Journal of Chromatography A最新文献

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A simplified one-pot derivatization/magnetic solid-phase extraction with integrated pH adjustment strategy coupled with liquid chromatography-fluorescence detection for fatty aldehyde analysis 一种简化的一锅衍生/磁固相萃取集成pH调整策略-液相色谱-荧光检测法分析脂肪醛
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-04-24 DOI: 10.1016/j.chroma.2025.465988
Nian Shi , Yuyang Wang , Mengyuan Lv , Xudong Xia , Zihan Li , Di Chen , Ranran Duan , Jinghua Zhang
{"title":"A simplified one-pot derivatization/magnetic solid-phase extraction with integrated pH adjustment strategy coupled with liquid chromatography-fluorescence detection for fatty aldehyde analysis","authors":"Nian Shi ,&nbsp;Yuyang Wang ,&nbsp;Mengyuan Lv ,&nbsp;Xudong Xia ,&nbsp;Zihan Li ,&nbsp;Di Chen ,&nbsp;Ranran Duan ,&nbsp;Jinghua Zhang","doi":"10.1016/j.chroma.2025.465988","DOIUrl":"10.1016/j.chroma.2025.465988","url":null,"abstract":"<div><div>A novel one-pot derivatization/magnetic solid-phase extraction with integrated pH adjustment (OPD/MSPE-pH) strategy was developed for the efficient and selective quantification of fatty aldehydes. This method seamlessly integrates pH regulation, derivatization, and magnetic separation in a single incubation step, where the sample solution, derivatization reagent, and magnetic composite (Fe₃O₄/MWCNTs-OH/CA) are processed together, significantly simplifying sample preparation. The magnetic composite, synthesized from Fe₃O₄ nanoparticles, hydroxylated multi-walled carbon nanotubes (MWCNTs-OH), and citric acid (CA), functions both as an acidic pH regulator and an efficient adsorbent for aldehyde-fluorenylmethyl carbazate (FMC) derivatives. Compared to conventional approaches, the OPD/MSPE-pH method exhibited superior operation efficiency, achieving low limits of detection (1.1–2.4 nM) and high recoveries (91.7–106.1 %). The optimized procedure was successfully applied to plasma and spiked plasma samples, demonstrating its effectiveness in complex biological matrices. This streamlined technique eliminates the need for additional pH-adjusting reagents and centrifugation, offering a practical, rapid, and highly efficient solution for fatty aldehyde analysis. Overall, the proposed OPD/MSPE-pH method provides a robust, sensitive, and reliable analytical platform for fatty aldehyde analysis, with potential applications in broader fields with suitable modifications.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465988"},"PeriodicalIF":3.8,"publicationDate":"2025-04-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143886699","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
Quantitative analysis of nonylphenol ethoxylates in textiles using ultrasonic/microwave-assisted extraction coupled with ultra-high-performance supercritical fluid chromatography-photodiode array-tandem mass spectrometry 超声波/微波辅助萃取-超高效超临界液相色谱-光电二极管阵列-串联质谱法定量分析纺织品中壬基酚聚氧乙烯酯
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-04-23 DOI: 10.1016/j.chroma.2025.465985
Haiyan Gao , Yuncheng Ge , Lili Tong , Lei Yin , Qiang Ma
{"title":"Quantitative analysis of nonylphenol ethoxylates in textiles using ultrasonic/microwave-assisted extraction coupled with ultra-high-performance supercritical fluid chromatography-photodiode array-tandem mass spectrometry","authors":"Haiyan Gao ,&nbsp;Yuncheng Ge ,&nbsp;Lili Tong ,&nbsp;Lei Yin ,&nbsp;Qiang Ma","doi":"10.1016/j.chroma.2025.465985","DOIUrl":"10.1016/j.chroma.2025.465985","url":null,"abstract":"<div><div>A sensitive and robust analytical method was developed for the simultaneous determination of nonylphenol ethoxylates (NPEOs) in textiles. The method utilizes ultra-high-performance supercritical fluid chromatography with photodiode array detection (UHPSFC-PDA) to assess monomer proportions across varying polymerization degrees, followed by quantitation via tandem mass spectrometry (UHPSFC-MS/MS) in multiple reaction monitoring (MRM) mode. Under optimized conditions, NPEOs (<em>n</em> = 2–39) were separated within 