首页 > 最新文献

Journal of separation science最新文献

英文 中文
Rambutan-Like Nickel Sulfide Modified With Carbon Nanospheres on Nickel Foam for Syringe Membrane Filter-Based Extraction of Nitroimidazoles 泡沫镍表面碳纳米球修饰类兰布坦硫化镍用于注射器膜过滤萃取硝基咪唑。
IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2026-02-03 DOI: 10.1002/jssc.70363
Honglin Qin, Wang Yao, Lizhen Qiao, Xiuchao Yao

In the present work, nickel sulfide (Ni3S2) was modified on the surface of Ni foams (NiF) by in-situ growth, and the prepared rambutan-like Ni3S2/NiF materials were further decorated with carbon nanospheres. Subsequently, the prepared C/Ni3S2/NiF was loaded into a syringe filter and used for syringe membrane filter-based solid-phase microextraction (SMF-SPME) of five nitroimidazoles (NDZs), followed by high-performance liquid chromatography-ultraviolet detection. The metal affinity of divalent Ni (II) and the imidazole group could contribute to the selective adsorption to NDZs, and the structural porous support of Ni foams, the in-situ modified Ni3S2, and carbon nanospheres facilitated the improvement of SMF-SPME efficiency. The main experimental parameters affecting the extraction efficiency were studied, including sample flow rate, adsorption cycle, salt concentration, pH of sample solution, the type and volume of desorption solvent. The selectivity of the adsorbent membrane C/Ni3S2/NiF to NDZs was evaluated, and the interactions existing between the modified materials on Ni foam and NDZs were examined to probe the possible adsorption mechanism. Under the optimal conditions, the proposed method showed good linearity from 0.05 to 200 µg L−1 and possessed low limits of detection within 0.01–0.05 µg L−1. The reproducibility and reusability of the C/Ni3S2/NiF adsorbent were investigated, and the effective enrichment and determination of NDZs in water, milk, and honey samples were also carried out with recoveries of 79.3%–114.5%. This study provides a new strategy for the enrichment and determination of some NDZs in different samples.

本文采用原位生长的方法在泡沫镍(Ni foam, NiF)表面改性硫化镍(Ni3S2),并用碳纳米球进一步修饰所制备的类rambutan Ni3S2/NiF材料。随后,将制备好的C/Ni3S2/NiF装入注射器过滤器,用于注射器膜过滤器固相微萃取(SMF-SPME)法提取5种硝基咪唑(ndz),并进行高效液相色谱-紫外检测。二价Ni (II)和咪唑基团的金属亲和力有助于对NDZs的选择性吸附,Ni泡沫、原位改性Ni3S2和碳纳米球的结构多孔支撑有助于SMF-SPME效率的提高。研究了影响萃取效率的主要实验参数,包括样品流速、吸附循环、盐浓度、样品溶液pH、解吸溶剂种类和体积。考察了C/Ni3S2/NiF吸附膜对NDZs的选择性,并考察了改性材料对Ni泡沫和NDZs的相互作用,探讨了可能的吸附机理。在最佳条件下,该方法在0.05 ~ 200µg L-1范围内线性良好,最低检出限在0.01 ~ 0.05µg L-1范围内。考察了C/Ni3S2/NiF吸附剂的重现性和可重复使用性,并对水、牛奶和蜂蜜样品中的ndz进行了有效富集和测定,回收率为79.3% ~ 114.5%。本研究为不同样品中某些ndz的富集和测定提供了新的策略。
{"title":"Rambutan-Like Nickel Sulfide Modified With Carbon Nanospheres on Nickel Foam for Syringe Membrane Filter-Based Extraction of Nitroimidazoles","authors":"Honglin Qin,&nbsp;Wang Yao,&nbsp;Lizhen Qiao,&nbsp;Xiuchao Yao","doi":"10.1002/jssc.70363","DOIUrl":"10.1002/jssc.70363","url":null,"abstract":"<div>\u0000 \u0000 <p>In the present work, nickel sulfide (Ni<sub>3</sub>S<sub>2</sub>) was modified on the surface of Ni foams (NiF) by in-situ growth, and the prepared rambutan-like Ni<sub>3</sub>S<sub>2</sub>/NiF materials were further decorated with carbon nanospheres. Subsequently, the prepared C/Ni<sub>3</sub>S<sub>2</sub>/NiF was loaded into a syringe filter and used for syringe membrane filter-based solid-phase microextraction (SMF-SPME) of five nitroimidazoles (NDZs), followed by high-performance liquid chromatography-ultraviolet detection. The metal affinity of divalent Ni (II) and the imidazole group could contribute to the selective adsorption to NDZs, and the structural porous support of Ni foams, the in-situ modified Ni<sub>3</sub>S<sub>2</sub>, and carbon nanospheres facilitated the improvement of SMF-SPME efficiency. The main experimental parameters affecting the extraction efficiency were studied, including sample flow rate, adsorption cycle, salt concentration, pH of sample solution, the type and volume of desorption solvent. The selectivity of the adsorbent membrane C/Ni<sub>3</sub>S<sub>2</sub>/NiF to NDZs was evaluated, and the interactions existing between the modified materials on Ni foam and NDZs were examined to probe the possible adsorption mechanism. Under the optimal conditions, the proposed method showed good linearity from 0.05 to 200 µg L<sup>−1</sup> and possessed low limits of detection within 0.01–0.05 µg L<sup>−1</sup>. The reproducibility and reusability of the C/Ni<sub>3</sub>S<sub>2</sub>/NiF adsorbent were investigated, and the effective enrichment and determination of NDZs in water, milk, and honey samples were also carried out with recoveries of 79.3%–114.5%. This study provides a new strategy for the enrichment and determination of some NDZs in different samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2026-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146113404","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Selective Adsorption Behavior of Gallium Ions on Graphene-Based Surface Ion-Imprinted Material From Simulated Acid Leach Solution of Fly Ash 模拟粉煤灰酸浸液中石墨烯基表面离子印迹材料对镓离子的选择性吸附行为
IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2026-02-03 DOI: 10.1002/jssc.70362
Bingbing Liu, Manman Zhang, Mingyang Chen, Lei Qin, Meiling Wang, Dongju Fu, Weifeng Liu, Xuguang Liu

A graphene-based material for the selective adsorption of gallium ions has been prepared by combining ion-imprinting technology with adsorption. This material is capable of separating and extracting gallium ions from the acid leachate of fly ash. Morphological and structural characterization of the material was performed using scanning electron microscopy and Fourier-transform infrared spectroscopy, which confirmed that the material possesses a three-dimensional structure and that functional monomers have successfully complexed with graphene oxide substrates. The maximum adsorption capacity of the material reaches 86.29 mg/g at a solution pH of 3. In the selective adsorption tests, the selective separation factors of gallium ions relative to aluminum, magnesium, iron, and calcium ions were 16.50, 49.50, 9.90, and 99.00, respectively. Meanwhile, the material maintained excellent adsorption capacity and structural stability in cyclic regeneration experiments, with no obvious dissolution loss observed. The adsorption mechanism of the material was analyzed via X-ray photoelectron spectroscopy, and the results indicated that it primarily involves cation exchange between carboxyl groups and gallium ions. This work demonstrates that the three-dimensional ion-imprinted hydrogel adsorbent plays a significant role in the selective adsorption of gallium ions and the subsequent solid-liquid separation.

