Pub Date : 2026-03-03DOI: 10.1016/j.chroma.2026.466864
Navratan Soni, Mukul Yadav, David Paul
The explosive growth of therapeutic biomacromolecules and bioparticles, such as monoclonal antibodies, nucleic acid therapeutics, viral vectors, lipid nanoparticles, and extracellular vesicles, has led to a critical need for advanced analytical & chromatographic techniques to resolve their structural, compositional, and physicochemical heterogeneity. Conventional analytical approaches are often inadequate for the characterization of important quality attributes, such as size and charge variants, post-translational modifications, conformational integrity, and particle-level heterogeneity, etc., in these complicated systems. This review discusses recent advances in some of the modern analytical chromatographic approaches for the separation and characterization of such complex biological systems, with high-end detection platforms such as mass spectrometry, multi-angle light scattering, and ion mobility spectrometry. Key developments in size-exclusion, ion-exchange, hydrophobic interaction, hydrophilic interaction, reverse-phase, affinity, hydrodynamic chromatography, and field-flow fractionation are critically discussed based on selected recent primary research studies. Comparative insights are provided to highlight the analytical competence, limitations, and applicability of each technique to different classes of biomolecules. Collectively, this review aims to be a decision-oriented guide for scientists and industrial practitioners seeking suitable analytical chromatographic strategies for characterizing emerging therapeutic biomacromolecules and bioparticles.
{"title":"A comprehensive review of advances in analytical chromatography for the characterization of therapeutic biomacromolecule and bioparticle.","authors":"Navratan Soni, Mukul Yadav, David Paul","doi":"10.1016/j.chroma.2026.466864","DOIUrl":"https://doi.org/10.1016/j.chroma.2026.466864","url":null,"abstract":"<p><p>The explosive growth of therapeutic biomacromolecules and bioparticles, such as monoclonal antibodies, nucleic acid therapeutics, viral vectors, lipid nanoparticles, and extracellular vesicles, has led to a critical need for advanced analytical & chromatographic techniques to resolve their structural, compositional, and physicochemical heterogeneity. Conventional analytical approaches are often inadequate for the characterization of important quality attributes, such as size and charge variants, post-translational modifications, conformational integrity, and particle-level heterogeneity, etc., in these complicated systems. This review discusses recent advances in some of the modern analytical chromatographic approaches for the separation and characterization of such complex biological systems, with high-end detection platforms such as mass spectrometry, multi-angle light scattering, and ion mobility spectrometry. Key developments in size-exclusion, ion-exchange, hydrophobic interaction, hydrophilic interaction, reverse-phase, affinity, hydrodynamic chromatography, and field-flow fractionation are critically discussed based on selected recent primary research studies. Comparative insights are provided to highlight the analytical competence, limitations, and applicability of each technique to different classes of biomolecules. Collectively, this review aims to be a decision-oriented guide for scientists and industrial practitioners seeking suitable analytical chromatographic strategies for characterizing emerging therapeutic biomacromolecules and bioparticles.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1774 ","pages":"466864"},"PeriodicalIF":4.0,"publicationDate":"2026-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147479199","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}
In this work, an environmentally method was proposed for the trace determination of benzoylureas by high performance liquid chromatography system after micro-solid phase extraction method. Sugarcane bagasse-based biochar alginate beads as were employed as sorbent material. The synthesized material was characterized. The univariate optimization approach was performed to determine optimum conditions for both preparation of sugarcane bead adsorbents and micro-solid phase extraction procedure. Under optimal conditions, the limit of detection was found to be in the range of 1.0 – 2.0 μg L–1 and the linearity was obtained between 3.0 and 400 μg L–1 with coefficient of determination greater than 0.99. The applicability of the investigated method was evaluated with recovery studies by spiking experiments in tea samples. The acceptable recovery results between 72.1 and 121.1 % by applying matrix matching calibration showed that the proposed analytical approach is feasible for the determination of benzoylurea insecticides in tea matrices.
