Journal of Chromatography A最新文献

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Construction of carboxyl-functionalized hyper-cross-linked porous polymers using waste polystyrene for effective adsorption of phenolic contaminants
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-03-31 DOI: 10.1016/j.chroma.2025.465925
Chenhuan Wang , Qianqian Wang , Kaiyuan Si
{"title":"Construction of carboxyl-functionalized hyper-cross-linked porous polymers using waste polystyrene for effective adsorption of phenolic contaminants","authors":"Chenhuan Wang ,&nbsp;Qianqian Wang ,&nbsp;Kaiyuan Si","doi":"10.1016/j.chroma.2025.465925","DOIUrl":"10.1016/j.chroma.2025.465925","url":null,"abstract":"<div><div>The extensive presence of phenolic organic contaminants (POCs) poses a serious threat to humans. Meanwhile, the upcycling/reusing of waste polystyrene to reduce the exponential growth of plastic pollution is a very important environmental issue. Addressing these demands, a series of carboxyl-functional hypercrosslinked polymers (labeled PP-HCPs) were constructed by knitting waste polystyrene with pyromellitic dianhydride at different ratios through a one-step Friedel-Crafts reaction for effective adsorption of POCs. Among the prepared PP-HCPs, PP-HCP2 displayed a large specific surface area with high adsorption capacity (37.3 mg g<sup>−1</sup>) for POCs. Using PP-HCP2 as solid phase extraction sorbent, six POCs were effectively extracted from water and peach drink samples, then subjected to high-performance liquid chromatography-ultraviolet detection. The method demonstrated good linearity in the range of 0.03–100.0 ng mL<sup>−1</sup> for water samples and 0.06–100.0 ng mL<sup>−1</sup> for peach drinks under optimum experimental conditions. At a signal-to-noise ratio of 3, low detection limits were found to be 0.01–0.10 ng mL<sup>−1</sup> for water samples and 0.02–0.15 ng mL<sup>−1</sup> for peach drinks. Good accuracy and repeatability were achieved with recoveries of 85.3–111.8 % and the relative standard deviations below 8.6 %. The PP-HCP2-based approach can be employed as a dependable and sensitive tool to detect POCs in water and peach drink samples. This work delivers a simple and economically viable approach to fabricate carboxyl-functional HCPs by converting waste foam into high-value-added sorbent, with great significance for sustainable development.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465925"},"PeriodicalIF":3.8,"publicationDate":"2025-03-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143759218","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}
引用次数: 0
A dual-polarity ion mobility spectrometer for capturing hyper-fast chromatographic peaks
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-03-29 DOI: 10.1016/j.chroma.2025.465923
Alexander Nitschke, Moritz Hitzemann, Jonas Winkelholz, Ansgar T. Kirk, Christoph Schaefer, Tim Kobelt, Christian Thoben, Martin Lippmann, Jan A. Wittwer, Stefan Zimmermann
{"title":"A dual-polarity ion mobility spectrometer for capturing hyper-fast chromatographic peaks","authors":"Alexander Nitschke,&nbsp;Moritz Hitzemann,&nbsp;Jonas Winkelholz,&nbsp;Ansgar T. Kirk,&nbsp;Christoph Schaefer,&nbsp;Tim Kobelt,&nbsp;Christian Thoben,&nbsp;Martin Lippmann,&nbsp;Jan A. Wittwer,&nbsp;Stefan Zimmermann","doi":"10.1016/j.chroma.2025.465923","DOIUrl":"10.1016/j.chroma.2025.465923","url":null,"abstract":"<div><div>For higher analytical performance, ion mobility spectrometers (IMS), especially when analyzing complex mixtures, are often coupled with gas chromatographs (GC). However, analysis time remains a critical parameter in gas chromatography. Therefore, a hyper-fast GC is a promising approach for GC-IMS to combine highest sensitivity of IMS with increased peak capacity while allowing for rapid analysis within the double-digit second range. For simultaneously recording of both ion polarities, a new dual drift tube IMS in axial configuration has been developed that is particularly designed for resolving even hyper-fast GC peaks. Key is a directed sample gas flow through the ionization region giving a small effective detector volume. To avoid condensation of the sample gas, the IMS is isothermally heated to 120 °C. A drift tube length of only <em>L<sub>D</sub></em> = 41 mm with a drift voltage of <em>U<sub>D</sub></em> = 2.7 kV leads to an IMS repetition rate of 100 Hz and high resolving power of <em>R<sub>p</sub></em> = 60, even for ions with low reduced ion mobility down to 0.43 cm<sup>2</sup>V<sup>-1</sup>s<sup>-1</sup>. This setup can resolve very short GC peaks with full width at half maximum of only 140 ms. For demonstration, two different hop varieties and a mixture of explosives were analyzed within a short time of just 20 s.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465923"},"PeriodicalIF":3.8,"publicationDate":"2025-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143759298","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Potential of green solvents as mobile phases in liquid chromatography