将离子印迹技术与吸附技术相结合,制备了一种选择性吸附镓离子的石墨烯基材料。该材料具有从粉煤灰酸性渗滤液中分离提取镓离子的能力。利用扫描电子显微镜和傅里叶变换红外光谱对材料进行了形态和结构表征,证实了材料具有三维结构,功能单体与氧化石墨烯衬底成功络合。在溶液pH = 3时,材料的最大吸附量达到86.29 mg/g。在选择性吸附试验中,镓离子相对于铝、镁、铁和钙离子的选择性分离系数分别为16.50、49.50、9.90和99.00。同时,在循环再生实验中,材料保持了良好的吸附能力和结构稳定性,无明显的溶解损失。通过x射线光电子能谱分析了材料的吸附机理,结果表明其主要涉及羧基与镓离子之间的阳离子交换。这项工作证明了三维离子印迹水凝胶吸附剂在镓离子的选择性吸附和随后的固液分离中起着重要的作用。
{"title":"Selective Adsorption Behavior of Gallium Ions on Graphene-Based Surface Ion-Imprinted Material From Simulated Acid Leach Solution of Fly Ash","authors":"Bingbing Liu,&nbsp;Manman Zhang,&nbsp;Mingyang Chen,&nbsp;Lei Qin,&nbsp;Meiling Wang,&nbsp;Dongju Fu,&nbsp;Weifeng Liu,&nbsp;Xuguang Liu","doi":"10.1002/jssc.70362","DOIUrl":"10.1002/jssc.70362","url":null,"abstract":"<div>\u0000 \u0000 <p>A graphene-based material for the selective adsorption of gallium ions has been prepared by combining ion-imprinting technology with adsorption. This material is capable of separating and extracting gallium ions from the acid leachate of fly ash. Morphological and structural characterization of the material was performed using scanning electron microscopy and Fourier-transform infrared spectroscopy, which confirmed that the material possesses a three-dimensional structure and that functional monomers have successfully complexed with graphene oxide substrates. The maximum adsorption capacity of the material reaches 86.29 mg/g at a solution pH of 3. In the selective adsorption tests, the selective separation factors of gallium ions relative to aluminum, magnesium, iron, and calcium ions were 16.50, 49.50, 9.90, and 99.00, respectively. Meanwhile, the material maintained excellent adsorption capacity and structural stability in cyclic regeneration experiments, with no obvious dissolution loss observed. The adsorption mechanism of the material was analyzed via X-ray photoelectron spectroscopy, and the results indicated that it primarily involves cation exchange between carboxyl groups and gallium ions. This work demonstrates that the three-dimensional ion-imprinted hydrogel adsorbent plays a significant role in the selective adsorption of gallium ions and the subsequent solid-liquid separation.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2026-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146113356","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Supercritical Carbon Dioxide Extraction With Dimethyl Carbonate and Bio-Ethanol as Co-Solvents for the Determination of Pesticide Residues in Black Pepper by Low-Pressure Gas Chromatography-Triple Quadrupole Mass Spectrometry. 碳酸二甲酯和生物乙醇为助溶剂超临界二氧化碳萃取法测定黑胡椒中农药残留
IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2026-02-01 DOI: 10.1002/jssc.70368
Alessia Arena, Mariosimone Zoccali, Luigi Mondello

The determination of pesticide residues in spices is analytically challenging due to their high content of essential oils and secondary metabolites that could interfere with detection and quantification. In this study, supercritical fluid extraction (SFE), using green co-solvents, was evaluated for the extraction of 44 pesticides from black pepper (Piper nigrum). The extraction performance of bio-ethanol (bio-EtOH) and dimethyl carbonate (DMC) was compared under mild operating conditions. Optimal recoveries were obtained with 10% DMC, yielding an average of 92.6% across 44 pesticides, comparable to 93.7% using bio-EtOH. Method performance was assessed by low-pressure gas chromatography-triple quadrupole mass spectrometry (LP-GC-QqQMS). Linearity was achieved over the tested range, with limits of detection (within the range 0.1-17.9 µg kg-1) and quantification (within the range 0.3-59.8 µg kg-1) always below European Union (EU) maximum residue levels (MRLs). Accuracy ranged from 74.4% to 107.7%, with intra-day precision between 0.8% and 16.1%. A pronounced matrix effect was observed (average ionization suppression: -47.6%). The application of the validated method to commercial black pepper samples revealed the presence of diphenylamine, quinalphos, and phosalone, with only quinalphos exceeding EU MRLs. These findings demonstrate that SFE with DMC as a co-solvent provides an efficient, greener, and reliable extraction approach for multi-residue pesticide analysis in a complex spice matrix. The combination of SFE with LP-GC-QqQMS supports the implementation of greener and high-throughput monitoring workflows for complex spice matrices.