7 min on a BEH C<sub>18</sub> column using compressed CO₂ and methanol as the mobile phase. Additionally, response surface methodology and Box-Behnken design were employed to optimize ultrasonic/microwave-assisted extraction (UMAE) parameters. The method demonstrated excellent linearity (R² &gt; 0.99) for 13 NPEO homologues (<em>n</em> = 2–14), with limits of detection (LODs) and quantitation (LOQs) values ranging from 0.26 to 45.09 μg/kg and 2.28–188.06 μg/kg, respectively. Intra- and inter-day precision values ranged from 0.8 % to 4.23 % and from 1.34 % to 9.59 %, respectively. Recoveries at low, medium, and high spiking levels were between 71.1 % and 102.5 % (RSD ≤ 12.98 %). The method was validated using quality control standards and successfully applied to commercial textile samples, revealing NPEO concentrations up to 2626.63 μg/kg. The combination of UMAE with UHPSFC-PDA-MS/MS offers a rapid, sensitive, and environmentally friendly solution for comprehensive NPEO analysis in textiles.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465985"},"PeriodicalIF":3.8,"publicationDate":"2025-04-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143895392","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
Simultaneous determination of cations in nuclear power plant water by conductometric ion chromatography equipped with fluorescence detector 带荧光检测器的电导离子色谱法同时测定核电站水中阳离子
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-04-23 DOI: 10.1016/j.chroma.2025.465984
Wen Huang, Xiaoting Li, Feifang Zhang, Yufeng Shen, Bingcheng Yang
{"title":"Simultaneous determination of cations in nuclear power plant water by conductometric ion chromatography equipped with fluorescence detector","authors":"Wen Huang,&nbsp;Xiaoting Li,&nbsp;Feifang Zhang,&nbsp;Yufeng Shen,&nbsp;Bingcheng Yang","doi":"10.1016/j.chroma.2025.465984","DOIUrl":"10.1016/j.chroma.2025.465984","url":null,"abstract":"<div><div>This study presents a simultaneous determination method for common corrosion-mark cations (Li⁺, NH₄⁺, monoethanolamine, Zn²⁺, and Cd²⁺) in nuclear power plant water. The analysis employs conductometric ion chromatography combined with a custom-built liquid core waveguide capillary scale fluorescence detector. Monovalent cations (Li⁺, NH₄⁺, monoethanolamine) were detected conductometrically with detection limits of 56–108 nM, while divalent heavy metals (Zn²⁺, Cd²⁺) were specifically quantified through the fluorescence detector, achieving detection limits of 42 nM and 33 nM, respectively. The method demonstrates good analytical performance, as indicated by the spiked recoveries ranging from 88.50 % to 128.54 % and relative standard deviations between 0.10 % and 4.16 % for all target analytes.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465984"},"PeriodicalIF":3.8,"publicationDate":"2025-04-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143877152","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 micro gas chromatographic column with in-situ growing macro-porous silicon as stationary phase support layer 以原位生长大孔硅为固定相支撑层的微型气相色谱柱
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-04-23 DOI: 10.1016/j.chroma.2025.465982
Wenbo Li , Shaojie Ma , Yuchen Zhu , Bin Zhao , Fei Feng
{"title":"A micro gas chromatographic column with in-situ growing macro-porous silicon as stationary phase support layer","authors":"Wenbo Li ,&nbsp;Shaojie Ma ,&nbsp;Yuchen Zhu ,&nbsp;Bin Zhao ,&nbsp;Fei Feng","doi":"10.1016/j.chroma.2025.465982","DOIUrl":"10.1016/j.chroma.2025.465982","url":null,"abstract":"<div><div>This paper reports a micro gas chromatographic column (μGCC) with in-situ growing macro-porous silicon as the stationary phase support layer. The macro-porous silicon stationary phase support layer (MPSL) with uniform thickness was fabricated in-situ on the inner surface of the μGCC channels by metal-assisted chemical etching. In order to avoid the negative effect of uneven thickness of the stationary phase, a 10 nm alumina film was deposited as the stationary phase on the MPSL using the atomic layer deposition technique. The macro-porous structure and high specific surface area of the MPSL provide longer diffusion paths and larger mass transfer interfaces for the analytes, which reduces the longitudinal gas diffusion and mass transfer resistance, thus improving the column efficiency. The μGCC with the MPSL achieved a 1306.7 % increase in the theoretical plate number and a 195.0 % improvement in the resolution for n-nonane compared with the μGCC without the MPSL.