{"title":"Development of a transportable High-Performance Liquid Chromatograph with Ultraviolet detection and a method for the rapid analysis of 13 carbonyl compounds hydrazones","authors":"Audrey Grandjean , Anaïs Becker , Mathilde Mascles , Franck Amiet , Jean-Philippe Amiet , Damien Bazin , Stéphane Le Calvé","doi":"10.1016/j.jcoa.2024.100201","DOIUrl":"10.1016/j.jcoa.2024.100201","url":null,"abstract":"<div><div>In environments with elevated air pollution, highly reactive aldehydes pose significant health concerns. This study proposes a simultaneous analysis of 13 carbonyl compounds, according to the ISO 16,000–3 reference method, adapted for a novel transportable High-Performance Liquid Chromatograph (HPLC) system. The transportable HPLC system consists of a reinforced analytical suitcase and a computer suitcase, each equipped with spring systems to fortify them against impact. The system features a straightforward isocratic pump, ensuring reliability and ease of operation, while sample delivery is managed by a piston pump coupled to a multiplexing valve. Derived carbonyl compounds with 2,4-dinitrophenylhydrazine were separated in isocratic mode using water and acetonitrile with a reverse-phase column in less than 20 min. Out of the 13 hydrazones, only 2-butanone-2,4-DNPH (BO-DNPH) and butanal-2,4-DNPH (BA-DNPH) were fully coeluted, and separation of the other critical pairs containing 3 and 4 carbons was achieved. The method was applied to the transportable HPLC equipped with a UV or light-emitting diode (LED) detector. These results were compared with the ones obtained on two benchtop laboratory HPLCs equipped with a diode array detector (DAD). The limit of detection (LOD) for the hydrazones of the carbonyl compounds ranged from 0.12 to 0.38 mg L<sup>–1</sup> with the UV detector and 0.45 to 1.04 mg L<sup>–1</sup> with the LED detector. Precision was determined from consecutive injections of the analytes to yield RSD<11.5% (UV) and RSD<14.1% (LED). Performances were close to that of the laboratory HPLCs, either in sensitivity, resolution, or repeatability with overall more accurate and robust results with the UV than with the LED detector. Despite the LED system not fully meeting the standard method requirements with linearities correlation coefficients lower than 0.999, both systems and methods were validated for the isocratic analysis of hydrazones for aldehydes and ketones quantification. An additional comparison was made with the literature regarding both the isocratic method developed and the transportable system.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100201"},"PeriodicalIF":0.0,"publicationDate":"2024-12-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168830","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Szabolcs Fekete , Mateusz Imiolek , Matthew Lauber
{"title":"Weak to strong ion-pair gradients to expand the selectivity of oligonucleotide separations in reversed phase liquid chromatography - A proof of concept","authors":"Szabolcs Fekete , Mateusz Imiolek , Matthew Lauber","doi":"10.1016/j.jcoa.2024.100200","DOIUrl":"10.1016/j.jcoa.2024.100200","url":null,"abstract":"<div><div>This study introduces a novel ion-pair reversed-phase liquid chromatography (IP-RPLC) method using a dual gradient approach to enhance the separation of oligonucleotides. By combining a weak ion-pairing (IP) agent in the starting (weaker) mobile phase with a strong IP agent in the final (stronger) mobile phase, this method widens the elution window, improving the resolution and selectivity for complex ON mixtures. The approach outperforms traditional single IP systems, particularly in separating sequence and size variants of ONs. Experimental results demonstrate that the weak-to-strong gradient yields better peak separation and higher selectivity compared to conventional methods. This innovative gradient strategy, combined with concave gradients, offers significant potential for optimizing ON separations in the development of oligonucleotide-based therapeutics.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100200"},"PeriodicalIF":0.0,"publicationDate":"2024-12-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168825","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Evaluation of thermodynamic contributions to extraction of medical devices by organic solvents as a sample preparation step in chemical characterization of medical devices","authors":"Jianwei Li","doi":"10.1016/j.jcoa.2024.100199","DOIUrl":"10.1016/j.jcoa.2024.100199","url":null,"abstract":"<div><div>The thermodynamic contribution to extraction of medical devices by organic solvents as a first sample preparation step in chemical characterization studies is evaluated by Abraham's solvation parameter model using five representative materials (low density polyethylene or LDPE, silicone, polyurethane or PU, polyoxymethylene or POM, and polyacrylate or PA) and ten solvents (methanol, ethanol, isopropanol, acetonitrile, ethylene glycol, acetone, butanone, hexane, olive oil, and triolein). The Abraham's model is used to predict the material-solvent partition system coefficients by the corresponding partition system