由于香料中含有大量的精油和次生代谢物,可能会干扰检测和定量,因此农药残留的测定在分析上具有挑战性。采用绿色助溶剂超临界流体萃取法对黑胡椒中44种农药进行了提取。比较了生物乙醇(bio-EtOH)和碳酸二甲酯(DMC)在温和操作条件下的提取性能。当DMC用量为10%时,44种农药的平均回收率为92.6%,生物乙醇回收率为93.7%。采用低压气相色谱-三重四极杆质谱(LP-GC-QqQMS)评价方法的性能。在测试范围内实现线性,检测限(0.1-17.9µg kg-1范围内)和定量限(0.3-59.8µg kg-1范围内)始终低于欧盟(EU)最大残留限量(MRLs)。准确度在74.4% ~ 107.7%之间,日内准确度在0.8% ~ 16.1%之间。观察到明显的基质效应(平均电离抑制:-47.6%)。经验证的方法在商业黑胡椒样品中的应用显示,二苯胺、醌和膦酮的存在,只有醌超过欧盟MRLs。这些结果表明,以DMC为助溶剂的SFE提取方法为复杂香料基质中多残留农药的分析提供了一种高效、环保、可靠的方法。SFE与LP-GC-QqQMS的结合支持对复杂香料矩阵实施更环保和高通量的监测工作流程。
{"title":"Supercritical Carbon Dioxide Extraction With Dimethyl Carbonate and Bio-Ethanol as Co-Solvents for the Determination of Pesticide Residues in Black Pepper by Low-Pressure Gas Chromatography-Triple Quadrupole Mass Spectrometry.","authors":"Alessia Arena, Mariosimone Zoccali, Luigi Mondello","doi":"10.1002/jssc.70368","DOIUrl":"10.1002/jssc.70368","url":null,"abstract":"<p><p>The determination of pesticide residues in spices is analytically challenging due to their high content of essential oils and secondary metabolites that could interfere with detection and quantification. In this study, supercritical fluid extraction (SFE), using green co-solvents, was evaluated for the extraction of 44 pesticides from black pepper (Piper nigrum). The extraction performance of bio-ethanol (bio-EtOH) and dimethyl carbonate (DMC) was compared under mild operating conditions. Optimal recoveries were obtained with 10% DMC, yielding an average of 92.6% across 44 pesticides, comparable to 93.7% using bio-EtOH. Method performance was assessed by low-pressure gas chromatography-triple quadrupole mass spectrometry (LP-GC-QqQMS). Linearity was achieved over the tested range, with limits of detection (within the range 0.1-17.9 µg kg<sup>-1</sup>) and quantification (within the range 0.3-59.8 µg kg<sup>-1</sup>) always below European Union (EU) maximum residue levels (MRLs). Accuracy ranged from 74.4% to 107.7%, with intra-day precision between 0.8% and 16.1%. A pronounced matrix effect was observed (average ionization suppression: -47.6%). The application of the validated method to commercial black pepper samples revealed the presence of diphenylamine, quinalphos, and phosalone, with only quinalphos exceeding EU MRLs. These findings demonstrate that SFE with DMC as a co-solvent provides an efficient, greener, and reliable extraction approach for multi-residue pesticide analysis in a complex spice matrix. The combination of SFE with LP-GC-QqQMS supports the implementation of greener and high-throughput monitoring workflows for complex spice matrices.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 2","pages":"e70368"},"PeriodicalIF":2.8,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12883146/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146142754","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Microscale Affinity Chromatography for Biointeraction Analysis: Strategies, Principles and Applications. 用于生物相互作用分析的微尺度亲和色谱:策略、原理和应用。
IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2026-02-01 DOI: 10.1002/jssc.70361
David S Hage, Nigar Sultana Pinky, B K Sajeeb, Md Masudur Rahman, Harshana Olupathage, Samiul Alim, Isaac Kyei, Zoe Zingler, Sanduni Heenkenda

The analysis of interactions between biological agents or with surrounding chemicals is important in many areas of modern biochemical, biomedical, and environmental research. Microscale platforms based on affinity chromatography have been shown to be a powerful set of tools for these studies. This approach makes use of an immobilized binding agent as a stationary phase in a microscale platform for either direct examination of the interactions of this agent with an applied target solute or as a secondary capture agent to probe a solution-phase interaction. This review will examine the various platforms and strategies that have been used in microscale affinity chromatography, or µAC, to characterize and study biointeractions. The general principles of µAC and schemes based on this approach will be examined, along with applications of this technique. Examples of approaches that will be considered will include zonal and frontal analysis methods, as well as a variety of schemes by which µAC can be employed in kinetic studies. In each case, the theory and principles of these methods will be provided along with examples of their use in biointeraction studies.

分析生物制剂之间或与周围化学物质的相互作用在现代生化、生物医学和环境研究的许多领域都很重要。基于亲和色谱的微尺度平台已被证明是这些研究的一套强大的工具。该方法利用固定化结合剂作为微尺度平台中的固定相,用于直接检测该结合剂与应用的目标溶质的相互作用,或作为二级捕获剂来探测溶液相相互作用。这篇综述将检查各种平台和策略,已用于微尺度亲和色谱,或µAC,表征和研究生物相互作用。µAC的一般原理和基于这种方法的方案将被检查,以及该技术的应用。将考虑的方法示例将包括区域和锋面分析方法,以及各种方案,其中µAC可用于动力学研究。在每种情况下,这些方法的理论和原理将与它们在生物相互作用研究中的应用实例一起提供。
{"title":"Microscale Affinity Chromatography for Biointeraction Analysis: Strategies, Principles and Applications.","authors":"David S Hage, Nigar Sultana Pinky, B K Sajeeb, Md Masudur Rahman, Harshana Olupathage, Samiul Alim, Isaac Kyei, Zoe Zingler, Sanduni Heenkenda","doi":"10.1002/jssc.70361","DOIUrl":"10.1002/jssc.70361","url":null,"abstract":"<p><p>The analysis of interactions between biological agents or with surrounding chemicals is important in many areas of modern biochemical, biomedical, and environmental research. Microscale platforms based on affinity chromatography have been shown to be a powerful set of tools for these studies. This approach makes use of an immobilized binding agent as a stationary phase in a microscale platform for either direct examination of the interactions of this agent with an applied target solute or as a secondary capture agent to probe a solution-phase interaction. This review will examine the various platforms and strategies that have been used in microscale affinity chromatography, or µAC, to characterize and study biointeractions. The general principles of µAC and schemes based on this approach will be examined, along with applications of this technique. Examples of approaches that will be considered will include zonal and frontal analysis methods, as well as a variety of schemes by which µAC can be employed in kinetic studies. In each case, the theory and principles of these methods will be provided along with examples of their use in biointeraction studies.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 2","pages":"e70361"},"PeriodicalIF":2.8,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12883148/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146142775","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Rational Design of Functional Metal-Organic Frameworks as Chromatographic Stationary Phases: From Synthesis to Advanced Applications. 功能金属-有机骨架色谱固定相的合理设计:从合成到高级应用。
IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2026-02-01 DOI: 10.1002/jssc.70369
Yan Ma, Yang Zhou, Danqin Li, Jiaping Cui, Xiangyu Ma, Qifeng Fu