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465982"},"PeriodicalIF":3.8,"publicationDate":"2025-04-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143892265","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
Membrane protected multi-template molecularly imprinted polymer based micro-solid phase extraction coupled with high performance liquid chromatography for analysis of chlorophenols 基于膜保护的多模板分子印迹聚合物微固相萃取-高效液相色谱法分析氯酚
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-04-22 DOI: 10.1016/j.chroma.2025.465981
Xiuqi Lang , Shanchao Fu , Huizhen Zhao , Wenhui Lu , Deyi Zhu , Shan Cao , Lingxin Chen , Jinhua Li
{"title":"Membrane protected multi-template molecularly imprinted polymer based micro-solid phase extraction coupled with high performance liquid chromatography for analysis of chlorophenols","authors":"Xiuqi Lang ,&nbsp;Shanchao Fu ,&nbsp;Huizhen Zhao ,&nbsp;Wenhui Lu ,&nbsp;Deyi Zhu ,&nbsp;Shan Cao ,&nbsp;Lingxin Chen ,&nbsp;Jinhua Li","doi":"10.1016/j.chroma.2025.465981","DOIUrl":"10.1016/j.chroma.2025.465981","url":null,"abstract":"<div><div>Multi-template molecularly imprinted materials (mt-MIPs) were prepared by surface imprinting and sealed into porous nylon membrane as micro-solid phase extraction (μ-SPE) device, coupled with high performance liquid chromatography (HPLC) to simultaneously extract and determine five typical chlorophenols (CPs) in leather matrices. By using well-prepared mesoporous silica modified multiwalled carbon nanotubes (MWCNTs@mSi) as supporting materials, and the mixture solution of five CPs as templates, the imprinted layer containing recognition sites of the CPs were formed via free radical polymerization. The as-prepared mt-MIPs were characterized by SEM, TEM, FT-IR and TGA, and the adsorption properties were investigated including static, dynamic and selective adsorption, showing high adsorption capacity of 39.15‒71.43 mg g<sup>−1</sup> and rapid mass transfer rate (within 30 min). Parameters affecting the extraction efficiency of membrane protected μ-SPE were optimized, including the type of membrane, amount of adsorbent, type and volume of desorption solvent, desorption time and salt effect. The established mt-MIPs-μ-SPE-HPLC method demonstrated satisfactory linearity of 2.0‒200 µg L<sup>−1</sup>, high sensitivity with LODs of 0.17‒0.52 µg L<sup>−1</sup>, and high enrichment factor (70.6‒144). Consequently, the method was successfully applied to the analysis of five CPs in tannery wastewater, finished leather and wet blue samples. Spike recoveries ranged from 73.00 %‒115.2 %, with RSDs of 0.28 %‒11.4 %, and matrix interference was examined to be negligible. The developed method proved viable for the simultaneous extraction and quantification of trace CPs in complex leather matrices.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465981"},"PeriodicalIF":3.8,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143886689","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 process development for hydrophobic interaction chromatography by considering prediction uncertainty analysis 考虑预测不确定度分析的疏水相互作用色谱的模型工艺开发
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-04-22 DOI: 10.1016/j.chroma.2025.465979
Yu-Xiang Yang, Shan-Jing Yao, Dong-Qiang Lin