{"title":"Eco-friendly sugarcane bagasse-based biochar alginate beads as green sorbents for rapid and highly efficient benzoylurea insecticides extraction in tea samples","authors":"Kittiya Sakhaem , Sujittra Aintharaprasert , Dararat Saenkam , Phatchara Rattanaphonsaen , Wannipha Khiaophong , Yanawath Santaladchaiyakit , Jitlada Vichapong","doi":"10.1016/j.chroma.2026.466701","DOIUrl":"10.1016/j.chroma.2026.466701","url":null,"abstract":"<div><div>In this work, an environmentally method was proposed for the trace determination of benzoylureas by high performance liquid chromatography system after micro-solid phase extraction method. Sugarcane bagasse-based biochar alginate beads as were employed as sorbent material. The synthesized material was characterized. The univariate optimization approach was performed to determine optimum conditions for both preparation of sugarcane bead adsorbents and micro-solid phase extraction procedure. Under optimal conditions, the limit of detection was found to be in the range of 1.0 – 2.0 μg L<sup>–1</sup> and the linearity was obtained between 3.0 and 400 μg L<sup>–1</sup> with coefficient of determination greater than 0.99. The applicability of the investigated method was evaluated with recovery studies by spiking experiments in tea samples. The acceptable recovery results between 72.1 and 121.1 % by applying matrix matching calibration showed that the proposed analytical approach is feasible for the determination of benzoylurea insecticides in tea matrices.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466701"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145964714","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}
Pub Date : 2026-02-22Epub Date: 2026-01-10DOI: 10.1016/j.chroma.2026.466703
FeiFei Dai , Ruoyu Zhang , Dandan Nie , Shuqing Ma , Yurong Qin
A quantitative method for determining 69 odorants in water was developed using arrow-type headspace solid-phase microextraction (SPME) coupled with gas chromatography-tandem mass spectrometry (GC–MS/MS). Key extraction parameters, including extraction and desorption temperatures and times, NaCl addition, fiber type, and rotation speed, were systematically optimized. Under the optimized conditions, target compounds were efficiently enriched, separated on a polar chromatographic column, detected in selected reaction monitoring (SRM) mode, and quantified using external calibration. The method demonstrated high sensitivity, with limits of detection (LODs) ranging from 0.015 to 75 ng/L, and 55 compounds exhibiting LODs below 10 ng/L. All analytes showed excellent linearity (R2 > 0.995) within their respective ranges. Precision was satisfactory, with relative standard deviations (RSDs) between 1.10 % and 17.85 %, including 59 compounds with RSDs <10 %. Average recoveries at three spiking levels ranged from 80 % to 120 %. This automated and environmentally friendly method offers high sensitivity and accuracy, meeting the analytical requirements for complex odorants in water.
{"title":"Development of an arrow solid-phase microextraction GC–MS/MS method for the determination of 69 odorants in water","authors":"FeiFei Dai , Ruoyu Zhang , Dandan Nie , Shuqing Ma , Yurong Qin","doi":"10.1016/j.chroma.2026.466703","DOIUrl":"10.1016/j.chroma.2026.466703","url":null,"abstract":"<div><div>A quantitative method for determining 69 odorants in water was developed using arrow-type headspace solid-phase microextraction (SPME) coupled with gas chromatography-tandem mass spectrometry (GC–MS/MS). Key extraction parameters, including extraction and desorption temperatures and times, NaCl addition, fiber type, and rotation speed, were systematically optimized. Under the optimized conditions, target compounds were efficiently enriched, separated on a polar chromatographic column, detected in selected reaction monitoring (SRM) mode, and quantified using external calibration. The method demonstrated high sensitivity, with limits of detection (LODs) ranging from 0.015 to 75 ng/L, and 55 compounds exhibiting LODs below 10 ng/L. All analytes showed excellent linearity (R<sup>2</sup> > 0.995) within their respective ranges. Precision was satisfactory, with relative standard deviations (RSDs) between 1.10 % and 17.85 %, including 59 compounds with RSDs <10 %. Average recoveries at three spiking levels ranged from 80 % to 120 %. This automated and environmentally friendly method offers high sensitivity and accuracy, meeting the analytical requirements for complex odorants in water.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466703"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145964651","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}
Pub Date : 2026-02-22Epub Date: 2026-01-07DOI: 10.1016/j.chroma.2026.466700
Jiafeng Pang , Zihan Zeng , Hui Zeng , Min Zhang , Weixiong Huang