Metal-organic frameworks (MOFs) have emerged as highly promising stationary phases in chromatographic separation technologies due to their exceptional structural tunability, high surface areas, and tailored pore environments. However, the transformation of these intrinsic advantages into practical chromatographic performance is often hindered by kinetic mass-transfer limitations, hydrolytic instability, and restricted accessibility for bulky analytes. This review systematically summarizes recent advances in the design and application of MOFs for chromatography, focusing on three critical material development directions: nano-sized MOFs, highly stable MOFs, and hierarchically porous MOFs. We first summarize the synthesis strategies, scientific challenges, and representative breakthroughs for each category, highlighting the transition between material properties and performance. The subsequent discussion critically evaluates their applications in gas chromatography (GC), liquid chromatography (HPLC), and capillary electrochromatography (CEC), with a particular focus on structure-performance relationships and the realization of material stability and nanoscale effects into enhanced separation efficiency, selectivity, and operational lifetime. By bridging the gap between advanced material synthesis and practical separation needs, this review aims to provide a roadmap for the development of next-generation and high-efficiency MOF-based stationary phases.

金属有机骨架(mof)由于其特殊的结构可调节性、高表面积和可定制的孔隙环境,已成为色谱分离技术中非常有前途的固定相。然而,将这些固有优势转化为实际色谱性能常常受到动力学传质限制、水解不稳定性和大体积分析物受限的阻碍。本文系统总结了近年来用于色谱的mof材料的设计和应用进展,重点介绍了纳米mof材料、高稳定mof材料和分层多孔mof材料的三个关键发展方向。我们首先总结了每个类别的合成策略、科学挑战和具有代表性的突破,重点介绍了材料性能和性能之间的过渡。随后的讨论批判性地评估了它们在气相色谱(GC),液相色谱(HPLC)和毛细管电色谱(CEC)中的应用,特别关注结构-性能关系以及材料稳定性和纳米级效应的实现,以提高分离效率,选择性和使用寿命。通过弥合先进材料合成与实际分离需求之间的差距,本文旨在为下一代高效mof基固定相的发展提供路线图。
{"title":"Rational Design of Functional Metal-Organic Frameworks as Chromatographic Stationary Phases: From Synthesis to Advanced Applications.","authors":"Yan Ma, Yang Zhou, Danqin Li, Jiaping Cui, Xiangyu Ma, Qifeng Fu","doi":"10.1002/jssc.70369","DOIUrl":"https://doi.org/10.1002/jssc.70369","url":null,"abstract":"<p><p>Metal-organic frameworks (MOFs) have emerged as highly promising stationary phases in chromatographic separation technologies due to their exceptional structural tunability, high surface areas, and tailored pore environments. However, the transformation of these intrinsic advantages into practical chromatographic performance is often hindered by kinetic mass-transfer limitations, hydrolytic instability, and restricted accessibility for bulky analytes. This review systematically summarizes recent advances in the design and application of MOFs for chromatography, focusing on three critical material development directions: nano-sized MOFs, highly stable MOFs, and hierarchically porous MOFs. We first summarize the synthesis strategies, scientific challenges, and representative breakthroughs for each category, highlighting the transition between material properties and performance. The subsequent discussion critically evaluates their applications in gas chromatography (GC), liquid chromatography (HPLC), and capillary electrochromatography (CEC), with a particular focus on structure-performance relationships and the realization of material stability and nanoscale effects into enhanced separation efficiency, selectivity, and operational lifetime. By bridging the gap between advanced material synthesis and practical separation needs, this review aims to provide a roadmap for the development of next-generation and high-efficiency MOF-based stationary phases.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 2","pages":"e70369"},"PeriodicalIF":2.8,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146142769","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Screening Potential Anti-Respiratory Syncytial Virus Substances From Forsythia suspensa Using a High-Expressing Fusion Protein Cell Membrane Chromatography 利用高表达融合蛋白膜层析技术筛选连翘中抗呼吸道合胞病毒物质。
IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-23 DOI: 10.1002/jssc.70344
Yongli Liu, Chang Gao, Shiyu Li, Jie Gao, Nan Wang

Respiratory syncytial virus (RSV) imposes a substantial health burden, particularly among pediatric and elderly populations. The RSV fusion (F) protein, a critical mediator of viral entry and syncytium formation, represents a promising and rational target for antiviral drug development. Forsythia suspensa (Lianqiao in Chinese), a traditional Chinese medicinal herb, has been empirically employed for decades in the prevention of viral infections; however, its pharmacologically active constituents remain poorly characterized. The present investigation developed a high-expression F protein cell membrane chromatography system, and integrated with UHPLC-MS, to screen pharmacological substances from FS and verified the anti-viral potential against RSV in vivo. Our study pinpointed Forsythoside A, Forsythoside B, Phillygenin, and Phillyrin as potential anti-RSV compounds in FS. The research findings suggest that Forsythoside A, Forsythoside B, and Phillygenin exhibit considerable suppressive effects on cell fusion induced by RSV, concurrently effectively diminishing the expression level of the F protein gene. In contrast, the inhibitory impact of Phillyrin seems relatively less potent. In conclusion, our findings provide a convenient, fast, and accurate method to screen potential anti-RSV ingredients in natural herbal medicines. These results may facilitate the development of RSV treatment.