{"title":"Model-based process development for hydrophobic interaction chromatography by considering prediction uncertainty analysis","authors":"Yu-Xiang Yang,&nbsp;Shan-Jing Yao,&nbsp;Dong-Qiang Lin","doi":"10.1016/j.chroma.2025.465979","DOIUrl":"10.1016/j.chroma.2025.465979","url":null,"abstract":"<div><div>Mechanistic models offer powerful tools for process development and optimization of hydrophobic interaction chromatography (HIC). Suitable parameter estimation approaches can efficiently calibrate the models, but some unavoidable biases between model prediction and actual experiment would reduce the credibility of the model’s applications. In this study, a well-calibrated HIC model was found some significant discrepancies between the predicted yield (97.3 %) and experimental yield (86.0 %) during the process optimization. Therefore, Bayesian inference with Markov Chain Monte Carlo method was employed to calculate the uncertainty of model parameters, which was then transformed into the uncertainty of model predictions. The results indicated that the model-predicted yield uncertainty interval was as large as 76.9∼96.5 %, which was consistent with the experiment. Moreover, the model prediction uncertainty analysis was integrated into process optimization to obtain a more reliable and low-risk separation condition. The re-optimized process significantly narrowed the uncertainty of the predicted yield (94.2∼98.9 %), and high experimental yield (95.8 %) was obtained. The results demonstrated that process optimization based on the uncertainty quantification could reasonably reflect model prediction deviations, assist process development and contribute to product quality improvement. Finally, a framework was proposed for process optimization based on the uncertainty analysis to improve the accuracy of model predictions and reducing the risk of model-based process development.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465979"},"PeriodicalIF":3.8,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143881873","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
Multi-component behavior of host-cell protein- and antibody-containing heteroaggregates in protein A chromatography 蛋白A层析中宿主细胞含蛋白和抗体异聚集体的多组分行为
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-04-22 DOI: 10.1016/j.chroma.2025.465954
Soumitra Bhoyar, Max Foster, Abraham M. Lenhoff
{"title":"Multi-component behavior of host-cell protein- and antibody-containing heteroaggregates in protein A chromatography","authors":"Soumitra Bhoyar,&nbsp;Max Foster,&nbsp;Abraham M. Lenhoff","doi":"10.1016/j.chroma.2025.465954","DOIUrl":"10.1016/j.chroma.2025.465954","url":null,"abstract":"<div><div>Despite its high selectivity and affinity towards the monoclonal antibody (mAb) product, protein A chromatography displays persistence of impurities such as host-cell proteins (HCPs) and high molecular weight (HMW) species, necessitating further purification steps. One factor in the persistence of HCPs and HMWs is the presence of mAb-HCP heteroaggregates that can co-elute with the mAb. This work investigates the chromatographic behavior of persistent aggregate species of a number of IgG1s and IgG4s, using both industrial harvested cell culture fluids (HCCFs) and protein A eluates as feeds. For two classes of aggregates, classified as small and large by size-exclusion chromatography (SEC), the protein A chromatography behavior was determined experimentally and a multi-component, mechanistic model based on the general rate model (GRM) was developed to describe and predict chromatographic breakthrough and elution under various process conditions. The model-predicted column outlet profiles and intra-particle uptake profiles agree satisfactorily with experimental chromatographic and confocal laser scanning microscopy data, respectively. Within the model framework, the basis for separation is that the binding affinity ratio for small aggregates (SA) relative to that of the mAb increases from near 1 at pH 7 to <span><math><mrow><mo>&gt;</mo><mn>4</mn></mrow></math></span> at pH 4.2, while for large aggregates (LA) the ratios are <span><math><mrow><mo>∼</mo><mn>25</mn></mrow></math></span> and <span><math><mrow><mo>∼</mo><mn>35</mn></mrow></math></span> respectively, resulting in lower elution pH ranges for the aggregates. These results and the model may aid in aggregate clearance and may also have broader application in multicomponent chromatographic modeling.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465954"},"PeriodicalIF":3.8,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143886692","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
