Journal of Chromatography A最新文献_第7页

Impact of nucleotide hydrophobicity on oligonucleotides separation in liquid chromatography 核苷酸疏水性对液相色谱中寡核苷酸分离的影响

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-14 DOI: 10.1016/j.chroma.2025.465968

Martin Gilar , Nils Schomann , Saskia Schott , Michael Rühl

{"title":"Impact of nucleotide hydrophobicity on oligonucleotides separation in liquid chromatography","authors":"Martin Gilar , Nils Schomann , Saskia Schott , Michael Rühl","doi":"10.1016/j.chroma.2025.465968","DOIUrl":"10.1016/j.chroma.2025.465968","url":null,"abstract":"<div><div>We investigated the contribution of nucleotide (nt) type and modifications on the retention and resolution of 22–24 nt long oligonucleotides in ion-pairing reversed-phase (IP RP) liquid chromatography (LC) and hydrophilic interaction chromatography (HILIC) methods. The nucleotides relative hydrophobicity affects the oligonucleotide LC retention and separation selectivity. The ion-pairing reagents of higher hydrophobicity (dipropylamine < dibutylamine < dipentylamine) require a greater organic solvents concentration to elute the oligonucleotides in IP RP LC. We observed that higher concentration of organic solvent reduced the contribution of (oligo)nucleotide hydrophobicity to the retention and led to more uniform separation of full-length oligonucleotide from its truncated products. We also investigated the diastereomeric resolution of 24 nt oligonucleotides with a single phosphorothioate modification at 5′-end. The diastereomeric separation is nucleotide-motif dependent; G (and modified G) nucleotides adjacent to the phosphorothioate linkage yield higher resolution of isomers than other types of nucleotides in IP RP LC and HILIC.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465968"},"PeriodicalIF":3.8,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143886693","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

Fast unmasking hazards of safe perfumes 快速揭露安全香水的危害

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-14 DOI: 10.1016/j.chroma.2025.465959

Gertrud E. Morlock , Julia Heil

{"title":"Fast unmasking hazards of safe perfumes","authors":"Gertrud E. Morlock , Julia Heil","doi":"10.1016/j.chroma.2025.465959","DOIUrl":"10.1016/j.chroma.2025.465959","url":null,"abstract":"<div><div>Perfumes are chemical cocktails and their effects on humans are complex and diverse. Only selected ingredients are studied, and risk assessment of the perfume is only theoretically carried out at the desk. To close the current gap in the hazard-related analysis of entire perfumes, a sustainable non-target chemical safety screening was developed. The 42 perfumes collected randomly were screened without any sample preparation for ten different adverse effects, <em>i.e.</em>, genotoxicity, cytotoxicity, antibacterial activity against Gram-negative and Gram-positive bacteria, neurotoxicity/-modulation, and endocrine-disrupting (aromatase-inhibiting, anti-/estrogenic, and anti-/androgenic) activities. Many hazardous compounds were detected in perfumes, regardless of price or gender-specific use. For example, the half-maximal effective dose (EC<sub>50</sub>) of genotoxicity was 1.3 µL perfume and the half-maximal aromatase inhibitory dose (IC<sub>50</sub>) was 11 nL perfume. One 100-µL spray shot of perfume on the skin exceeded the EC<sub>50</sub> by 77-fold and the IC<sub>50</sub> by 9,090-fold. The new hazard-related profiling of the entire perfumes has provided for the first time in-depth information and significant advances in the understanding of lifestyle products as entry paths for hazardous compounds to the human body. It empowers stakeholders to produce hazard-free perfumes according to ethical statements for the sake of consumer health, authorities to change to a proactive safety screening and address the current underregulation, and scientists to contribute to the global transition towards more sustainable analytical methods and products on the global market.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 465959"},"PeriodicalIF":3.8,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143929185","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

Assessment of LC-QTOF-MS data independent acquisition for quantification and suspect screening of pesticides in agriculture impacted water samples 评估独立于 LC-QTOF-MS 数据采集的农业影响水样中农药定量和可疑筛选方法