Open tubular ion chromatography (OTIC) offers a lightweight, low-pressure and efficient platform for on-site ion analysis. Polyetheretherketone (PEEK) is an attractive column substrate because of its mechanical strength, chemical resistance and thermal stability, yet conventional sulfuric-acid sulfonation limits ion-exchange capacity and requires long preparation times. Here, a mixed methanesulfonic and sulfuric acid reagent followed by acetone rinsing was used to streamline the sulfonation process, producing a roughened inner surface with higher functional group density. The optimized 25 μm i.d. PEEK capillaries achieved a cation-exchange capacity of 2.5 ± 0.1 peq/mm2, roughly eight times higher than that from single-acid treatment. The latex-coated columns had an anion-exchange capacity of 20.0 ± 0.8 peq/mm2 and enabled baseline separation of perchlorate within 5 min using 6 mM sodium salicylate as the eluent. When integrated with a nonsuppressed OTIC system and electromembrane extraction, the method exhibited high reproducibility (RSD < 3%), a quantitation limit of 0.2 μM, and recoveries of 87.6–114.9% in environmental samples, confirming its reliability and sensitivity for perchlorate analysis.
{"title":"Polyetheretherketone (PEEK)-based open tubular ion chromatography for perchlorate detection","authors":"Jiafeng Pang , Zihan Zeng , Hui Zeng , Min Zhang , Weixiong Huang","doi":"10.1016/j.chroma.2026.466700","DOIUrl":"10.1016/j.chroma.2026.466700","url":null,"abstract":"<div><div>Open tubular ion chromatography (OTIC) offers a lightweight, low-pressure and efficient platform for on-site ion analysis. Polyetheretherketone (PEEK) is an attractive column substrate because of its mechanical strength, chemical resistance and thermal stability, yet conventional sulfuric-acid sulfonation limits ion-exchange capacity and requires long preparation times. Here, a mixed methanesulfonic and sulfuric acid reagent followed by acetone rinsing was used to streamline the sulfonation process, producing a roughened inner surface with higher functional group density. The optimized 25 μm i.d. PEEK capillaries achieved a cation-exchange capacity of 2.5 ± 0.1 peq/mm<sup>2</sup>, roughly eight times higher than that from single-acid treatment. The latex-coated columns had an anion-exchange capacity of 20.0 ± 0.8 peq/mm<sup>2</sup> and enabled baseline separation of perchlorate within 5 min using 6 mM sodium salicylate as the eluent. When integrated with a nonsuppressed OTIC system and electromembrane extraction, the method exhibited high reproducibility (RSD < 3%), a quantitation limit of 0.2 μM, and recoveries of 87.6–114.9% in environmental samples, confirming its reliability and sensitivity for perchlorate analysis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466700"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145973878","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}
Pub Date : 2026-02-22Epub Date: 2026-01-21DOI: 10.1016/j.chroma.2026.466722
Maby Moll Martínez-Garzón , José Martin Posada-Lotero , Milton Hernando Rosero-Moreano , Elisabeth Restrepo-Parra , Francy Nelly Jiménez-García
Environmental concern regarding the presence of steroid hormones in hospital wastewater treatment plants underscores the need for effective monitoring and removal strategies. Even at trace levels, steroid estrogens exhibit strong biological activity and bioaccumulation potential, classifying them as endocrine-disrupting compounds. In this study, a Montmorillonite/Hydroxyapatite (MMT/HAp) composite was proposed as an environmentally friendly and low-cost alternative for the extraction of estrone (E1), 17β-estradiol (E2), 17α-ethinylestradiol (EE2), and estriol (E3). Sample preparation was carried out using a green analytical method based on rotating disk sorptive extraction. Considering the complexity of wastewater matrices, analytes were determined using gas chromatography coupled to mass spectrometry (GC–MS) in selective ion monitoring mode. A Doehlert experimental design was applied to optimize the extraction process, yielding the following optimal conditions: extraction time of 87 min, sample volume of 16 mL, and stirring speed of 1080 rpm. Hospital wastewater samples from Manizales (Caldas, Colombia) were analyzed, and concentrations of E1, E2, EE2, and E3 were 7.2, 0.1, 6.7, and 33.2 µg L⁻¹, respectively. Limits of detection ranged from 0.06 to 0.40 µg L⁻¹, and limits of quantification from 0.16 to 1.20 µg L⁻¹. Calibration curves for all analytes showed R² values above 0.98. Recovery values obtained through standard addition calibration ranged from 56 % to 90 %, despite significant matrix effects (–67 to 230). The MMT/HAp composite demonstrated comparable performance to the commercial HLB sorbent, confirming its potential for environmental applications.