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-03-29 DOI: 10.1016/j.chroma.2025.465810
Karen Gaudin
{"title":"Potential of green solvents as mobile phases in liquid chromatography","authors":"Karen Gaudin","doi":"10.1016/j.chroma.2025.465810","DOIUrl":"10.1016/j.chroma.2025.465810","url":null,"abstract":"<div><div>This review summarizes the key points and focuses on the use of green solvents in reversed-phase high-performance liquid chromatography. Ethanol, acetone, ethyl lactate, propylene carbonate, dimethyl carbonate, methyl acetate, Cyrene, and glycerol are examined as green solvents, with an emphasis on their properties related to HPLC applications. A total of 135 articles published between 1990 and the present, which utilize ethanol-water mobile phases in RP-HPLC, highlight the established use of ethanol as a green solvent for RP-HPLC. Although ethanol is often characterized by its high viscosity and UV absorbance, it remains one of the most commonly used green solvents. This study shows that approximately 30 % of the ethanol-based methods developed employed columns with reduced particle diameters, without the need for column heating. In 26 % of cases, UV detection was used, even at wavelengths egal to or below 220 nm. However, ethanol's volatility and flammability pose risks of operator exposure and fire hazards. Consequently, alternative solvents have been explored to mitigate these issues.</div><div>Acetone, with over 20 years of use, presents similar safety concerns, compounded by its high UV absorbance. Recent advances in greener solvents, such as Cyrene, glycerol, and natural deep eutectic solvents, have been investigated to address VOC concerns in HPLC. However, these solvents still face challenges, including UV absorption, immiscibility with water, high viscosity, and limited availability in HPLC-grade quality. Therefore, additional research is needed to facilitate their broader application.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465810"},"PeriodicalIF":3.8,"publicationDate":"2025-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143747595","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}
引用次数: 0
Green analytical approaches for contaminants: Sustainable alternatives to conventional chromatographic methods 污染物的绿色分析方法:传统色谱法的可持续替代方法
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-03-28 DOI: 10.1016/j.chroma.2025.465921
Víctor Cutillas, Carmen Ferrer, María Jesús Martínez-Bueno, Amadeo R. Fernández-Alba
{"title":"Green analytical approaches for contaminants: Sustainable alternatives to conventional chromatographic methods","authors":"Víctor Cutillas,&nbsp;Carmen Ferrer,&nbsp;María Jesús Martínez-Bueno,&nbsp;Amadeo R. Fernández-Alba","doi":"10.1016/j.chroma.2025.465921","DOIUrl":"10.1016/j.chroma.2025.465921","url":null,"abstract":"<div><div>The growing importance of environmental sustainability has driven advancements in analytical chemistry, particularly in the development of green chromatographic techniques. This review explores various chromatographic methods that align with green chemistry principles, offering environmentally friendly alternatives to traditional gold-standard approaches. Techniques such as supercritical fluid chromatography (SFC), miniaturized liquid chromatography (LC), and gas chromatography (GC) with alternative carrier gases (e.g., hydrogen and nitrogen) are discussed in depth for their ability to reduce solvent consumption, minimize waste, and improve operational efficiency. These methods not only maintain high sensitivity and accuracy but also reduce the ecological impact of contaminant analysis. By comparing these sustainable approaches to conventional techniques, this review highlights their potential to meet regulatory standards while supporting eco-friendly practices within routine analysis laboratories.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465921"},"PeriodicalIF":3.8,"publicationDate":"2025-03-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143759297","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Sulfonic acid-functionalized covalent organic framework@Ti3C2Tx as efficient solid-phase microextraction blade coating for the extraction of monoamine neurotransmitters in rat serum samples
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-03-28 DOI: 10.1016/j.chroma.2025.465919
Cheng Yang , Nian Yang , Di Zhao , Zhiyu Zhang , Junying Song , Zhenqiang Zhang , Kai Hu , Shusheng Zhang