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-13 DOI: 10.1016/j.chroma.2025.465957

V. Fernández-Fernández, G. Castro, M. Ramil, I. Rodríguez

{"title":"Assessment of LC-QTOF-MS data independent acquisition for quantification and suspect screening of pesticides in agriculture impacted water samples","authors":"V. Fernández-Fernández, G. Castro, M. Ramil, I. Rodríguez","doi":"10.1016/j.chroma.2025.465957","DOIUrl":"10.1016/j.chroma.2025.465957","url":null,"abstract":"<div><div>Assessing the impact of agricultural pesticides, and their potential transformation products, in surface (SW) and groundwater (GW) requires the application of target and screening methodologies to cover the maximum number of species. This research investigates the performance of the data independent acquisition (DIA) mode for the quantification of target compounds and the suspect screening of additional pesticides in SW and GW based on a single chromatographic run. Samples were analysed using a liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) platform, combined with an on-line solid-phase extraction (SPE) step. A suite of fungicides and insecticides, widely employed in intensive viticulture areas, was selected to assess the performance of target and screening methodologies in combination with a database of product ion spectra for more than 700 pesticides. As regards quantification of targets, the method achieved limits of quantification (LOQs) between 2 ng l<sup>-1</sup> and 25 ng l<sup>-1</sup>, with linear responses from LOQs up to 500 ng l<sup>-1</sup>. Accuracy remained between 70 % and 120 %, based on the use of ultrapure water calibration standards. Suspect screening permitted the identification of 90 % of tested compounds when added to SW and GW at levels above 50 ng l<sup>-1</sup>, improving the percentage of correct identifications versus those attained operating the LC-QTOF-MS platform in the data dependent acquisition (DDA) mode.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1751 ","pages":"Article 465957"},"PeriodicalIF":3.8,"publicationDate":"2025-04-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143828622","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

The complete 2025 Wayne State University compound descriptor database for use with the solvation parameter model 完整的2025年韦恩州立大学化合物描述符数据库用于溶剂化参数模型

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-13 DOI: 10.1016/j.chroma.2025.465958

Colin F. Poole

{"title":"The complete 2025 Wayne State University compound descriptor database for use with the solvation parameter model","authors":"Colin F. Poole","doi":"10.1016/j.chroma.2025.465958","DOIUrl":"10.1016/j.chroma.2025.465958","url":null,"abstract":"<div><div>The solvation parameter model is a well-established quantitative structure-property relationship model suitable for describing the contribution of intermolecular interactions in a wide range of separation, chemical, biological, and environmental processes. The model employs six descriptors (seven for compounds that exhibit variable hydrogen-bond basicity) to characterize the capability of non-ionic compounds to interact with their environment. McGowan's characteristic volume (V) and excess molar refraction (E) for liquids at 20 °C can be calculated from structure and a refractive index value in the case of E. The other descriptors identified as dipolarity/polarizability (S), overall hydrogen-bond acidity (A),overall hydrogen-bond basicity (B or B°), the gas-liquid partition constant at 25 °C (L), and E for solids at 20 °C are experimental values assigned from retention factor measurements by gas, reversed-phase liquid, and micellar and microemulsion electrokinetic chromatography and liquid-liquid partition constants using the Solver method. The assembled descriptor database of 387 varied compounds (hydrocarbons, alcohols, aldehydes, anilines, amides, halohydrocarbons, esters, ethers, ketones, nitrohydrocarbons, phenols, steroids, organosiloxanes, and N-heterocyclic compounds) provide improved precision and predictive capability compared with the WSU-2020 descriptor database. The expanded and updated WSU-2025 descriptor database replaces the WSU-2020 descriptor database.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465958"},"PeriodicalIF":3.8,"publicationDate":"2025-04-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143834217","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

Theoretical study of modified multiple dual-mode elution counter-current chromatography based on chiral separation 基于手性分离的改良多重双模洗脱逆流色谱的理论研究

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-12 DOI: 10.1016/j.chroma.2025.465955