医院废水处理厂中存在类固醇激素的环境问题突出表明,需要制定有效的监测和去除战略。即使在微量水平,类固醇雌激素也表现出很强的生物活性和生物积累潜力,将其归类为内分泌干扰化合物。本研究提出了蒙脱土/羟基磷灰石(MMT/HAp)复合材料作为一种环保、低成本的提取雌酮(E1)、17β-雌二醇(E2)、17α-炔雌二醇(EE2)和雌三醇(E3)的替代材料。采用旋转圆盘吸附萃取绿色分析方法制备样品。考虑到废水基质的复杂性,在选择性离子监测模式下,采用气相色谱-质谱联用(GC-MS)对分析物进行测定。采用Doehlert实验设计优化提取工艺,得到最佳提取条件:提取时间87 min,进样量16 mL,搅拌速度1080 rpm。医院废水样本马尼萨莱斯(卡尔达斯、哥伦比亚)进行了分析和浓度的E1, E2, EE2,和E3是7.2,0.1,6.7,和33.2µg L⁻¹,分别。检测范围为0.06 - 0.40µg L -毒血症,定量范围为0.16 - 1.20µg L -毒血症。所有分析物的校正曲线R²值均在0.98以上。尽管有显著的基质效应(-67至230),但通过标准添加校准获得的回收率从56%到90%不等。MMT/HAp复合材料表现出与商用HLB吸附剂相当的性能,证实了其在环境应用方面的潜力。
{"title":"Development of a green analytical method based on a Montmorillonite/Hydroxyapatite composite coupled with rotating disk sorptive extraction and GC–MS for monitoring steroid hormones in hospital wastewater","authors":"Maby Moll Martínez-Garzón , José Martin Posada-Lotero , Milton Hernando Rosero-Moreano , Elisabeth Restrepo-Parra , Francy Nelly Jiménez-García","doi":"10.1016/j.chroma.2026.466722","DOIUrl":"10.1016/j.chroma.2026.466722","url":null,"abstract":"<div><div>Environmental concern regarding the presence of steroid hormones in hospital wastewater treatment plants underscores the need for effective monitoring and removal strategies. Even at trace levels, steroid estrogens exhibit strong biological activity and bioaccumulation potential, classifying them as endocrine-disrupting compounds. In this study, a Montmorillonite/Hydroxyapatite (MMT/HAp) composite was proposed as an environmentally friendly and low-cost alternative for the extraction of estrone (E1), 17β-estradiol (E2), 17α-ethinylestradiol (EE2), and estriol (E3). Sample preparation was carried out using a green analytical method based on rotating disk sorptive extraction. Considering the complexity of wastewater matrices, analytes were determined using gas chromatography coupled to mass spectrometry (GC–MS) in selective ion monitoring mode. A Doehlert experimental design was applied to optimize the extraction process, yielding the following optimal conditions: extraction time of 87 min, sample volume of 16 mL, and stirring speed of 1080 rpm. Hospital wastewater samples from Manizales (Caldas, Colombia) were analyzed, and concentrations of E1, E2, EE2, and E3 were 7.2, 0.1, 6.7, and 33.2 µg L⁻¹, respectively. Limits of detection ranged from 0.06 to 0.40 µg L⁻¹, and limits of quantification from 0.16 to 1.20 µg L⁻¹. Calibration curves for all analytes showed R² values above 0.98. Recovery values obtained through standard addition calibration ranged from 56 % to 90 %, despite significant matrix effects (–67 to 230). The MMT/HAp composite demonstrated comparable performance to the commercial HLB sorbent, confirming its potential for environmental applications.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466722"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146045902","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}
Pub Date : 2026-02-22Epub Date: 2026-01-02DOI: 10.1016/j.chroma.2025.466669
Wenjing Ma, Caitlin N. Cain, Robert E. Synovec
Accurate identification of all detectable analyte components in a single comprehensive two-dimensional (2D) gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS) chromatogram is a fundamental interest in the field. While commercial software tools intended for this purpose are available, the performance of these tools to generate an accurate peak table has generally not been validated. To address this, we developed a new algorithmic software approach called 2D mzCompare to generate accurate peak tables for GC × GC-TOFMS. Extending from our original method for one-dimensional GC–MS data, the 2D mzCompare algorithm discovers selective mass channels (m/z) for each analyte to resolve overlapping peaks and improve analyte identification, by leveraging the similarity in retention time and peak shape across m/z of the same analyte. The 2D mzCompare algorithm calculates the peak shape similarity between m/z at every modulation, followed by clustering and focusing steps, to generate a final peak table. To evaluate this