Journal of Chromatography A最新文献

{"title":"Green and controlled synthesis of copper-based tryptophan flower-like chiral metal-organic framework for enantioselective recognition and volatile organic compound separation","authors":"Jinhua Xu ,&nbsp;Minghui Tang ,&nbsp;Jinyu Zhang ,&nbsp;Wenmin Zhang ,&nbsp;Shiye Xie ,&nbsp;Lan Zhang","doi":"10.1016/j.chroma.2025.466020","DOIUrl":"10.1016/j.chroma.2025.466020","url":null,"abstract":"<div><div>This study reports the synthesis and application of a flower-like chiral metal-organic framework (CMOF) based on copper ions and tryptophan (Cu(Trp)-CMOF). The Cu(Trp)-CMOF was successfully synthesized at room temperature through a facile method with hexadecyl trimethyl ammonium bromide (CTAB) as a structure-directing agent. The material exhibits a flower-like morphology with hierarchical porosity and well-defined crystallinity in the monoclinic P2₁/c space group. Comprehensive characterization revealed that different optical configurations ((<em>R</em>)-type, (<em>S</em>)-type, and (RS)-type) could be selectively obtained by controlling the chirality of tryptophan ligands. The synthesized CMOFs demonstrated excellent performance in two key applications: colorimetric recognition of amino acid enantiomers and separation of volatile organic compounds (VOCs). When used as a chromatographic stationary phase, the CMOF significantly enhanced the separation of challenging structural isomers, particularly improving the resolution (R_S) of xylene isomers (R_S from 1.03 to 2.62) and ethyltoluene isomers (R_S from 4.83 to 9.23) compared to conventional columns. This work provides new insights into the design and application of CMOFs for chiral separation and recognition.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 466020"},"PeriodicalIF":3.8,"publicationDate":"2025-05-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143917457","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":"Recent advances in molecular-imprinting-based solid-phase microextraction for determination of pharmaceutical residues","authors":"Jingyi Yan ,&nbsp;Jingying Huang ,&nbsp;Siyuan Peng ,&nbsp;Dani Sun ,&nbsp;Wenhui Lu ,&nbsp;Zhihua Song ,&nbsp;Jiping Ma ,&nbsp;Jinmao You ,&nbsp;Huaying Fan ,&nbsp;Lingxin Chen ,&nbsp;Jinhua Li","doi":"10.1016/j.chroma.2025.466016","DOIUrl":"10.1016/j.chroma.2025.466016","url":null,"abstract":"<div><div>Pharmaceutical residues usually exist in various complicated matrices at trace levels, but pose potential threats to human health and ecological environment. Recognition and determination of the residues are important and urgent. Therefore, efficient sample pretreatment techniques become a research hotspot for the sensitive and precise determination by chromatography and mass spectrometry. Molecular-imprinting-based solid-phase microextraction (MI-SPME) combines the rapidity, high enrichment and solvent-free property of SPME with the specific recognition and selective adsorption ability of molecularly imprinted polymers (MIPs), and shows significant advantages in the highly selective separation and enrichment of drug residues in complex samples. Herein, we review recent advances in MI-SPME for determination of pharmaceutical residues since 2019. Firstly, the basic characteristics and operation process of SPME are briefly introduced, and then the polymerization methods of MIPs including free radical polymerization, in-situ polymerization and sol-gel polymerization, and new imprinting technologies and strategies including surface imprinting, nano-imprinting, dummy template, multi-template/functional monomer imprinting and stimuli-responsive imprinting, are comprehensively overviewed. Then, various modes of MI-SPME device are meticulously discussed, mainly including MIPs-coated fiber SPME, MIPs-based in-tube SPME, dispersible SPME, MIPs in-tip SPME, MIPs stir bar sorptive extraction, and MIPs thin film microextraction. Subsequently, typical application cases of MI-SPME coupled with chromatography and mass spectrometry for the determination of drug residues are summarized, in the fields of food safety, biological medicine and environmental monitoring, specially mentioning chiral drug detection and matrix effects and interferences. Finally, the possible challenges of MI-SPME in drug residue detection are presented, and the research prospects and development trends of MI-SPME are proposed.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 466016"},"PeriodicalIF":3.8,"publicationDate":"2025-05-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143929631","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":"Analytical factors for optimization of chain-length distribution analysis of mRNA using capillary gel electrophoresis","authors":"Takenori Yamamoto,&nbsp;Tokuyuki Yoshida,&nbsp;Yasunori Uchida,&nbsp;Nobumichi Ohoka,&nbsp;Takuma Yamashita,&nbsp;Eriko Uchida,&nbsp;Takao Inoue","doi":"10.1016/j.chroma.2025.466019","DOIUrl":"10.1016/j.chroma.2025.466019","url":null,"abstract":"<div><div>The development of mRNA vaccines against coronavirus disease-2019 has garnered attention in utilizing mRNA-based modalities such as mRNA vaccines and therapeutics. mRNA length is a crucial factor