{"title":"Sulfonic acid-functionalized covalent organic framework@Ti3C2Tx as efficient solid-phase microextraction blade coating for the extraction of monoamine neurotransmitters in rat serum samples","authors":"Cheng Yang ,&nbsp;Nian Yang ,&nbsp;Di Zhao ,&nbsp;Zhiyu Zhang ,&nbsp;Junying Song ,&nbsp;Zhenqiang Zhang ,&nbsp;Kai Hu ,&nbsp;Shusheng Zhang","doi":"10.1016/j.chroma.2025.465919","DOIUrl":"10.1016/j.chroma.2025.465919","url":null,"abstract":"<div><div>Herein, a sulfonic-functionalized covalent organic framework@Ti<sub>3</sub>C<sub>2</sub>T<em><sub>x</sub></em> nanocomposite (SO<sub>3</sub>H<img>COF@Ti<sub>3</sub>C<sub>2</sub>T<em><sub>x</sub></em>) was synthesized and employed as solid phase microextraction (SPME) coating for isolation and extraction of monoamine neurotransmitters (MNTs) from rat serum samples. The resultant composite can combine the characteristics of hydrophilic Ti<sub>3</sub>C<sub>2</sub>T<em><sub>x</sub></em> and SO<sub>3</sub>H<img>COF, which endow it has multiple adsorption sites and can provide multiple interactions such as cation exchange, hydrogen bonding and π-π with the target MNTs. The synthesized SO<sub>3</sub>H<img>COF@Ti<sub>3</sub>C<sub>2</sub>T<em><sub>x</sub></em> SPME blades have excellent protein exclusion capability, ensuring high adsorption efficiency for MNTs. Under the optimized conditions, the proposed SO<sub>3</sub>H<img>COF@Ti<sub>3</sub>C<sub>2</sub>T<em><sub>x</sub></em> blades-based SPME-HPLC method exhibited good linearities (<em>r</em><sup>2</sup>≥0.9963), low limits of detection (0.015–0.030 ng mL<sup>-1</sup>) and low matrix effect (0.83 %-17.36 %). The recoveries of MNTs in the rat serum were in range of 90.3 %-118.3 %, with RSDs &lt;10.8 %. The SPME-HPLC method was successfully applied for the analysis of 4 MNTs in the serum of depression model rats. This work not only details the development of a multi-functional composite, but it also presents an effective strategy for the determination of trace MNTs in serum sample.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465919"},"PeriodicalIF":3.8,"publicationDate":"2025-03-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143747598","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}
引用次数: 0
Development of a highly sensitive field-amplified capillary electrophoresis tandem triple quadrupole mass spectrometry for the quantification of trace methamphetamine in sewage
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-03-28 DOI: 10.1016/j.chroma.2025.465920
Yanping Wei , Yujie Zhang , Yueting Hu , Fan Shui , Jia Tang , Yiyang Yu , Guocan Zheng , Jing Zeng
{"title":"Development of a highly sensitive field-amplified capillary electrophoresis tandem triple quadrupole mass spectrometry for the quantification of trace methamphetamine in sewage","authors":"Yanping Wei ,&nbsp;Yujie Zhang ,&nbsp;Yueting Hu ,&nbsp;Fan Shui ,&nbsp;Jia Tang ,&nbsp;Yiyang Yu ,&nbsp;Guocan Zheng ,&nbsp;Jing Zeng","doi":"10.1016/j.chroma.2025.465920","DOIUrl":"10.1016/j.chroma.2025.465920","url":null,"abstract":"<div><div>Accurate quantification of trace levels of illicit drugs in wastewater, such as methamphetamine (MAMP), is crucial for sewage epidemiology. In this study, we developed a novel method that integrates field-amplified sample injection capillary electrophoresis with triple quadrupole mass spectrometry (FASI-CE-QQQ MS). This method enables simultaneous on-line preconcentration and separation, coupled with highly sensitive detection. Validation demonstrated excellent linearity within the range of 1 to 200 ng/L (R² = 0.9996), a limit of detection (LOD) of 0.1 ng/L (S/<em>N</em> = 12.3), high accuracy (RE &lt; 6.4 %) and precision (RSD &lt; 11.4 %). It was successfully applied to quantify MAMP in two unknown water samples, yielding average concentrations of 3.70 ng/L and 84.73 ng/L, respectively. These results were consistent with those obtained from an interlaboratory comparison exercise across China using on-line solid-phase extraction coupled with ultra-high performance liquid chromatography tandem triple quadrupole mass spectrometry (on-line SPE-UHPLC-QQQ MS). Finally, a comprehensive comparison between the newly developed FASI-CE-QQQ MS and the on-line SPE-UHPLC-QQQ MS methods revealed that the FASI-CE-QQQ MS offers significant advantages in terms of sensitivity, rapidity, and reduced solvent and sample consumption, making it a promising approach for the accurate determination of trace drugs in water.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465920"},"PeriodicalIF":3.8,"publicationDate":"2025-03-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143747596","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}
引用次数: 0
Model-based analysis of a hydrophobic interaction chromatography for antibody-drug conjugate purification
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-03-27 DOI: 10.1016/j.chroma.2025.465916
Tobias Hahn , Fara Lyu , Pia Graf , Steve Richter , Jorge Gandarilla , Dean Clyne , Lei Cao , Chen Wang