software, we simulated realistic GC × GC-TOFMS data in the context of the statistical overlap theory (SOT), so the exact number and identities of analytes are known a priori. Utilizing an in-house mass spectrum library of similar compounds, GC × GC-TOFMS chromatograms were simulated with varying degrees of 2D chromatographic saturation (). At low saturation factors ( = 0.01, 0.03, and 0.1), over 95% of the simulated components are found to be mathematically resolved singlets (pure analyte components) by 2D mzCompare. Meanwhile, approximately 62% were found at = 1, exceeding predictions made by SOT. Application of 2D mzCompare computationally reduces the 2D peak widths, resulting in an ∼12-fold reduction in . The results of this research are simultaneously two-fold. First, we provide a new algorithmic approach, 2D mzCompare, to resolve overlapped analytes in GC × GC-TOFMS data, and second, we validate the accuracy of the software performance using SOT.
{"title":"Developing 2D mzCompare for single comprehensive two-dimensional chromatography time-of-flight mass spectrometry chromatograms: Substantial resolution enhancement in the context of statistical overlap theory","authors":"Wenjing Ma, Caitlin N. Cain, Robert E. Synovec","doi":"10.1016/j.chroma.2025.466669","DOIUrl":"10.1016/j.chroma.2025.466669","url":null,"abstract":"<div><div>Accurate identification of all detectable analyte components in a single comprehensive two-dimensional (2D) gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS) chromatogram is a fundamental interest in the field. While commercial software tools intended for this purpose are available, the performance of these tools to generate an accurate peak table has generally not been validated. To address this, we developed a new algorithmic software approach called 2D mzCompare to generate accurate peak tables for GC × GC-TOFMS. Extending from our original method for one-dimensional GC–MS data, the 2D mzCompare algorithm discovers selective mass channels (<em>m/z</em>) for each analyte to resolve overlapping peaks and improve analyte identification, by leveraging the similarity in retention time and peak shape across <em>m/z</em> of the same analyte. The 2D mzCompare algorithm calculates the peak shape similarity between <em>m/z</em> at every modulation, followed by clustering and focusing steps, to generate a final peak table. To evaluate this software, we simulated realistic GC × GC-TOFMS data in the context of the statistical overlap theory (SOT), so the exact number and identities of analytes are known <em>a priori</em>. Utilizing an in-house mass spectrum library of similar compounds, GC × GC-TOFMS chromatograms were simulated with varying degrees of 2D chromatographic saturation (<span><math><msub><mi>α</mi><mrow><mn>2</mn><mi>D</mi></mrow></msub></math></span>). At low saturation factors (<span><math><msub><mi>α</mi><mrow><mn>2</mn><mi>D</mi></mrow></msub></math></span> = 0.01, 0.03, and 0.1), over 95% of the simulated components are found to be mathematically resolved singlets (pure analyte components) by 2D mzCompare. Meanwhile, approximately 62% were found at <span><math><msub><mi>α</mi><mrow><mn>2</mn><mi>D</mi></mrow></msub></math></span> = 1, exceeding predictions made by SOT. Application of 2D mzCompare computationally reduces the <sup>2</sup>D peak widths, resulting in an ∼12-fold reduction in <span><math><msub><mi>α</mi><mrow><mn>2</mn><mi>D</mi></mrow></msub></math></span>. The results of this research are simultaneously two-fold. First, we provide a new algorithmic approach, 2D mzCompare, to resolve overlapped analytes in GC × GC-TOFMS data, and second, we validate the accuracy of the software performance using SOT.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466669"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145909699","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}
Pub Date : 2026-02-22Epub Date: 2026-01-10DOI: 10.1016/j.chroma.2026.466702