呼吸道合胞病毒(RSV)造成了巨大的健康负担,特别是在儿科和老年人人群中。RSV融合(F)蛋白是病毒进入和合胞体形成的关键介质,是抗病毒药物开发的一个有希望和合理的靶标。连翘(连翘)是一种传统的中草药,几十年来一直被用于预防病毒感染;然而,其药理活性成分的特征仍然很差。本研究建立了高表达F蛋白细胞膜层析系统,并结合超高效液相色谱-质谱联用,从FS中筛选药理学物质,验证其对RSV的体内抗病毒潜力。我们的研究确定了连翘苷A、连翘苷B、连翘苷元和连翘苷是FS中潜在的抗rsv化合物。研究结果表明,连翘苷A、连翘苷B和连翘苷元对RSV诱导的细胞融合具有明显的抑制作用,同时有效降低F蛋白基因的表达水平。相比之下,philyrin的抑制作用似乎相对较弱。总之,本研究结果为筛选天然草药中潜在的抗rsv成分提供了一种方便、快速、准确的方法。这些结果可能促进RSV治疗的发展。
{"title":"Screening Potential Anti-Respiratory Syncytial Virus Substances From Forsythia suspensa Using a High-Expressing Fusion Protein Cell Membrane Chromatography","authors":"Yongli Liu,&nbsp;Chang Gao,&nbsp;Shiyu Li,&nbsp;Jie Gao,&nbsp;Nan Wang","doi":"10.1002/jssc.70344","DOIUrl":"10.1002/jssc.70344","url":null,"abstract":"<div>\u0000 \u0000 <p>Respiratory syncytial virus (RSV) imposes a substantial health burden, particularly among pediatric and elderly populations. The RSV fusion (F) protein, a critical mediator of viral entry and syncytium formation, represents a promising and rational target for antiviral drug development. <i>Forsythia suspensa</i> (Lianqiao in Chinese), a traditional Chinese medicinal herb, has been empirically employed for decades in the prevention of viral infections; however, its pharmacologically active constituents remain poorly characterized. The present investigation developed a high-expression F protein cell membrane chromatography system, and integrated with UHPLC-MS, to screen pharmacological substances from FS and verified the anti-viral potential against RSV in vivo. Our study pinpointed Forsythoside A, Forsythoside B, Phillygenin, and Phillyrin as potential anti-RSV compounds in FS. The research findings suggest that Forsythoside A, Forsythoside B, and Phillygenin exhibit considerable suppressive effects on cell fusion induced by RSV, concurrently effectively diminishing the expression level of the F protein gene. In contrast, the inhibitory impact of Phillyrin seems relatively less potent. In conclusion, our findings provide a convenient, fast, and accurate method to screen potential anti-RSV ingredients in natural herbal medicines. These results may facilitate the development of RSV treatment.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 1","pages":""},"PeriodicalIF":2.8,"publicationDate":"2026-01-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146041190","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Prediction of Thermal Modulated Comprehensive Two-Dimensional Gas Chromatographic Separation Using a Modular, Graph-Based Simulation Platform 基于模块化图形模拟平台的热调制综合二维气相色谱分离预测。
IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-21 DOI: 10.1002/jssc.70351
Jan Leppert, Tillman Brehmer, Matthias Wüst

Comprehensive two-dimensional gas chromatography (GC×GC) offers exceptional separation performance, but method development remains time-consuming and sensitive to numerous system parameters. In this study, we present a modular simulation framework for GC×GC systems with thermal modulation, implemented in the open-source Julia package GasChromatographySystems.jl. The simulation is based on a graph-based abstraction of the GC system and models solute migration through column and modulator modules using previously established retention models. A simplified but effective model for thermal modulation enables the generation of realistic two-dimensional retention times and peak widths. Simulation results were validated against experimental measurements from a GC×GC-ToF-MS system using different modulation periods and temperature programs. Systematic deviations between simulated and measured retention times could be explained and corrected by adjusting parameters such as the actual modulation period and modulator shift. The final model achieved root mean squared error (rmse${mathrm{rmse}}$) of below 15 s (less than 1%) for first-dimension retention times and 55 ms (8%) for the second dimension. Peak width predictions were less accurate, with deviations of up to 3 s (40%) in the first dimension and up to 40 ms (60%) in the second. This modular and adaptable simulation framework provides a robust foundation for future applications in automated method development and system diagnostics in multidimensional gas chromatography.

全面的二维气相色谱(GC×GC)提供了卓越的分离性能,但方法开发仍然耗时和敏感的众多系统参数。在这项研究中,我们提出了一个具有热调制的GC×GC系统的模块化模拟框架,在开源的Julia包GasChromatographySystems.jl中实现。模拟是基于GC系统的基于图形的抽象,并使用先前建立的保留模型模拟溶质通过柱和调制器模块的迁移。一个简化但有效的热调制模型能够生成真实的二维保留时间和峰宽。采用不同的调制周期和温度程序对GC×GC-ToF-MS系统的实验测量结果进行了仿真验证。模拟和测量的保持时间之间的系统偏差可以通过调整实际调制周期和调制器位移等参数来解释和纠正。最终模型实现了第一维保留时间的均方根误差(rmse ${mathrm{rmse}}$)小于15秒(小于1%),第二维保留时间的均方根误差为55毫秒(8%)。峰宽预测不太准确,在第一个维度上偏差高达3秒(40%),在第二个维度上偏差高达40毫秒(60%)。这种模块化和适应性强的模拟框架为未来在多维气相色谱自动化方法开发和系统诊断中的应用提供了坚实的基础。
{"title":"Prediction of Thermal Modulated Comprehensive Two-Dimensional Gas Chromatographic Separation Using a Modular, Graph-Based Simulation Platform","authors":"Jan Leppert,&nbsp;Tillman Brehmer,&nbsp;Matthias Wüst","doi":"10.1002/jssc.70351","DOIUrl":"10.1002/jssc.70351","url":null,"abstract":"<p>Comprehensive two-dimensional gas chromatography (GC×GC) offers exceptional separation performance, but method development remains time-consuming and sensitive to numerous system parameters. In this study, we present a modular simulation framework for GC×GC systems with thermal modulation, implemented in the open-source Julia package GasChromatographySystems.jl. The simulation is based on a graph-based abstraction of the GC system and models solute migration through column and modulator modules using previously established retention models. A simplified but effective model for thermal modulation enables the generation of realistic two-dimensional retention times and peak widths. Simulation results were validated against experimental measurements from a GC×GC-ToF-MS system using different modulation periods and temperature programs. Systematic deviations between simulated and measured retention times could be explained and corrected by adjusting parameters such as the actual modulation period and modulator shift. The final model achieved root mean squared error (<span></span><math>\u0000 <semantics>\u0000 <mi>rmse</mi>\u0000 <annotation>${mathrm{rmse}}$</annotation>\u0000 </semantics></math>) of below 15 s (less than 1%) for first-dimension retention times and 55 ms (8%) for the second dimension. Peak width predictions were less accurate, with deviations of up to 3 s (40%) in the first dimension and up to 40 ms (60%) in the second. This modular and adaptable simulation framework provides a robust foundation for future applications in automated method development and system diagnostics in multidimensional gas chromatography.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 1","pages":""},"PeriodicalIF":2.8,"publicationDate":"2026-01-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12824439/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146018609","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Combining Fractionation and High-Resolution Mass Spectrometry Approaches to Characterize a Bio-Oil From Flax Shive Pyrolysis 结合分馏和高分辨率质谱方法表征亚麻籽裂解的生物油。
IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-21 DOI: 10.1002/jssc.70354
Théo Imhoff, Jason Devaux, Estelle Deschamps, Juliette Vievard, Pedro F. Brandão, Carlos Afonso, Regina M. B. O. Duarte, Mélanie Mignot

