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}
Eliza K. Hanson, Samuel W. Foster, Christopher Piccolo, James P. Grinias
{"title":"Considerations for method development and method translation in capillary liquid chromatography: A tutorial","authors":"Eliza K. Hanson, Samuel W. Foster, Christopher Piccolo, James P. Grinias","doi":"10.1016/j.jcoa.2024.100190","DOIUrl":"10.1016/j.jcoa.2024.100190","url":null,"abstract":"<div><div>HPLC remains one of the most widely used measurement techniques for chemical analysis. Capillary LC, which utilizes narrow diameter columns operated at lower flow rates than analytical-scale LC, continues to gain adoption based on its reduced mobile phase consumption and increased sensitivity when coupled to MS detection. This tutorial offers practical insights into the most critical aspects of translating analytical-scale separations to the capillary scale. The selection of pumping systems, detectors, and the potential for performance loss due to extra-column effects are examined within the context of separations using columns with inner diameters ≤ 0.3 mm. Column choices within this diameter range are also detailed, both in terms of stationary phase support options and general commercial availability. The impact of these various factors on the effective development/translation of LC methods down to flow rates under 10 µL/min is described to provide readers with a basis for implementing these strategies within their own analytical workflows.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100190"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142653574","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":"Tutorial on modelling chromatographic surrogation of biological processes","authors":"Elisabet Fuguet , Martí Rosés","doi":"10.1016/j.jcoa.2024.100189","DOIUrl":"10.1016/j.jcoa.2024.100189","url":null,"abstract":"<div><div>The accurate emulation of biological partition systems through physicochemical models is crucial in pharmacology, toxicology, and environmental science for understanding the ADMET profiles of substances. Direct experimentation on biological systems can be long, expensive, and ethically and practically challenging, so developing reliable physicochemical models is essential. These models help predict compound behaviour in organisms, reduce animal testing, and streamline drug discovery and risk assessment. Chromatographic systems are of particular interest to mimic biological or environmental processes because of its versatility, as they provide a large number of different partition systems only by changing the nature of the mobile and stationary or pseudostationary phases. The effectiveness of any physicochemical system in emulating biological processes is usually evaluated through empirical correlation with biological data. However, the characterization of physicochemical and biological systems using a common model, such as Abraham's solvation model, allows to identify the best physicochemical systems to surrogate particular biological or environmental processes, only by comparison of the system constants of the models. This tutorial demonstrates how to compare, predict, and improve the efficiency of physicochemical systems to surrogate biological or environmental ones without the need for previous empirical correlations. Skin permeation is presented as example of chromatographic surrogation and case study.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100189"},"PeriodicalIF":0.0,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142572261","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 Imiołek , Matthew Lauber
{"title":"Ion-pair reversed-phase chromatography analysis of oligonucleotides using ultra-short (20 x 2.1 mm) columns. Tutorial","authors":"Szabolcs Fekete , Mateusz Imiołek , Matthew Lauber","doi":"10.1016/j.jcoa.2024.100187","DOIUrl":"10.1016/j.jcoa.2024.100187","url":null,"abstract":"<div><div>With this work, we present a comprehensive tutorial for the analysis of oligonucleotides (ONs, 5 to 100 mer) using ion-pair reversed-phase liquid chromatography (IP-RPLC) on ultra-short columns (20 × 2.1 mm). We explore the impact of ion-pairing (IP) agents on ON retention and demonstrate that while IP agents significantly influence absolute retention, their effect on selectivity is often minimal. Our findings emphasize the utility of systematic method development, including software-assisted retention modeling, to optimize gradient steepness and temperature such that resolution can be optimized for both sequence and length variants. We recommend the use of low-adsorption column hardware to minimize nonspecific interactions, which is to the benefit of improving method robustness, peak shapes and recovery (especially of shortmer impurities). Our results confirm the utility of so-called ultra-short column formats as is demonstrated by way of the example, quick run time separations and high-throughput ON analyses. The study establishes practical guidelines for developing robust, reproducible, and high-efficiency IP-RPLC methods for ONs which will be of assistance to analysts working on new therapeutics and new sequencing and diagnostic reagents alike.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100187"},"PeriodicalIF":0.0,"publicationDate":"2024-10-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142533861","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}
Shun-Hsin Liang, Moubani Chakraborty, Justin A. Steimling
{"title":"Incorporating ultrashort-chain compounds into the comprehensive analysis of per- and polyfluorinated substances in potable and non-potable waters by LC-MS/MS","authors":"Shun-Hsin Liang, Moubani Chakraborty, Justin A. Steimling","doi":"10.1016/j.jcoa.2024.100188","DOIUrl":"10.1016/j.jcoa.2024.100188","url":null,"abstract":"<div><div>Ultrashort-chain (USC) per- and polyfluoroalkyl substances (PFAS) are small and very polar compounds with carbon chain lengths shorter than C4. Their ubiquitous and high levels of occurrence in environmental aquatic systems are emerging as a significant concern, rivaling the well-established issues associated with long-chain PFAS contamination. Therefore, it is important to analyze both USC and long-chain PFAS together in water samples to comprehensively assess and address the full spectrum of PFAS contamination. The high polarity of USC PFAS poses a challenge for standard chromatographic practices in PFAS analysis, primarily due to insufficient chromatographic retention. In this study, a simple and reliable workflow was developed for the simultaneous analysis of C1 to C14 perfluoroalkyl carboxylic and sulfonic acids, along with other groups of PFAS, in both potable and non-potable waters. The chromatographic separation was conducted using a polar-embedded reversed-phase LC column with an inert coating on the hardware. Three different water matrices (tap water, bottled water, sewage treatment wastewater) were chosen for method evaluation to demonstrate the applicability of the developed workflow for measuring 45 PFAS compounds in diverse water samples. A dilute-and-shoot workflow was evaluated by accuracy and precision analysis at five fortification levels, ranging from 2 to 250 ng/L. Eighteen isotopically labeled PFAS, serving as extracted internal standards, were added to the samples at 100 ng/L to validate the accuracy of the entire workflow. Calibration standards were prepared in reverse osmosis water due to its cleanliness for all analytes. The calibration ranges varied among different analytes, spanning from 1 – 1000 ng/L. All analytes and extracted internal standards exhibited recovery values ranging from 70% to 130% of the nominal concentration across all fortification levels. Satisfactory method precision was demonstrated with %RSD values below 20%. Additional potable and non-potable waters collected from various source waters were tested to further demonstrate that the established workflow is suitable for the accurate quantification of targeted PFAS in a wide range of water matrices.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100188"},"PeriodicalIF":0.0,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142533860","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}