Chiara De Luca , Chiara Nosengo , Amirmohammad Faraji Shovey , Antonio Ricci , Martina Catani , Alberto Cavazzini , Fabrice Gritti , Simona Felletti
This research examined the kinetic behavior of two chiral probes (FMOC-Alanine and Haloxyfop) using a zwitterionic teicoplanin-based column and an aqueous-methanol mobile phase. More specifically, experimental results, supported by literature data measured using the same elution mode, indicate that the presence of a water layer adsorbed on the particle surface hinders analyte surface diffusion leading to localized adsorption. This shows cascading effects on longitudinal diffusion, solid–liquid mass transfer resistance and eddy dispersion, which become analyte-independent. The only difference in the measured plate heights is therefore given only by slow adsorption–desorption kinetics, confirming an important correlation between analyte structure and the extent of band broadening in chiral chromatography.
The findings reported in this study can be expanded to other molecules, suggesting that similar kinetic behavior could be expected if the same experimental conditions are maintained (e.g., same column manufacturer, silica particles, and elution mode). This would help accelerating the method development and the understanding of both the chiral recognition mechanism and the sources of band broadening occurring in chiral chromatography.
{"title":"Exploring adsorption–desorption kinetics and eddy dispersion in enantioselective hydrophilic interaction chromatography using teicoplanin-based chiral stationary phase","authors":"Chiara De Luca , Chiara Nosengo , Amirmohammad Faraji Shovey , Antonio Ricci , Martina Catani , Alberto Cavazzini , Fabrice Gritti , Simona Felletti","doi":"10.1016/j.chroma.2026.466702","DOIUrl":"10.1016/j.chroma.2026.466702","url":null,"abstract":"<div><div>This research examined the kinetic behavior of two chiral probes (FMOC-Alanine and Haloxyfop) using a zwitterionic teicoplanin-based column and an aqueous-methanol mobile phase. More specifically, experimental results, supported by literature data measured using the same elution mode, indicate that the presence of a water layer adsorbed on the particle surface hinders analyte surface diffusion leading to localized adsorption. This shows cascading effects on longitudinal diffusion, solid–liquid mass transfer resistance and eddy dispersion, which become analyte-independent. The only difference in the measured plate heights is therefore given only by slow adsorption–desorption kinetics, confirming an important correlation between analyte structure and the extent of band broadening in chiral chromatography.</div><div>The findings reported in this study can be expanded to other molecules, suggesting that similar kinetic behavior could be expected if the same experimental conditions are maintained (e.g., same column manufacturer, silica particles, and elution mode). This would help accelerating the method development and the understanding of both the chiral recognition mechanism and the sources of band broadening occurring in chiral chromatography.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466702"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145973877","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}
Pub Date : 2026-02-22Epub Date: 2025-12-24DOI: 10.1016/j.chroma.2025.466657
Wei-Qi Xie, Ya-Yun Wang, Yi-Xan Gong
This study developed a gas-evolving phase-transfer strategy for precise sodium chromate quantification. The analytical approach utilized the chemical reaction between sodium chromate and oxalic acid to generate measurable carbon dioxide, which was subsequently quantified via headspace gas chromatography equipped with thermal conductivity detector (HS-GC-TCD). Experimental validation confirmed the method's exceptional analytical performance in sodium chromate determination. The developed phase transformation technique established a robust and efficient protocol for sodium chromate assessment while simultaneously creating a framework for extending this analytical paradigm to other gas-evolving compounds.