Multifaceted separations approach for elucidation of the physical and chemical properties of extracellular hydrocolloids 细胞外水胶体的物理和化学性质的阐明的多方面分离方法
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-04-22 DOI: 10.1016/j.chroma.2025.465980
Kaitlin C. Lesco , Stefanie Van Wychen , Arnav Deshpande , Lieve M.L. Laurens , S. Kim Ratanathanawongs Williams
{"title":"Multifaceted separations approach for elucidation of the physical and chemical properties of extracellular hydrocolloids","authors":"Kaitlin C. Lesco ,&nbsp;Stefanie Van Wychen ,&nbsp;Arnav Deshpande ,&nbsp;Lieve M.L. Laurens ,&nbsp;S. Kim Ratanathanawongs Williams","doi":"10.1016/j.chroma.2025.465980","DOIUrl":"10.1016/j.chroma.2025.465980","url":null,"abstract":"<div><div>A multifaceted separations platform that incorporates the strengths of asymmetrical flow field-flow fractionation with multi-detectors (AF4-MD), high performance anion exchange chromatography (HPAEC), and hydrophilic interaction liquid chromatography with mass spectrometry (HILIC-MS) is developed to obtain a more complete picture of the molecular weights (MW), composition, and salt-induced aggregation behavior of extracellular polymeric substances (EPS) produced by the algae <em>Chlorella vulgaris</em>. The absence of a stationary phase makes AF4-MD particularly well suited for characterizing polydisperse hydrocolloid polymers as well as studies that investigate the effect of ionic environments that aligns with the natural environment of <em>C. vulgaris</em>. Fractionation of <em>C. vulgaris</em> EPS revealed three distinct MW populations ranging from 4 × 10⁴ to 3 × 10⁸ Daltons. This exceeds the previously reported MW by three orders of magnitude and reports a previously unknown size subpopulation. The optimized AF4-MD technique was then used to produce two size fractions that were probed using HPAEC and LC-MS. These orthogonal methods uncovered compositional heterogeneity across fractions, with variations in monosaccharides and amino acids.</div><div>AF4-MD is also well suited for studying the behavior of EPS in the presence of different salts. For each salt studied, e.g., NaNO<sub>3</sub>, NaCl, and MgCl<sub>2</sub>, an increase in solution ionic strength results in aggregation as corroborated by a shift to higher MWs. Each salt exhibited distinct effects on EPS aggregation, with NaCl causing the least aggregation and MgCl<sub>2</sub> the most. These findings highlight the need for multiple techniques when analyzing complex polymers such as EPS and the benefits of AF4-MD in elucidating complex polymer behaviors in different ionic environments.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465980"},"PeriodicalIF":3.8,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143886694","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
Diels-Alder post-crosslinked sulfonic acid-functionalized polymer for high-performance chiral separation of fluoxetine enantiomers diols - alder后交联磺酸功能化聚合物用于氟西汀对映体的高效手性分离
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-04-21 DOI: 10.1016/j.chroma.2025.465978
Ghadah Aljohani , Nawaf Albeladi , Khadra B. Alomari , Aliyah S. Alhawiti , M. Monier , Ibrahim Youssef