in the quality assessment of mRNA-based modalities, confirming the integrity of mRNA as an active component. Capillary gel electrophoresis is a representative analytical method used to examine mRNA chain length and should sufficiently separate full-length mRNAs and impurity RNAs (shortmers and longmers) to accurately evaluate mRNA quality. However, the analytical parameters affecting the separation of mRNAs have not been adequately verified. This study comprehensively analyzed the analytical parameters of capillary gel electrophoresis, and found that the gel concentration, denaturant, preheating treatment, capillary temperature, and fluorescent dye remarkably affect the separation of long-chain-length RNAs. The separation limits of capillary gel electrophoresis analysis were examined under adjusted analytical parameter conditions. Consequently, RNAs of approximately 4,000 nucleotides length and their defective RNAs of ≥200 nucleotides could be effectively separated. Furthermore, when RNA separation under our adjusted conditions was compared with that under the conditions recommended in the United States Pharmacopeia (USP) draft guidelines, our method demonstrated higher RNA separation for both RNA prepared in this study and that of the approved mRNA vaccine.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 466019"},"PeriodicalIF":3.8,"publicationDate":"2025-05-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143942904","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":"Prediction of HPLC chromatograms under linear and curved gradient elution by linear gradient trials with initial hold time","authors":"Weiqiang Hao ,&nbsp;Jie Tang ,&nbsp;Yuying Deng ,&nbsp;Lei Jiang ,&nbsp;Qiong He ,&nbsp;Jin Xu ,&nbsp;Yibo Huang ,&nbsp;Bo Li ,&nbsp;Xiuxiu Qi","doi":"10.1016/j.chroma.2025.466018","DOIUrl":"10.1016/j.chroma.2025.466018","url":null,"abstract":"<div><div>It is demonstrated that initial hold time (<em>t_I</em>) before gradient elution may be taken as an extension of dwell time (<em>t_D</em>) of the chromatograph. On the basis of this property, we deduce the expressions for retention time (<em>t_R</em>) and band compression factor (<em>G_Z</em>) under linear gradient with <em>t_I</em> which is also called scouting gradient in this work. In the case of linear solvent strength model (LSSM) and when the analyte is eluted from the column after the end of linear gradient, an algebraic expression for <em>G_Z</em> is deduced. A nonlinear fit based on the Levenberg-Marquardt algorithm was applied to the experimental data of <em>t_R</em> acquired from six scouting gradient runs to obtain the retention parameters in LSSM as well as quadratic solvent strength model (QSSM). The plate number of the column was also calculated from the gradient elution experimental results. With the retention parameters and plate number obtained, the chromatograms under linear and curved gradient elution were predicted in the case of chiral and reversed-phase HPLC separation. The experimental and predicted chromatograms are consistent, and QSSM is generally better than LSSM for the prediction, especially in the case of chiral separation.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 466018"},"PeriodicalIF":3.8,"publicationDate":"2025-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143906248","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":"Separation of Fab therapeutic charge variants by ion-exchange chromatography using iterative mathematical and artificial neutral network modeling approaches","authors":"Anupa Anupa ,&nbsp;Pratik Punj ,&nbsp;Lalita Kanwar Shekhawat ,&nbsp;Anurag Rathore","doi":"10.1016/j.chroma.2025.466015","DOIUrl":"10.1016/j.chroma.2025.466015","url":null,"abstract":"<div><div>Linear pH, salt, or dual pH-salt gradient elution is the most common ion-exchange chromatography method for monoclonal and Fab antibody purification, but maintaining precise gradients during biomanufacturing is challenging. In the present study, using chromatographic data of linear salt gradient elution of Fab therapeutic performed at different conditions of pH and linear gradient lengths, a step gradient elution has been developed using iterative mathematical and artificial neutral networks modeling approaches. The proposed approaches utilizes classical Yamamoto method and Mollerup’s thermodynamic approach offering satisfactory prediction of distribution coefficient of protein species (main Fab and two A1 and A2 acidic variants) as a function of salt concentration based on the stoichiometric displacement model for different fixed pH conditions. The standard deviation (<span><math><mi>σ</mi></math></span>) between mathematical and neural network approach was compared for the model optimized thermodynamic parameters and binding charge. The deviation was found to vary from small {± (0-0.3)} <span><math><mi>σ</mi></math></span>, to moderate {± (0.4-0.6)} <span><math><mi>σ</mi></math></span> range for main Fab and acidic (A1 and A2) variants. The optimized conditions of pH and salt concentration were successfully identified from the model predicted distribution coefficient curves and were utilized to design a three-step salt gradient elution at a fixed pH chromatography process without further optimization, giving final purified Fab with a purity of 92% and yield of 76%. The presented approach for conversion of linear gradient to step gradient can be highly useful for developing a robust and simplified commercial scale chromatography purification process for complex biomolecules.