constants and representative extractables. The partition system constants are indirectly derived by a “thermodynamic circle conversion” method, based on material-water partition systems and solvent- water partition systems or material-air partition systems and solvent-air water partition systems. The material-solvent partition coefficient, <span><math><msub><mi>P</mi><mrow><mi>M</mi><mo>/</mo><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub></math></span>=<span><math><mrow><msub><mi>C</mi><mi>M</mi></msub><mo>/</mo><msub><mi>C</mi><mrow><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub></mrow></math></span>, defined as the concentration in the material phase divided by the concentration in the solvent phase, is used as the solvent extraction strength. <span><math><mrow><mi>log</mi><mo>(</mo><msub><mi>P</mi><mrow><mi>M</mi><mo>/</mo><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub><mo>)</mo></mrow></math></span> values are predicted for all material-solvent pairs using the representative extractables, mostly from Wayne state university experimental descriptor database (WSUEDD). The predictive <span><math><mrow><mi>log</mi><mo>(</mo><msub><mi>P</mi><mrow><mi>M</mi><mo>/</mo><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub><mo>)</mo></mrow></math></span> values of material-solvent pairs are considered as the upper bound, indicating the significance of partitioning effect in solvent extraction. The calculation results using water-based or air-based partition systems are also compared. The predictive results are discussed in relation to the solvent-material interaction or swelling as well. Several conclusions can be drawn from this study. First, the predictive consistency of two conversion systems (water-based or air-based) is established, indicating the accuracy and robustness of Abraham's model. Second, the predicted partition coefficients are confirmed by available experimental values (LDPE and silicone), and the predicted solvent extraction strengths are supported by available experimental extraction data. Third, the kinetic effect, rather than the thermodynamic effect, is the dominant extractables release process in sample preparation step of chemical characterization studies. The solvent sel","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100199"},"PeriodicalIF":0.0,"publicationDate":"2024-12-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168827","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yash Mehta , Dhavalkumar Patel , Iqra Pervaiz, Ulrich Bickel, Abraham Jacob Al-Ahmad
{"title":"Targeted proteomics for absolute quantification of glucose transporter 1 in mammalian brain cells using liquid chromatography-mass spectrometry","authors":"Yash Mehta , Dhavalkumar Patel , Iqra Pervaiz, Ulrich Bickel, Abraham Jacob Al-Ahmad","doi":"10.1016/j.jcoa.2024.100198","DOIUrl":"10.1016/j.jcoa.2024.100198","url":null,"abstract":"<div><div>Glucose represents a major source of energy for mammalian brains. Its uptake is tributary to a functional glucose transporter (GLUT1) expression at the blood-brain barrier (BBB). However, detecting and quantifying GLUT1 at the protein level using antibodies-based methods can be challenging. In this study, we have described an analytical method (using liquid-chromatography mass-spectrometry (LC-MS/MS)) to provide a specific and absolute quantification of GLUT1 in human and non-human cells.</div><div>We identified a specific peptide signature for GLUT1 (TFDEIASGFR), with a retention time of 1.53 min with three distinct MRM transitions (571.8 > 894.3, 571.8 > 537.2 and 571.8 > 650.3 m/z ratios respectively). Following optimization, we compared the GLUT1 protein expression of our method versus immunoblot and concluded that our method was superior in terms of sensitivity (LLOQ=0.78ng/mL vs. 3.125μg/lane), better dynamic range (0.78–200ng/mL versus 3.125–25μg/lane) and better linearity (R2 = 0.999 versus R2 = 0.929) than the immunoblots counterpart. Furthermore, we used such a method to provide absolute GLUT1 quantification in various brain endothelial cells, showing differences in protein expression. Finally, we also used this method to assess changes in GLUT1 protein levels during the differentiation of induced pluripotent stem cells (iPSCs) into astrocyte-like cells (iAstros) and brain microvascular endothelial cell-like cells (iBMECs). Taken together, we have developed and optimized a proteomic method for the absolute quantification of GLUT1 in mammalian cells, which allows an alternative method for protein quantification independent of the antibody-based ones.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100198"},"PeriodicalIF":0.0,"publicationDate":"2024-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168828","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Carlos Andrés López-Vargas , Pablo Richter , Milton Rosero-Moreano
