bioactivities, mainly derived from <em>Panax</em> genus plants. However, there are still challenges in achieving efficient and green separation of ginsenosides from complex plant matrices. Traditional methods often suffer from high consumption of organic solvents, poor selectivity, and complex purification processes. In this study, a boronic acid-functionalized dendritic mesoporous silica nanomaterial was constructed based on the reversible covalent interaction between boronic acid ligands and the cis-diol motifs in ginsenosides. It was used as the solid phase extraction adsorbent for the separation and purification of ginsenosides. Taking the decoction of <em>Panax notoginseng</em> stems and leaves as an example, the adsorption performance and impurity removal efficiency of this strategy were systematically evaluated. The key extraction parameters were optimized by single-factor experiments and Box-Behnken response surface methodology. Quantitative analysis of nine major ginsenosides using HPLC-CAD demonstrated that the developed strategy outperformed traditional macroporous resin, achieving enrichment fold of 3.4-4.0, which were nearly 2.0 times higher than those of the resin, along with adsorption recoveries of 93.5-98.7% and desorption recoveries of 88.9–97.9%. The extracted sample was further analyzed by UPLC-Q-TOF-MS. 127 ginsenosides were successfully identified, and the interference signals of non-ginsenosides were markedly reduced. The greenness evaluation by Analytical GREEnness metric and Green Analytical Procedure Index indicated that the boron affinity strategy had significant advantages in terms of environmental friendliness and process sustainability. The solid phase extraction technique based on boron-affinity materials provides a promising approach for the efficient, large-scale and green preparation of ginsenosides and other cis-diol natural products.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1770 ","pages":"Article 466737"},"PeriodicalIF":4.0,"publicationDate":"2026-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146083672","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}