In a context where environmental concerns and circular economy drive innovation, co-products from the flax industry emerge as valuable lignocellulosic feedstocks. Pyrolysis of these biomasses generates bio-oils with complex and highly oxygenated composition, which requires in-depth molecular characterization to optimize valorization processes. This study focuses on the molecular-level characterization of bio-oil derived from flax shives, a local co-product in Normandy. Size-exclusion chromatography (SEC) was used to fractionate the bio-oil into five distinct fractions based on apparent molecular size. The complete bio-oil and each SEC fraction were then analyzed by high-resolution mass spectrometry (Fourier-transform ion cyclotron resonance [FT-ICR MS] and Orbitrap MS) to identify and compare thousands of molecular formulae. A custom Python-based workflow was developed to align and annotate Orbitrap MS data using the FT-ICR MS dataset as a reference, allowing for rapid molecular formula assignment. Chemical class distribution, oxygen content, and Van Krevelen analysis revealed specific trends across fractions, indicating that SEC separation was influenced not only by molecular size but also by polarity and structural interactions. This approach offers a refined strategy for exploring the chemical complexity of lignocellulosic bio-oils and supports future efforts in their upgrading and application.

在环境问题和循环经济推动创新的背景下,亚麻工业的副产品成为有价值的木质纤维素原料。这些生物质热解生成具有复杂和高氧成分的生物油,这需要深入的分子表征来优化增值过程。本研究的重点是从诺曼底当地的副产品亚麻片中提取的生物油的分子水平表征。采用排粒径色谱法(SEC)根据表观分子大小将生物油分离成5个不同的组分。然后通过高分辨率质谱分析(傅里叶变换离子回旋共振[FT-ICR MS]和Orbitrap MS)对完整的生物油和每个SEC部分进行分析,以识别和比较数千种分子式。开发了基于python的定制工作流程,以FT-ICR质谱数据集为参考,对Orbitrap质谱数据进行对齐和注释,从而实现快速分子式分配。化学类分布、氧含量和Van Krevelen分析揭示了不同组分的特定趋势,表明SEC分离不仅受分子大小的影响,还受极性和结构相互作用的影响。这种方法为探索木质纤维素生物油的化学复杂性提供了一种精细的策略,并支持其升级和应用的未来努力。
{"title":"Combining Fractionation and High-Resolution Mass Spectrometry Approaches to Characterize a Bio-Oil From Flax Shive Pyrolysis","authors":"Théo Imhoff,&nbsp;Jason Devaux,&nbsp;Estelle Deschamps,&nbsp;Juliette Vievard,&nbsp;Pedro F. Brandão,&nbsp;Carlos Afonso,&nbsp;Regina M. B. O. Duarte,&nbsp;Mélanie Mignot","doi":"10.1002/jssc.70354","DOIUrl":"10.1002/jssc.70354","url":null,"abstract":"<div>\u0000 \u0000 <p>In a context where environmental concerns and circular economy drive innovation, co-products from the flax industry emerge as valuable lignocellulosic feedstocks. Pyrolysis of these biomasses generates bio-oils with complex and highly oxygenated composition, which requires in-depth molecular characterization to optimize valorization processes. This study focuses on the molecular-level characterization of bio-oil derived from flax shives, a local co-product in Normandy. Size-exclusion chromatography (SEC) was used to fractionate the bio-oil into five distinct fractions based on apparent molecular size. The complete bio-oil and each SEC fraction were then analyzed by high-resolution mass spectrometry (Fourier-transform ion cyclotron resonance [FT-ICR MS] and Orbitrap MS) to identify and compare thousands of molecular formulae. A custom Python-based workflow was developed to align and annotate Orbitrap MS data using the FT-ICR MS dataset as a reference, allowing for rapid molecular formula assignment. Chemical class distribution, oxygen content, and Van Krevelen analysis revealed specific trends across fractions, indicating that SEC separation was influenced not only by molecular size but also by polarity and structural interactions. This approach offers a refined strategy for exploring the chemical complexity of lignocellulosic bio-oils and supports future efforts in their upgrading and application.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 1","pages":""},"PeriodicalIF":2.8,"publicationDate":"2026-01-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146018544","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
HPLC Chiral Separation and Elution Reversal Mechanism of a Typical Light-Driven Molecular Motor, 1-(9H-Fluoren-9-Ylidene)-2,3-Dihydro-2-Methyl-1H-Benz[e]Indene 典型光驱动分子马达-1 -(9h -芴-9-吡啶)-2,3-二氢-2-甲基- 1h - benz [e]茚酮的HPLC手性分离与洗脱反转机理
IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-21 DOI: 10.1002/jssc.70355
Wen-long Zhang, Xin-yi Huang, Can Xia, Min-jin Xu, Wei-guang Zhang, Jian Sun, Ru-jian He, Jun Fan

1-(9H-Fluoren-9-ylidene)-2,3-dihydro-2-methyl-1H-benz[e]indene (short as FMB) as one of second-generation light-driven molecular motors contains a chiral carbon atom, and has attracted considerable attentions due to macroscopic chiral structures and light-driven behaviors through supramolecular assembly and cooperative effects. Herein, chiral analysis and semi-preparative separation of FMB enantiomers have been studied by high-performance liquid chromatography (HPLC) on polysaccharide-derived chiral stationary phases (CSPs). Effects of factors on chiral separation of FMB enantiomers, including type of CSP, composition and ratio of mobile phase, temperature, and flow rate, have been discussed in detail. Best separation of racemic FMB was achieved on cellulose tri(3,5-dimethylphenylcarbamate)-coated CSP with the resolution of 2.50 using the hexane–ethanol mixture (99:1, v/v). Then, each FMB enantiomer was obtained through semi-preparative separation with enantiomeric purity over 99%, and their absolute configurations as well as elution order were determined by electronic circular dichroism spectroscopy. Surprisingly, elution reversal phenomenon of FMB enantiomers was observed on cellulose- and amylose- tri(3,5-dimethylphenyl carbamate)-coated CSPs, in which (S)-FMB was eluted first on cellulose tri(3,5-dimethylphenylcarbamate)-coated CSP, and (R)-enantiomer was eluted first on the other. Moreover, molecular docking simulation has been employed to explain the recognition mechanism and elution reversal of FMB enantiomers on these two CSPs. The docking results revealed that π–π stacks, π–lone pair interactions, π– σ, and π–alkyl interactions between FMB and CSPs were the primary forces driving chiral separation, and the differences between them led to the enantiomer elution reversal on these two CSPs. Briefly, this work would provide valuable information for the separation and elution mechanisms of chiral molecular motors on polysaccharide-based CSPs.