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 466015"},"PeriodicalIF":3.8,"publicationDate":"2025-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143929183","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":"Logical criteria for estimating gas chromatographic retention indices of organic compounds using their physicochemical properties","authors":"Igor G. Zenkevich","doi":"10.1016/j.chroma.2025.465983","DOIUrl":"10.1016/j.chroma.2025.465983","url":null,"abstract":"<div><div>There is no unified equation that would correlate gas chromatographic retention indices of any organic compounds with their normal boiling points (at atmospheric pressure). Nevertheless, RI estimation with acceptable accuracy is possible using principal physicochemical properties, namely, boiling points, relative densities, and indices of refraction. The main feature of the algorithms proposed is the application of a logical criteria for comparing so-called indices of boiling points I(<em>T</em>_b), molecular weights I(<em>M</em>), and molar refractions I(MR_D). If the comparison of these indices confirms the approximate equality of any two or all three of them (that is typical for nonpolar organic compounds), then as the best estimate of GC retention indices (RI_calc) we can accept I(<em>T</em>_b) values without any additional calculations. Such comparison is formally equivalent to the application of logical criteria for I(<em>T</em>_b), I(<em>M</em>), and I(MR_D) values. For polar analytes, the relation I(<em>T</em>_b) &gt; <em>I</em>(MR_D) &gt; <em>I</em>(<em>M</em>) is valid, and in these cases the inequality I(<em>T</em>_b) &gt; RI_calc &gt; <em>I</em>(<em>M</em>) appeared to be correct. Instead of large intervals between <em>I</em>(<em>T</em>_b) and <em>I</em>(<em>M</em>) for estimating RI_calc, the use of the relation RI_calc ≈ (1 – <em>a</em>)I(<em>T</em>_b) + <em>a</em>I(MR_D) + <em>b</em> is proposed. The indices of molecular weights are not used for the calculations directly, but they are needed just for application of the logical criteria.</div><div>The average accuracy of RI estimation by the method proposed is 9–16 index units for nonpolar compounds of any chemical nature and up to 27 for polar analytes. This high accuracy is comparable to that of the more sophisticated modern algorithms. The restriction of this approach is the impossibility of applying it to poly- and perfluoroorganic compounds.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 465983"},"PeriodicalIF":3.8,"publicationDate":"2025-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143936827","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":"Fast and accurate discrimination analysis of Angelicae Pubescentis Radix using non-targeted analytical profiles images and two-dimensional convolution neural network","authors":"Yue Huang,&nbsp;Li Jun Tang,&nbsp;Zhuo Ling Yang,&nbsp;Xiang-Zhi Zhang,&nbsp;Bao Qiong Li","doi":"10.1016/j.chroma.2025.466014","DOIUrl":"10.1016/j.chroma.2025.466014","url":null,"abstract":"<div><div>This study developed an effective approach for discriminating geographical origins of Duhuo samples using non-targeted UPLC chromatograms and UV-Vis spectrogram images combined with a two-dimensional convolution neural network (2D-CNN). For comparison, four machine learning methods-extreme gradient boosting (XGBoost), random forest (RF), partial least squares discriminant analysis (PLS-DA), and support vector machine (SVM) were applied to analyze UPLC, UV-Vis data matrix, and concentrations of seven target compounds. Enhanced by data augmentation, 2D-CNN demonstrated superior accuracy, with 98.28% accuracy for UV-Vis images and 100% for UPLC images, while traditional machine learning models showed considerable variation across datasets. These results demonstrate the integration of 2D-CNN with UPLC and UV-Vis images enable robustness, accurate and non-destructive analysis for the efficient discrimination of TCM samples. Specifically, UV-Vis spectroscopy provides a convenient method for quick detection. Overall, the employed approach offers a powerful tool for the precise and reliable analysis of herbal medicines.