{"title":"Efficient analysis of sodium chromate by combining phase-transfer headspace strategy and GC-TCD","authors":"Wei-Qi Xie, Ya-Yun Wang, Yi-Xan Gong","doi":"10.1016/j.chroma.2025.466657","DOIUrl":"10.1016/j.chroma.2025.466657","url":null,"abstract":"<div><div>This study developed a gas-evolving phase-transfer strategy for precise sodium chromate quantification. The analytical approach utilized the chemical reaction between sodium chromate and oxalic acid to generate measurable carbon dioxide, which was subsequently quantified via headspace gas chromatography equipped with thermal conductivity detector (HS-GC-TCD). Experimental validation confirmed the method's exceptional analytical performance in sodium chromate determination. The developed phase transformation technique established a robust and efficient protocol for sodium chromate assessment while simultaneously creating a framework for extending this analytical paradigm to other gas-evolving compounds.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466657"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145973879","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}
Pub Date : 2026-02-22Epub Date: 2026-01-22DOI: 10.1016/j.chroma.2026.466728
Yilin Liu , Juan Wen , Xu Zhang , Xiao Lin , Zhuangzhuang Feng , Dejun Bao , Xiaojian Hu , Ying Zhu
Endocrine disrupting chemicals (EDCs) are a class of emerging contaminants that have raised significant public health concerns. Human co-exposure to mixtures of specific EDCs, such as phthalate and bisphenols, and the associated health risks remain poorly understood. To support biomonitoring and epidemiological studies on these compounds, there is a critical need for sensitive and reliable methods for their quantification in human specimens. Herein, we developed and validated an analytical method based on ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) for the simultaneous determination of 15 phthalate metabolites and 9 bisphenols in human serum. A systematic comparison between liquid-liquid extraction (LLE) and high-efficiency matrix removal (HMR) clean-up approach revealed that HMR offered advantages in terms of extraction efficiency and matrix effect reduction, and was ultimately selected as the final clean-up method for this study. The developed method demonstrated satisfactory performance, with recoveries ranging from 81 % to 115 %, with the relative standard deviations (RSD) below 18 %. The calibration curves established using isotope-labeled internal standards exhibited good linearity, with correlation coefficients (R2) consistently above 0.997. The limits of detection (LODs) and limits of quantification (LOQs) were determined to be in the range of 0.01 ng/mL to 0.2 ng/mL and 0.04 ng/mL to 0.7 ng/mL, respectively. Both intra-day and inter-day precision were satisfactory, with RSDs values ranging from 4.2 % to 13 % and 6.9 % to 14 %, respectively. This sensitive analytical method was successfully applied to the determination of target analytes in human serum samples from 15 pregnant women, demonstrating its applicability for monitoring of these emerging contaminants in human serum.