{"title":"Diels-Alder post-crosslinked sulfonic acid-functionalized polymer for high-performance chiral separation of fluoxetine enantiomers","authors":"Ghadah Aljohani ,&nbsp;Nawaf Albeladi ,&nbsp;Khadra B. Alomari ,&nbsp;Aliyah S. Alhawiti ,&nbsp;M. Monier ,&nbsp;Ibrahim Youssef","doi":"10.1016/j.chroma.2025.465978","DOIUrl":"10.1016/j.chroma.2025.465978","url":null,"abstract":"<div><div>Selective isolation and determination of chiral drugs remain among the biggest hurdles in the pharmaceutical and analytical domains. In this research, a sulfonic acid-functionalized phenolic resin (P-SO<sub>3</sub>H) was synthesized as a high-capacity adsorbent for S-fluoxetine (S-FX) utilizing electrostatic interaction and hydrogen bonding for the enhancement of adsorption. For introduction of enantioselectivity and stabilization of binding sites, imprinting was performed through Diels-Alder (DA) post-crosslinking with bis(maleimido)ethane (BMO), resulting in the S-FX-imprinted polymer (S-FX-P). Batch adsorption experiments revealed maximum adsorption in the pH range of 6–7 where S-FX-P expressed a 12 times stronger affinity towards S-FX than R-FX, indicating the presence of well-defined molecular recognition sites. Isotherm analysis indicated that adsorption was according to the Langmuir model with &gt;490 mg/g maximum adsorption capacity. Column-based enantioseparation led to 97 % enantiomeric excess (ee) of R-FX in the initial eluate and 91 % ee of S-FX in the recovered fraction. In contrast, the non-imprinted polymer (NIP) was enantioselective-free. These results attest to the competence of post-crosslinked sulfonated MIPs in high-performance chiral separation with prospect application in the purification of drugs and enantiomeric drug analysis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465978"},"PeriodicalIF":3.8,"publicationDate":"2025-04-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143903921","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 GC-ITQ-MS chromatographic system for the identification of hydroxy derivatives of polycyclic aromatic hydrocarbons in wastewater GC-ITQ-MS色谱系统用于废水中多环芳烃羟基衍生物的鉴定
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2025-04-20 DOI: 10.1016/j.chroma.2025.465969
Justyna Pamuła , Elżbieta Sochacka-Tatara , Katarzyna Styszko
{"title":"Development of GC-ITQ-MS chromatographic system for the identification of hydroxy derivatives of polycyclic aromatic hydrocarbons in wastewater","authors":"Justyna Pamuła ,&nbsp;Elżbieta Sochacka-Tatara ,&nbsp;Katarzyna Styszko","doi":"10.1016/j.chroma.2025.465969","DOIUrl":"10.1016/j.chroma.2025.465969","url":null,"abstract":"<div><div>The purpose of the study was to develop and validate a method for determining selected hydroxy derivatives of polycyclic aromatic hydrocarbons (OH-PAHs) in environmental samples such as wastewater using gas chromatography-ion trap mass spectrometry (GC-ITQ-MS). This was motivated by the environmental and health risks posed by OH-PAHs, which are widespread pollutants known for their potential carcinogenic and mutagenic properties. The research focused on the selection of GC-ITQ-MS operating parameters, optimizing the extraction and derivatization processes to ensure accurate and reliable detection of these compounds in wastewater. Solid phase extraction using C18 columns eluted with tetrahydrofuran and dichloromethane mixtures provided the best recoveries for most OH-PAHs. The derivatization process was optimized by determining the optimal temperature and time conditions, with the conclusion that MTBSTFA was effective for all seven OH-PAHs analyzed. The developed method was applied to real wastewater samples from the Płaszów Wastewater Treatment Plant in Krakow. The presence of OH-PAH was detected in concentrations ranging from several to several hundred ng/l. The average concentration values were 75.0 ng/L and 646.8 ng/L for 1- and 2-hydroxynaphthalene, 23.4 ng/L and 543.4 ng/L for 2- and 9-hydroxyfluorene, 13.2 ng/L for 9-hydroxyphenanthrene, and 16.3 ng/L for 1-hydroxypyrene, respectively. Analyses of real samples were preceded by experiments on the stability of OH-PAHs in wastewater. These studies showed that PAH metabolites change in the aqueous phase, with degradation within a few hours ranging from several to several dozen percent.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465969"},"PeriodicalIF":3.8,"publicationDate":"2025-04-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143877151","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
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