{"title":"Extraction of estrogenic hormones in wastewater samples by using rotating disk and modified clays with ionic liquids","authors":"Carlos Andrés López-Vargas , Pablo Richter , Milton Rosero-Moreano","doi":"10.1016/j.jcoa.2024.100194","DOIUrl":"10.1016/j.jcoa.2024.100194","url":null,"abstract":"<div><div>Both synthetic and natural hormones—17α-ethinylestradiol (EE2), 17β-estradiol (E2), and estriol (E3)—are present in wastewater samples in concentrations typically expressed in ng <span>l</span><sup>-1</sup>. These concentrations are significant, as the presence of such hormones in water sources poses risks to both living organisms and the environment. Steroidal hormones from human sources are categorized as emerging pollutants and endocrine-disrupting compounds (EDCs), which constitute a health hazard.</div><div>In this study, the Rotating Disk Sorption Extraction (RDSE) method was used with modified clays incorporating ionic liquids to detect estrogenic hormones in hospital wastewater treatment plant (HWWTP) samples. Sodium montmorillonite was modified to enhance its extractive capacity by intercalating ionic liquids ([C16MIM<sup>+</sup>][anion<sup>-</sup>], where anion = Br<sup>-</sup>, OH<sup>-</sup>, or BF<sub>4</sub><sup>-</sup>) between its interlayers. Following extraction, the concentrated analytes were measured using liquid chromatography coupled with photodiode array detection (HPLC-PDA). The method achieved absolute recoveries of 61 % for EE2, 41 % for E2, and 20 % for E3; these recoveries were lower than those obtained with a commercial C18 sorbent. However, the technique achieved enrichment factors of 13, 23, and 32 for E3, EE2, and E2, respectively. In wastewater, the intra-disk reproducibility (RSD) was below 12 %. The method also provided limits of detection and quantification in HWWTP samples of 0.18–0.42 ng mL<sup>-1</sup> for E3, 0.15–0.37 ng mL<sup>-1</sup> for E2, and 0.07–0.16 ng mL<sup>-1</sup> for EE2 when using the modified adsorbents. Average concentrations in hospital wastewater were measured at 4.30, 3.85, and 7.23 ng mL<sup>-1</sup> in the influent (before treatment) and 3.81, 1.33, and 4.00 ng mL<sup>-1</sup> in the effluent (after treatment) for E3, E2, and EE2, respectively.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100194"},"PeriodicalIF":0.0,"publicationDate":"2024-12-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168826","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Esther A. Olonimoyo , Naresh Kumar Amradi , Stephanie Lansing , Akua A. Asa-Awuku , Candice M. Duncan
{"title":"An improved underivatized, cost-effective, validated method for six short-chain fatty organic acids by high-performance liquid chromatography","authors":"Esther A. Olonimoyo , Naresh Kumar Amradi , Stephanie Lansing , Akua A. Asa-Awuku , Candice M. Duncan","doi":"10.1016/j.jcoa.2024.100193","DOIUrl":"10.1016/j.jcoa.2024.100193","url":null,"abstract":"<div><div>A fast analytical method for a High-Performance Liquid Chromatograph coupled with a Photodiode Array detector (HPLC-PDA) for quantifying six short-chain fatty acids: formic, acetic, propionic, butyric, isovaleric, and valeric acids is optimized and validated. The improved method is compared to existing literature, does not require derivatization, and produces rapid results with relatively low chromatographic cost. Elution modes, mobile phase, pH, and column temperature are optimized to improve peak separation and shorten analysis time without derivatization. The optimized method is characterized by a gradient elution mode with flow rates ranging from 1 to 2.5 mL min <sup>−1</sup> and a short analysis time (7.6 mins). The limits of detection for all six acids (LOD) ranged from 0.0003 to 0.068 mM, while the limits of quantification (LOQ) ranged from 0.001 to 0.226 mM. The improved method showed acceptable sensitivity, precision, and dynamic range. Validation and quantification were tested using fermentation broth samples. This optimized method is characterized by lower detection limits and a 50 % shorter analysis time and is applicable to aqueous samples with complex matrices.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100193"},"PeriodicalIF":0.0,"publicationDate":"2024-12-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168845","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
P. Peiró-Vila, J.R. Torres-Lapasió, M.C. García-Alvarez-Coque
{"title":"Global retention models in reversed-phase liquid chromatography. A tutorial","authors":"P. Peiró-Vila, J.R. Torres-Lapasió, M.C. García-Alvarez-Coque","doi":"10.1016/j.jcoa.2024.100192","DOIUrl":"10.1016/j.jcoa.2024.100192","url":null,"abstract":"<div><div>Developing methods in liquid chromatography for complex samples with hundreds of constituents presents significant challenges, particularly when standards are unavailable or unknown, as is the case of natural products such as medicinal plants. Even when all standards are accessible, optimising experimental conditions for effective separation would require extensive, time-consuming experimentation, often impractical in real-world scenarios. To overcome these challenges, we recently introduced and validated a novel approach based on global retention modelling. This approach has been successfully applied not only to complex samples, but also to simpler ones where standards are available. Global retention models differentiate between solute-specific retention parameters and those characterising the column and solvent, which are shared across the entire set of analytes. These common parameters are derived from chromatographic data for a subset of compounds tracked across experiments in the training design. Once the initial model is built, it can be extended to include additional analytes outside the training set, significantly reducing the need for further extensive experiments. This tutorial provides a comprehensive background on global models, along with a step-by-step explanation of the novel approach. To illustrate its practical application, an example is presented involving a large set of diverse compounds, using a MATLAB set of functions created for this tutorial to showcase the implementation of global retention modelling.