Fuxin Zhang , Xingcui Wang , Xinyi Huang , Jinlong Zhang , Duolong Di , Dong Pei , Jun Hai

{"title":"Theoretical study of modified multiple dual-mode elution counter-current chromatography based on chiral separation","authors":"Fuxin Zhang , Xingcui Wang , Xinyi Huang , Jinlong Zhang , Duolong Di , Dong Pei , Jun Hai","doi":"10.1016/j.chroma.2025.465955","DOIUrl":"10.1016/j.chroma.2025.465955","url":null,"abstract":"<div><div>The fact that both phases are liquids makes it simple to implement counter-current chromatography (CCC), which involves alternating elution modes and phase roles during the separation process. Using two distinct multiple dual-mode (MDM) elution techniques for chiral separation, the team demonstrated a superior separation effect in a prior study. When selecting a chiral selector with high enantiomer recognition capability is difficult, the separation efficiency of the CCC column can be enhanced through multiple cycles. This approach facilitates the preparation of enantiomers that are challenging to isolate under classical CCC conditions. A straightforward mathematical model was created in this study to forecast the number of cycles and the mode conversion time needed for the separation process after the modified MDM method was further examined theoretically. After modeling molecules, the theoretical model was confirmed, and the outcomes generally agreed with the calculations from the theoretical model. This offers substantial support for the modified MDM method's real-world implementation in chiral separation.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465955"},"PeriodicalIF":3.8,"publicationDate":"2025-04-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143855526","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

Accelerating mechanistic model calibration in protein chromatography using artificial neural networks 利用人工神经网络加速蛋白质色谱机制模型校准

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-11 DOI: 10.1016/j.chroma.2025.465953

Dominik Voltmer, Tinu Koshy, Raena Morley, Felix Wittkopp

{"title":"Accelerating mechanistic model calibration in protein chromatography using artificial neural networks","authors":"Dominik Voltmer, Tinu Koshy, Raena Morley, Felix Wittkopp","doi":"10.1016/j.chroma.2025.465953","DOIUrl":"10.1016/j.chroma.2025.465953","url":null,"abstract":"<div><div>In the manufacturing of therapeutic monoclonal antibodies (mAbs), mechanistic models can aid the evaluation and selection of suitable chromatography operating conditions during process development. However, model calibration remains a common bottleneck for model implementation in industrial settings. To accelerate the calibration process, the present study proposes a semi-automated, artificial neural network (ANN)-assisted calibration workflow for the efficient estimation of model parameters. The workflow is applied for the calibration of the multicomponent kinetic formulation of the steric mass-action (SMA) isotherm model for cation exchange chromatography (CEX). Three case studies using two mAb feedstocks of differing complexity regarding their structure and impurities are investigated. Different combinations of training data (low and/or high load density) and parameter groupings (one-step approach for estimation of all parameters simultaneously; two-step approach for estimation of (1) equilibrium and charge followed by (2) effective mass transfer coefficient, kinetic, and shielding) are applied for the target compounds and impurities.</div><div>The ANN-assisted calibration workflow provided acceptable model parameter estimations and subsequent good agreement between experimental and simulated chromatograms with only minimal refinement by inverse fitting for the target compounds of both feedstocks. For the impurities, the one-step parameter estimation approach showed satisfactory prediction quality only for the simple feedstock. For the complex feedstock, the two-step approach using only high loading data improved parameter prediction for both the impurities and the target compound. The observed reduction in calibration effort suggests great potential for ANN applications to facilitate mechanistic model calibration, thus enhancing and streamlining downstream process development for complex antibodies.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465953"},"PeriodicalIF":3.8,"publicationDate":"2025-04-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143844131","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

The implicit role of the hold-up volume in defining the adsorbed layer thickness 在确定吸附层厚度时，截留量的隐含作用

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-10 DOI: 10.1016/j.chroma.2025.465952

Hung-Wei Tsui , Wen-Lan Zhou , Cheng-Da Wu

引用次数: 0

Separation method using column sealing technology with silicon pneumatic microvalve in capillary gas chromatography 毛细管气相色谱分离方法采用硅胶气动微阀柱密封技术