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 466014"},"PeriodicalIF":3.8,"publicationDate":"2025-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143917324","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 liquid chromatography/ultraviolet and evaporating light scattering detector platform for simultaneous quantification of ginsenosides","authors":"Inho Jung ,&nbsp;Yujin Lee ,&nbsp;Tae-Jin Yang ,&nbsp;Kyoung Heon Kim ,&nbsp;Jungyeon Kim","doi":"10.1016/j.chroma.2025.466010","DOIUrl":"10.1016/j.chroma.2025.466010","url":null,"abstract":"<div><div>Ginsenosides, the primary bioactive components in ginseng, offer various health benefits, including anti-inflammatory, anti-osteoporosis, and neuroprotective effects. For consistent product quality and better understanding of these effects, accurate quantification of ginsenosides is essential. Although liquid chromatography–mass spectrometry (LC/MS) can identify up to 200 ginsenosides, it is costly, complex, and requires specialized personnel. In contrast, liquid chromatography coupled with ultraviolet (UV) or evaporative light scattering detectors (ELSD) is more accessible but typically limited to quantifying no more than 24 ginsenosides. In this study, we developed an LC/UV-ELSD platform that enables the simultaneous quantification of 41 ginsenosides in a single run—38 quantified by UV and 3 by ELSD. The platform demonstrated excellent reproducibility (RSD: 0.341–2.653 %) and sensitivity, with detection limits as low as 0.073 µg/mL for UV and 5–10 µg/mL for ELSD. Application to ginseng samples showed total ginsenoside concentrations of 39.54 ± 10.72 mg/g in field-cultivated roots, 103.68 ± 14.41 mg/g in wild-simulated leaves, and 37.02 ± 5.52 mg/g in wild-simulated roots. Quantification results closely matched those from LC/MS analysis, with a difference of less than 10 %. Our LC/UV-ELSD platform offers a simple, cost-effective, and reliable solution for comprehensive ginsenoside analysis and is well suited for both research and industry use in quality control and functional evaluation of ginseng products.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 466010"},"PeriodicalIF":3.8,"publicationDate":"2025-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143901938","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":"Prediction of infinite dilution activity coefficients for compounds in water at 298.15 K using reversed-phase liquid chromatography","authors":"Sanka N. Atapattu","doi":"10.1016/j.chroma.2025.466008","DOIUrl":"10.1016/j.chroma.2025.466008","url":null,"abstract":"<div><div>Infinite dilution activity coefficients (γ∞) in water are valuable for various industrial applications. However, the experimental methods used to determine these coefficients can be tedious and labour-intensive, often requiring specialized expertise and training in specific techniques. As a result, predictive models are generally favoured over experimental methods for estimating infinite dilution activity coefficients in water. These predictive models rely on molecular descriptors to estimate the values of the coefficients. In this work the correlation of reversed-phase liquid chromatography retention factors to estimate infinite dilution activity coefficients in water was explored. Of the screened isocratic reversed-phase liquid chromatography systems the XTerra Phenyl stationary phase with a binary solvent composition of 70 % methanol (v/v) is the best retention factor correlation model with a prediction standard error of 0.226, and Fisher statistic of 1020.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 466008"},"PeriodicalIF":3.8,"publicationDate":"2025-04-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143917326","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":"Rapid screening of illicit drugs in wastewater based on-site automated solid phase extraction and portable mass spectrometry techniques","authors":"Liangming Luo ,&nbsp;Chenlu Wang ,&nbsp;Yong Wu ,&nbsp;Hao Zhang ,&nbsp;Feng Xu ,&nbsp;Keqi Tang ,&nbsp;Jiancheng Yu","doi":"10.1016/j.chroma.2025.466011","DOIUrl":"10.1016/j.chroma.2025.466011","url":null,"abstract":"<div><div>Screening for illicit drugs in urban wastewater provides an important tool for monitoring and tracing the use of illicit drugs, increasingly leaning towards on-site detection of wastewater samples. This study established an on-site detection method for three illicit drugs—ketamine (KET), cocaine (COC), and codeine(COD)—in wastewater, based on an automatic solid-phase extraction device and a portable mass spectrometer. After enrichment and purification of samples using HLB solid-phase extraction cartridges, a portable mass spectrometer equipped with a sub-atmospheric pressure chemical ionization source was used for quantitative analysis of target drugs in selected ion monitoring mode. The solid-phase extraction conditions and parameters of the subatmospheric pressure chemical ionization source were studied and optimized, and the method was evaluated. The results showed that ketamine, cocaine, and codeine exhibited good linearity (R² &gt; 0.99) within the concentration range of 1∼40 μg/L, with limits of detection (LODs) of 0.30∼0.42 μg/L. The recoveries were between 70.52 % and 118.56 %. This method can be used for on-site rapid screening of illicit drugs in wastewater. Compared to traditional laboratory analysis methods, it reduces sample transportation and storage costs, shortens the detection cycle. Finally, evaluations based on GAPI, AGREE, and BAGI indicators indicated that this method could serve as a green alternative for the screening of illicit drugs in wastewater.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 466011"},"PeriodicalIF":3.8,"publicationDate":"2025-04-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143910966","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}