{"title":"Model-based analysis of a hydrophobic interaction chromatography for antibody-drug conjugate purification","authors":"Tobias Hahn ,&nbsp;Fara Lyu ,&nbsp;Pia Graf ,&nbsp;Steve Richter ,&nbsp;Jorge Gandarilla ,&nbsp;Dean Clyne ,&nbsp;Lei Cao ,&nbsp;Chen Wang","doi":"10.1016/j.chroma.2025.465916","DOIUrl":"10.1016/j.chroma.2025.465916","url":null,"abstract":"<div><div>Antibody-drug conjugates (ADCs) are a class of biopharmaceutical drugs designed as a targeted therapy for treating cancer while sparing healthy cells. ADCs are complex molecules composed of an antibody linked to a biologically active cytotoxic drug. The drug-to-antibody ratio (DAR), which represents the number of drugs conjugated to an antibody, is an important quality attribute of ADCs. The conjugation process typically yields a complex DAR profile, which requires further purification to remove undesired DAR species. Separation of DAR species post conjugation reaction can be achieved using hydrophobic interaction chromatography (HIC). HIC utilizes the hydrophobicity differences of different drug-loaded ADCs to separate them by reversible interaction between the proteins and the hydrophobic stationary phase. The buffer greatly influences the binding interaction between hydrophobic proteins and a HIC resin, but the process is also sensitive to variations in temperature, resin attributes, and the solid-liquid ratio of the column. A mechanistic model that captures these critical process parameters and material and column properties was established from calibration studies using multiple well-characterized HIC columns and resin lots. This model enabled in-silico characterization of the HIC process and facilitated understanding of unexpected process performance observations. It revealed the importance of controlling resin-specific hydrophobic capacity to minimize the DAR separation variations. It led to identifying an effective process control strategy to ensure a consistent DAR profile.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465916"},"PeriodicalIF":3.8,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143747594","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}
引用次数: 0
Off-line in-tube solid-phase microextraction of some herbicides based on poly(styrene-divinylbenzene) coated Fe3O4 nanoparticles
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-03-26 DOI: 10.1016/j.chroma.2025.465910
Maedeh Saadat , Yadollah Yamini , Nasser Nikfarjam , Hanieh Kefayati
{"title":"Off-line in-tube solid-phase microextraction of some herbicides based on poly(styrene-divinylbenzene) coated Fe3O4 nanoparticles","authors":"Maedeh Saadat ,&nbsp;Yadollah Yamini ,&nbsp;Nasser Nikfarjam ,&nbsp;Hanieh Kefayati","doi":"10.1016/j.chroma.2025.465910","DOIUrl":"10.1016/j.chroma.2025.465910","url":null,"abstract":"<div><div>Triazines are a class of persistent micropollutants in environmental areas with high toxicity. Because of their general usage and poisonous and stability of their deteriorated products, extraction and determination trace amounts of triazines are important. Off-line in-tube solid phase microextraction efficiently used for extraction of trace amounts of analytes. In addition, magnetic field was used to keep the nanoparticles in the tube and also to enhance preconcentration of the analytes. Magnetic nanoparticles can be utilized as a reusable sorbent with high surface area, strong interaction, chemical stability and high selectivity.</div><div>A novel approach was introduced using a magnetic nanocomposite of cross-linked poly(styrene-divinylbenzene) for the in-tube solid-phase microextraction of triazine herbicides. The prepared material was characterized using various techniques. High performance liquid chromatography-ultraviolet detection was used to separate and determine the analytes. The effects of pH (6), extraction time (20 min), type and volume of elution solvent (500 µL methanol) and extraction flow rate (2 mL min<sup>-1</sup>), desorption flow rate (50 µL min<sup>-1</sup>) and salt addition (15%) and applying magnetic field on the extraction efficiency of the triazines were investigated. Under optimum conditions, calibration curves were found to be linear in the range of 0.3-500 µg L<sup>−1</sup> for cyanazine, simazine, and propazine with a coefficient of determination (R<sup>2</sup>) of 0.9951, 0.9984, and 0.9984, respectively. The LODs were 0.1 µg L<sup>−1</sup> for all of the analytes. The method was successfully used for the extraction and determination of triazine herbicides in fruit juice samples.</div><div>Magnetic nano particles illustrate minimum back pressure in tube due to elimination of filters, high surface-to-volume ratio and lot of active sites favorable for the adsorption of the analytes. Despite the limitations imposed by the chemical conditions of extraction on the application of nanoparticles and polymeric sorbents, variables such as pH, concentration, and surface charges do not influence the magnetic interactions of MNPs. By applying magnetic field, the magnetic nature of the analytes is effective on the preconcentration of them.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465910"},"PeriodicalIF":3.8,"publicationDate":"2025-03-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143747597","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}