1-(9h -芴-9-吡啶)-2,3-二氢-2-甲基- 1h -苯并[e]烯(简称FMB)作为第二代光驱动分子马达之一,含有一个手性碳原子,由于其宏观手性结构和通过超分子组装和协同效应实现的光驱动行为而备受关注。本研究采用高效液相色谱法(HPLC)在多糖源性手性固定相(CSPs)上对FMB对映体进行了手性分析和半制备分离。详细讨论了CSP类型、流动相组成及配比、温度、流速等因素对FMB对映体手性分离的影响。在正己烷-乙醇混合物(99:1,v/v)的条件下,三(3,5-二甲基苯基氨基甲酸酯)包被CSP对外消旋FMB的分离效果最好,分离分辨率为2.50。然后,通过半制备分离得到每个FMB对映体,对映体纯度大于99%,并通过电子圆二色光谱确定它们的绝对构型和洗脱顺序。令人惊讶的是,在纤维素-和直链淀粉-三(3,5-二甲基苯基氨基甲酸酯)包被的CSP上观察到FMB对映体的洗脱反转现象,其中(S)-FMB在三(3,5-二甲基苯基氨基甲酸酯)包被的CSP上首先被洗脱,(R)-对映体在另一个CSP上首先被洗脱。此外,利用分子对接模拟解释了FMB对映体在这两种csp上的识别机制和洗脱反转。对接结果表明,FMB和csp之间的π-π堆积、π-孤对相互作用、π- σ和π-烷基相互作用是手性分离的主要驱动力,它们之间的差异导致了这两种csp的对映体洗脱逆转。简要地说,这项工作将为手性分子马达在多糖基csp上的分离和洗脱机制提供有价值的信息。
{"title":"HPLC Chiral Separation and Elution Reversal Mechanism of a Typical Light-Driven Molecular Motor, 1-(9H-Fluoren-9-Ylidene)-2,3-Dihydro-2-Methyl-1H-Benz[e]Indene","authors":"Wen-long Zhang,&nbsp;Xin-yi Huang,&nbsp;Can Xia,&nbsp;Min-jin Xu,&nbsp;Wei-guang Zhang,&nbsp;Jian Sun,&nbsp;Ru-jian He,&nbsp;Jun Fan","doi":"10.1002/jssc.70355","DOIUrl":"10.1002/jssc.70355","url":null,"abstract":"<div>\u0000 \u0000 <p>1-(9H-Fluoren-9-ylidene)-2,3-dihydro-2-methyl-1H-benz[e]indene (short as FMB) as one of second-generation light-driven molecular motors contains a chiral carbon atom, and has attracted considerable attentions due to macroscopic chiral structures and light-driven behaviors through supramolecular assembly and cooperative effects. Herein, chiral analysis and semi-preparative separation of FMB enantiomers have been studied by high-performance liquid chromatography (HPLC) on polysaccharide-derived chiral stationary phases (CSPs). Effects of factors on chiral separation of FMB enantiomers, including type of CSP, composition and ratio of mobile phase, temperature, and flow rate, have been discussed in detail. Best separation of racemic FMB was achieved on cellulose tri(3,5-dimethylphenylcarbamate)-coated CSP with the resolution of 2.50 using the hexane–ethanol mixture (99:1, v/v). Then, each FMB enantiomer was obtained through semi-preparative separation with enantiomeric purity over 99%, and their absolute configurations as well as elution order were determined by electronic circular dichroism spectroscopy. Surprisingly, elution reversal phenomenon of FMB enantiomers was observed on cellulose- and amylose- tri(3,5-dimethylphenyl carbamate)-coated CSPs, in which (<i>S</i>)-FMB was eluted first on cellulose tri(3,5-dimethylphenylcarbamate)-coated CSP, and (<i>R</i>)-enantiomer was eluted first on the other. Moreover, molecular docking simulation has been employed to explain the recognition mechanism and elution reversal of FMB enantiomers on these two CSPs. The docking results revealed that π–π stacks, π–lone pair interactions, π– σ, and π–alkyl interactions between FMB and CSPs were the primary forces driving chiral separation, and the differences between them led to the enantiomer elution reversal on these two CSPs. Briefly, this work would provide valuable information for the separation and elution mechanisms of chiral molecular motors on polysaccharide-based CSPs.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 1","pages":""},"PeriodicalIF":2.8,"publicationDate":"2026-01-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146018564","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Impact of Column Load and Signal-to-Noise Threshold on the Accuracy and Repeatability of Jet A Hydrocarbon Profiling via GC×GC/FID 柱载和信噪比阈值对GC×GC/FID射流A烃谱分析精度和可重复性的影响
IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-21 DOI: 10.1002/jssc.70356
Brent A. Modereger, Louis Edwards Caceres-Martinez, Michael E. Peretich, Hilkka I. Kenttämaa, Gozdem Kilaz

Comprehensive two-dimensional gas chromatography with flame ionization detection (GC×GC/FID) is a powerful technique for quantifying hydrocarbons in jet fuel. However, factors such as column load and the signal-to-noise (S/N) ratio threshold used for peak inclusion can significantly influence the accuracy and repeatability of hydrocarbon composition measurements. Despite their importance, the effects of these parameters have not been systematically studied. Accurate and precise quantitation of individual hydrocarbon groups (e.g., C7 isoalkanes) is particularly critical, as specific jet fuel properties, such as flash point, freezing point, and kinematic viscosity, are highly dependent on the concentrations of specific hydrocarbon classes. In this study, we investigated the influence of column load (0.05 vs. 2.5 nL) and S/N threshold (0–150) on the measured hydrocarbon composition of Jet A fuel using GC×GC/FID. Results show that both variables significantly affected the number of compounds detected, their measured weight percentages, and the repeatability of the analysis. A higher column load (2.5 nL) generally resulted in more accurate and repeatable measurements compared to a lower load (0.05 nL). In addition, an inverse relationship was found for both the accuracy and repeatability of the hydrocarbon composition measurements versus the S/N threshold value used. These findings demonstrate that GC×GC/FID measurement quality in terms of accuracy and repeatability can be optimized by maximizing the column load value (without incurring on chromatographic performance deterioration) and by minimizing the S/N threshold value.