{"title":"Determination of 15 phthalates metabolites and 9 bisphenols in human serum by using high-performance liquid chromatography coupled with tandem mass spectrometry","authors":"Yilin Liu , Juan Wen , Xu Zhang , Xiao Lin , Zhuangzhuang Feng , Dejun Bao , Xiaojian Hu , Ying Zhu","doi":"10.1016/j.chroma.2026.466728","DOIUrl":"10.1016/j.chroma.2026.466728","url":null,"abstract":"<div><div>Endocrine disrupting chemicals (EDCs) are a class of emerging contaminants that have raised significant public health concerns. Human co-exposure to mixtures of specific EDCs, such as phthalate and bisphenols, and the associated health risks remain poorly understood. To support biomonitoring and epidemiological studies on these compounds, there is a critical need for sensitive and reliable methods for their quantification in human specimens. Herein, we developed and validated an analytical method based on ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) for the simultaneous determination of 15 phthalate metabolites and 9 bisphenols in human serum. A systematic comparison between liquid-liquid extraction (LLE) and high-efficiency matrix removal (HMR) clean-up approach revealed that HMR offered advantages in terms of extraction efficiency and matrix effect reduction, and was ultimately selected as the final clean-up method for this study. The developed method demonstrated satisfactory performance, with recoveries ranging from 81 % to 115 %, with the relative standard deviations (RSD) below 18 %. The calibration curves established using isotope-labeled internal standards exhibited good linearity, with correlation coefficients (<em>R<sup>2</sup></em>) consistently above 0.997. The limits of detection (LODs) and limits of quantification (LOQs) were determined to be in the range of 0.01 ng/mL to 0.2 ng/mL and 0.04 ng/mL to 0.7 ng/mL, respectively. Both intra-day and inter-day precision were satisfactory, with RSDs values ranging from 4.2 % to 13 % and 6.9 % to 14 %, respectively. This sensitive analytical method was successfully applied to the determination of target analytes in human serum samples from 15 pregnant women, demonstrating its applicability for monitoring of these emerging contaminants in human serum.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466728"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146023325","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}
Supercritical fluid chromatography coupled to high-resolution mass spectrometry (SFCHRMS) is gaining attention for non-target screening (NTS), yet systematic evaluations of data-processing workflows remain scarce. Here, we present the first comprehensive comparison between a component-profile (CP) approach based on Region of Interest analysis combined with Component Detection Algorithm and Multivariate Curve Resolution (ROI-CODA-MCR) and a feature-profile (FP) workflow, MS-DIAL. Using extracted ion chromatograms (EICs) as ground truth, both workflows were optimized and benchmarked for standard detection, peak intensity reliability, blank filtering performance, and suspect screening for wastewater samples. Both detected a comparable number of standards (33–35 out of 37) but ROI-derived intensities closely matched EICs (average ratio ≈1, RSD = 5.8%), while MS-DIAL intensities deviated substantially (up to two orders of magnitude, RSD >200%). In non-target analysis, MS-DIAL produced ≈1000 features with many false positives, while ROI-CODA-MCR yielded ≈200 components with lower blank contributions and superior resolution of in-source fragments and adducts. MS-DIAL detected more suspect compounds, highlighting a higher risk of false negatives in the CP approach, particularly for low-intensity or sparse signals. Our results demonstrate that SFCHRMS datasets, often including intense background signals, challenge key assumptions underlying both FP and CP workflows and necessitate careful parameter optimization.
{"title":"Comparative assessment of feature and component profiling workflow for supercritical fluid chromatography – high resolution mass spectrometry analysis","authors":"Samuele Pellacani , Giorgio Tomasi , Gerrit Renner , Selina Tisler","doi":"10.1016/j.chroma.2026.466730","DOIUrl":"10.1016/j.chroma.2026.466730","url":null,"abstract":"<div><div>Supercritical fluid chromatography coupled to high-resolution mass spectrometry (SFC<img>HRMS) is gaining attention for non-target screening (NTS), yet systematic evaluations of data-processing workflows remain scarce. Here, we present the first comprehensive comparison between a component-profile (CP) approach based on Region of Interest analysis combined with Component Detection Algorithm and Multivariate Curve Resolution (ROI-CODA-MCR) and a feature-profile (FP) workflow, MS-DIAL. Using extracted ion chromatograms (EICs) as ground truth, both workflows were optimized and benchmarked for standard detection, peak intensity reliability, blank filtering performance, and suspect screening for wastewater samples. Both detected a comparable number of standards (33–35 out of 37) but ROI-derived intensities closely matched EICs (average ratio ≈1, RSD = 5.8%), while MS-DIAL intensities deviated substantially (up to two orders of magnitude, RSD >200%). In non-target analysis, MS-DIAL produced ≈1000 features with many false positives, while ROI-CODA-MCR yielded ≈200 components with lower blank contributions and superior resolution of in-source fragments and adducts. MS-DIAL detected more suspect compounds, highlighting a higher risk of false negatives in the CP approach, particularly for low-intensity or sparse signals. Our results demonstrate that SFC<img>HRMS datasets, often including intense background signals, challenge key assumptions underlying both FP and CP workflows and necessitate careful parameter optimization.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466730"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146045905","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}