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100192"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142701103","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Editorial on “Advances in enantioseparations” virtual special issue","authors":"Salvatore Fanali, Bezhan Chankvetadze","doi":"10.1016/j.jcoa.2024.100186","DOIUrl":"10.1016/j.jcoa.2024.100186","url":null,"abstract":"","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100186"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143167659","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Knox-Saleem kinetic performance limits in liquid chromatography—A contemporary tutorial","authors":"Leonid M. Blumberg","doi":"10.1016/j.jcoa.2024.100184","DOIUrl":"10.1016/j.jcoa.2024.100184","url":null,"abstract":"<div><div>The kinetic performance limits evaluated by Knox and Saleem in 1969 are reevaluated herein. Published 55 years ago, the original study did not address several key features of contemporary chromatography. The following features of chromatographic analyses were assumed in the source:<ul><li><span>•</span><span><div>The <em>static</em> operations (isothermal isobaric GC, isocratic isothermal isobaric LC).</div></span></li><li><span>•</span><span><div>The columns packed with discrete particles.</div></span></li><li><span>•</span><span><div>The columns were optimized to deliver the smallest plate height.</div></span></li></ul>Additionally, currently obsolete parameters and notations were used complicating comprehension of the original study.</div><div>In this tutorial focusing mostly on LC, the original Knox-Saleem study is extended to gradient elution LC, to the columns with arbitrary structure (open, packed, pillar array, monolithic, etc.) and to suboptimal operations – all expressed in contemporary notations. The study is based on previously published basic structure-independent equations of column kinetic performance.</div><div>Some conclusions of this tutorial are different from previous ones. It has been concluded herein that at any pressure (no matter how low) any separation performance (no matter how high) can be achieved as long as the analysis time is acceptable. This seems to contradict with Knox-Saleem statement suggesting that there is “the critical pressure below which a separation number <em>S</em> cannot be achieved however much time is available.” Similar statement was also previously known from Giddings (1962): “critical pressure, <em>p</em><sub>c</sub>, the inlet pressure below which a [required, LB] separation can never be obtained”.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100184"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142552128","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Light-emitting diode-based absorbance detectors for flow-through analysis in analytical chemistry: A tutorial","authors":"Leo Lebanov , Ibraam Emad Mikhail , Brett Paull","doi":"10.1016/j.jcoa.2024.100191","DOIUrl":"10.1016/j.jcoa.2024.100191","url":null,"abstract":"<div><div>The development of light-emitting diodes (LEDs) has played a significant role supporting many recent advances made in chemical analysis. Their small size, low power consumption, and semi-monochromaticity make them ideal light sources for portable photometric devices used in field and on-site analysis, environmental monitoring, and industrial applications, such as process analytical technology (PAT) and continuous real-time analysis. This tutorial provides an overview and critical comparison of the key components in LED-based absorbance detectors, including light sources, optical fibres, flow cells, and photodetectors. Fundamental aspects of LEDs relating to their use in such simple detectors are discussed in detail, along with the development of multi-wavelength detectors that incorporate multiple LEDs. The tutorial also details the different methodologies for assessing and characterising the LED-based absorbance detectors. Finally, this tutorial presents some selected applications of LED based photometric detectors in gas sensing, flow injection analysis (FIA), and coupled with separation techniques such as ion chromatography, liquid chromatography, and capillary zone electrophoresis (CZE).</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100191"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142653575","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}