综合二维气相色谱-火焰电离检测(GC×GC/FID)是一种定量测定喷气燃料中碳氢化合物的有力技术。然而,柱载和用于包裹体峰的信噪比阈值等因素会显著影响碳氢化合物成分测量的准确性和可重复性。尽管这些参数很重要,但它们的影响还没有得到系统的研究。由于特定的喷气燃料特性(如闪点、冰点和运动粘度)高度依赖于特定碳氢化合物类别的浓度,因此对单个碳氢化合物组(如C7异烷烃)进行准确和精确的定量尤为重要。在本研究中,我们使用GC×GC/FID研究了柱载(0.05 vs. 2.5 nL)和S/N阈值(0-150)对Jet A燃料碳氢化合物组成的影响。结果表明,这两个变量显著影响检测到的化合物的数量、它们的测量重量百分比和分析的可重复性。与较低的柱载量(0.05 nL)相比,较高的柱载量(2.5 nL)通常导致更准确和可重复的测量。此外,油气成分测量的准确性和可重复性与所使用的S/N阈值呈反比关系。这些结果表明,GC×GC/FID测量质量的准确性和可重复性可以通过最大化柱负载值(不导致色谱性能下降)和最小化S/N阈值来优化。
{"title":"Impact of Column Load and Signal-to-Noise Threshold on the Accuracy and Repeatability of Jet A Hydrocarbon Profiling via GC×GC/FID","authors":"Brent A. Modereger,&nbsp;Louis Edwards Caceres-Martinez,&nbsp;Michael E. Peretich,&nbsp;Hilkka I. Kenttämaa,&nbsp;Gozdem Kilaz","doi":"10.1002/jssc.70356","DOIUrl":"10.1002/jssc.70356","url":null,"abstract":"<p>Comprehensive two-dimensional gas chromatography with flame ionization detection (GC×GC/FID) is a powerful technique for quantifying hydrocarbons in jet fuel. However, factors such as column load and the signal-to-noise (S/N) ratio threshold used for peak inclusion can significantly influence the accuracy and repeatability of hydrocarbon composition measurements. Despite their importance, the effects of these parameters have not been systematically studied. Accurate and precise quantitation of individual hydrocarbon groups (e.g., C<sub>7</sub> isoalkanes) is particularly critical, as specific jet fuel properties, such as flash point, freezing point, and kinematic viscosity, are highly dependent on the concentrations of specific hydrocarbon classes. In this study, we investigated the influence of column load (0.05 vs. 2.5 nL) and S/N threshold (0–150) on the measured hydrocarbon composition of Jet A fuel using GC×GC/FID. Results show that both variables significantly affected the number of compounds detected, their measured weight percentages, and the repeatability of the analysis. A higher column load (2.5 nL) generally resulted in more accurate and repeatable measurements compared to a lower load (0.05 nL). In addition, an inverse relationship was found for both the accuracy and repeatability of the hydrocarbon composition measurements versus the S/N threshold value used. These findings demonstrate that GC×GC/FID measurement quality in terms of accuracy and repeatability can be optimized by maximizing the column load value (<i>without incurring on chromatographic performance deterioration</i>) and by minimizing the S/N threshold value.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 1","pages":""},"PeriodicalIF":2.8,"publicationDate":"2026-01-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12824433/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146018604","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
期刊
Journal of separation science
全部 Acc. Chem. Res. ACS Applied Bio Materials ACS Appl. Electron. Mater. ACS Appl. Energy Mater. ACS Appl. Mater. Interfaces ACS Appl. Nano Mater. ACS Appl. Polym. Mater. ACS BIOMATER-SCI ENG ACS Catal. ACS Cent. Sci. ACS Chem. Biol. ACS Chemical Health & Safety ACS Chem. Neurosci. ACS Comb. Sci. ACS Earth Space Chem. ACS Energy Lett. ACS Infect. Dis. ACS Macro Lett. ACS Mater. Lett. ACS Med. Chem. Lett. ACS Nano ACS Omega ACS Photonics ACS Sens. ACS Sustainable Chem. Eng. ACS Synth. Biol. Anal. Chem. BIOCHEMISTRY-US Bioconjugate Chem. BIOMACROMOLECULES Chem. Res. Toxicol. Chem. Rev. Chem. Mater. CRYST GROWTH DES ENERG FUEL Environ. Sci. Technol. Environ. Sci. Technol. Lett. Eur. J. Inorg. Chem. IND ENG CHEM RES Inorg. Chem. J. Agric. Food. Chem. J. Chem. Eng. Data J. Chem. Educ. J. Chem. Inf. Model. J. Chem. Theory Comput. J. Med. Chem. J. Nat. Prod. J PROTEOME RES J. Am. Chem. Soc. LANGMUIR MACROMOLECULES Mol. Pharmaceutics Nano Lett. Org. Lett. ORG PROCESS RES DEV ORGANOMETALLICS J. Org. Chem. J. Phys. Chem. J. Phys. Chem. A J. Phys. Chem. B J. Phys. Chem. C J. Phys. Chem. Lett. Analyst Anal. Methods Biomater. Sci. Catal. Sci. Technol. Chem. Commun. Chem. Soc. Rev. CHEM EDUC RES PRACT CRYSTENGCOMM Dalton Trans. Energy Environ. Sci. ENVIRON SCI-NANO ENVIRON SCI-PROC IMP ENVIRON SCI-WAT RES Faraday Discuss. Food Funct. Green Chem. Inorg. Chem. Front. Integr. Biol. J. Anal. At. Spectrom. J. Mater. Chem. A J. Mater. Chem. B J. Mater. Chem. C Lab Chip Mater. Chem. Front. Mater. Horiz. MEDCHEMCOMM Metallomics Mol. Biosyst. Mol. Syst. Des. Eng. Nanoscale Nanoscale Horiz. Nat. Prod. Rep. New J. Chem. Org. Biomol. Chem. Org. Chem. Front. PHOTOCH PHOTOBIO SCI PCCP Polym. Chem.
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
0
微信
客服QQ
Book学术公众号 扫码关注我们
反馈
×
意见反馈
请填写您的意见或建议
请填写您的手机或邮箱
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
现在去查看 取消
×
提示
确定
Book学术官方微信
Book学术文献互助
Book学术文献互助群
群 号:604180095
Book学术
文献互助 智能选刊 最新文献 互助须知 联系我们:info@booksci.cn
Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。
Copyright © 2023 Book学术 All rights reserved.
ghs 京公网安备 11010802042870号 京ICP备2023020795号-1