引用次数: 0
An injection filling method for packing chromatography devices
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-03-26 DOI: 10.1016/j.chroma.2025.465913
Raja Ghosh, Justin Bernar
{"title":"An injection filling method for packing chromatography devices","authors":"Raja Ghosh,&nbsp;Justin Bernar","doi":"10.1016/j.chroma.2025.465913","DOIUrl":"10.1016/j.chroma.2025.465913","url":null,"abstract":"<div><div>An injection filling method for packing resin media in a chromatography device for protein separation is discussed in this paper. The method is first demonstrated by packing anion exchange resin within a cuboid chromatography device and a squat column, both having 7.5 mL bed volume. The method is further demonstrated by packing size exclusion chromatography media in a 50 mL cuboid chromatography device. Overall, the packing method is simple and is less demanding in terms of requirement for operator skill and experience. The devices packed using the injection filling method had excellent separation efficiency attributes. Flow through and eluted protein peaks obtained using a device with an intentional minor indentation on the inner surface of the chromatography device showed pre-peaks (or fronting) and these peaks were wider than those obtained with a device without such an indentation. Surface imperfections had a greater impact on eluted peaks than on flow-through peaks. Size exclusion chromatography experiment carried out at high flow rates showed that protein separation obtained with the 50 mL cuboid device packed using the injection filling method was superior to that obtained with a conventional 50 mL column packed with the same media. At a high flow rate. the resin-bed within the column compacted very significantly while no such compaction was observed in the cuboid device.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465913"},"PeriodicalIF":3.8,"publicationDate":"2025-03-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143738638","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Study of the aberrant retention behavior of a semi-crystalline polyamide in reversed-phase liquid chromatography
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-03-26 DOI: 10.1016/j.chroma.2025.465887
Jordy D. Kruijswijk , Stefan Wijker , Harry J.A. Philipsen , Peter J. Schoenmakers , Govert W. Somsen
{"title":"Study of the aberrant retention behavior of a semi-crystalline polyamide in reversed-phase liquid chromatography","authors":"Jordy D. Kruijswijk ,&nbsp;Stefan Wijker ,&nbsp;Harry J.A. Philipsen ,&nbsp;Peter J. Schoenmakers ,&nbsp;Govert W. Somsen","doi":"10.1016/j.chroma.2025.465887","DOIUrl":"10.1016/j.chroma.2025.465887","url":null,"abstract":"<div><div>The elution behavior of semi-crystalline polyamides (PAs) in reversed-phase liquid chromatography (RPLC) was examined. RPLC of the aliphatic polyamide 4,6 (PA46) yielded a single broad peak. However, the partly aromatic polyamide X (PAX) displayed a deviating elution profile, encompassing early- and late-eluting portions, which changed in relative abundance when varying injection and gradient conditions. These bands were suspected to be due to formation of amorphous and crystalline phases, respectively. RPLC fractions of the PAs were subjected to the same RPLC system and to size-exclusion chromatography. The presumed amorphous PAX portion showed two bands in RPLC, suggesting that (largely) amorphous and crystalline phases are formed upon sample injection. Differential scanning calorimetry (DSC) demonstrated that reducing the crystallinity of PAX decreased the relative abundance of the late-eluting fraction, approaching the behavior of aliphatic polyamides. X-ray diffraction and static-light-scattering analyses confirmed the semi-crystallinity of the two solid PA samples. Although both small particles and larger aggregates were observed in solution, these findings could not be correlated to the differences in elution profile of the PAs. Cloud-point measurements indicated that the solubility of both PA46 and PAX was almost independent of temperature. Strikingly, at low column temperatures (i.e. below the depressed melting point), PAX eluted as a single broad PAX peak. To conclude, the semi-crystallinity of PAX influences its RPLC-elution behavior, and by ensuring complete dissolution of the crystalline phase useful chemical information can be extracted from the obtained chromatograms.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465887"},"PeriodicalIF":3.8,"publicationDate":"2025-03-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143759299","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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