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-10 DOI: 10.1016/j.chroma.2025.465950

Shigeaki Shibamoto, Wenjian Lu, Ayaka Sato

引用次数: 0

Extended multidimensional design space studies: Comparing volatile and non-volatile buffer systems in UPLC 扩展多维设计空间研究：UPLC中挥发性和非挥发性缓冲系统的比较

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-10 DOI: 10.1016/j.chroma.2025.465951

Arnold Zöldhegyi , Barnabás Soós , Krisztián Horváth , Imre Molnár , Róbert Kormány

{"title":"Extended multidimensional design space studies: Comparing volatile and non-volatile buffer systems in UPLC","authors":"Arnold Zöldhegyi , Barnabás Soós , Krisztián Horváth , Imre Molnár , Róbert Kormány","doi":"10.1016/j.chroma.2025.465951","DOIUrl":"10.1016/j.chroma.2025.465951","url":null,"abstract":"<div><div>Selecting the appropriate pH modifiers for separating ionizable compounds in HPLC often presents complex challenges that are frequently overlooked by industry practitioners. In Reversed-Phase Chromatography (RPC), defining pH is particularly problematic due to the presence of organic solvents, which influence the dissociation behavior of buffering agents, ionizable analytes, and residual silanol groups on the silica base material. Additional factors such as temperature changes and varying buffering capacities further complicate the interpretation of pH-effects on the separation.</div><div>A key practical question arises: can a volatile acetate buffer effectively replace an equimolar non-volatile phosphate buffer within the same pH range? To explore this, we utilized an Analytical Quality by Design (AQbD) modeling approach with DryLab to construct and compare three-dimensional (t<sub>G</sub>-T-pH) separation models for terazosin and selected impurities across a pH range of 6.0–8.0. These Design Space (DS) models provided a comprehensive understanding of the dynamic changes occurring within each separation system. Notably, our findings revealed not only equivalent separation performance, as indicated by overlapping Method Operable Design Regions (MODRs), but also critical insights into buffer-specific differences in the selectivity of HPLC-separations.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1751 ","pages":"Article 465951"},"PeriodicalIF":3.8,"publicationDate":"2025-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143823617","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

Integrated mammalian cell culture and growth measurement using headspace analysis: Experimental and modeling results 综合哺乳动物细胞培养和生长测量使用顶空分析：实验和建模结果

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-09 DOI: 10.1016/j.chroma.2025.465947

Hui-Jun Jin , Zi-Dong Qiu , Chun-Yun Zhang , Yu Peng

{"title":"Integrated mammalian cell culture and growth measurement using headspace analysis: Experimental and modeling results","authors":"Hui-Jun Jin , Zi-Dong Qiu , Chun-Yun Zhang , Yu Peng","doi":"10.1016/j.chroma.2025.465947","DOIUrl":"10.1016/j.chroma.2025.465947","url":null,"abstract":"<div><div>Closed-system mammalian cell culture methods have gained prominence due to their potential to minimize contamination risks and support compact experimental designs. However, complete closed-systems often encounter challenges such as pH regulation and oxygen supplementation. This study introduces a novel approach that integrates headspace analysis with mammalian cell culture. The method enables in-situ measurement of CO<sub>2</sub> production by cells, providing quantitative understanding of cell growth. Importantly, we developed mathematical models to elucidate the dynamics of pH changes and oxygen depletion, offering predictive insights for optimizing culture conditions for different cell lines. Using HepG2 cells as a model cell line, the present method agreed well with the reference method (i.e., sulforhodamine B assay) on determining the cell growth curve (R<sup>2</sup> = 0.98). Furthermore, the method demonstrated good precision, with biological replicates showing relative standard deviations below 7 % across 24-, 36-, and 48-hour culture periods. This integrated approach not only provides solutions for mitigating the limitations of closed-system cell culture but also establishes a framework for high-throughput and efficient applications in biomanufacturing and biomedical research.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1751 ","pages":"Article 465947"},"PeriodicalIF":3.8,"publicationDate":"2025-04-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143826444","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