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}
{"title":"Recent developments in the use of electrokinetic methods for rapid cell viability assessments and separations","authors":"Blanca H. Lapizco-Encinas","doi":"10.1016/j.jcoa.2024.100185","DOIUrl":"10.1016/j.jcoa.2024.100185","url":null,"abstract":"<div><div>Rapid cell viability assessments are essential in a growing number of fields, including clinical analysis, healthcare, drug development and food safety. Electrokinetic (EK) methodologies have proved to be robust and reliable platforms of the analysis of cells, including viability assessments. Discussed here are applications of two EK phenomena, dielectrophoresis and electrophoresis, which can discriminate cells by their viability status and also sort and separate cells into separate viable and nonviable fractions, so further analysis can be performed. For each EK method, the operating principle is presented, followed by a brief historical overview and a detailed analysis of recent reports published between 2015 and 2024. The concluding remarks include a summary of the content of this review article and present a future perspective on the expected future advances on EK-based systems for the assessment and separation of cells based on their viability status.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100185"},"PeriodicalIF":0.0,"publicationDate":"2024-10-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142533859","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}
Laurine Réset, Clément De Saint Jores, Caroline West
{"title":"Chiral and achiral analysis of chiral flavonoids with liquid and supercritical fluid chromatography – A review","authors":"Laurine Réset, Clément De Saint Jores, Caroline West","doi":"10.1016/j.jcoa.2024.100183","DOIUrl":"10.1016/j.jcoa.2024.100183","url":null,"abstract":"<div><div>Flavonoids have been the topic of numerous studies for decades because they possess varied interesting bioactivities including <em>e.g</em>. antioxidant and anticancer properties. In particular, some flavonoids possess chiral features, due to the presence of one or two chiral carbon atoms on their aglycone root. They include flavans, isoflavans, flavanones, flavanonols, flavanols and auronols. In addition, other chirality centres may be observed on the carbohydrate groups attached to the aglycone root, but these will not be considered in the present paper. However, as stereoisomers usually have different bioactivity, analysis methods focusing on these specific flavonoid classes should be of interest to better understand their mode of action and their biosynthetic pathways. In the present review, we have examined chromatographic analyses in the liquid phase (LC) and the supercritical phase (SFC) in achiral and chiral modes to analyse chiral flavonoids. One- and two-dimensional methods are reported, and the different detection modes are also examined. Note that this review did not aim at being comprehensive, but rather at displaying the diversity and main features of current methods.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100183"},"PeriodicalIF":0.0,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142446009","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}
Wesley W. Barnhart, Muhammad Qamar Farooq, Imad A. Haidar Ahmad
{"title":"A simplified tutorial on charged aerosol detection: Understanding the basics, optimization, and troubleshooting","authors":"Wesley W. Barnhart, Muhammad Qamar Farooq, Imad A. Haidar Ahmad","doi":"10.1016/j.jcoa.2024.100181","DOIUrl":"10.1016/j.jcoa.2024.100181","url":null,"abstract":"<div><div>The charged aerosol detector (CAD) measures the overall charge deposited on aerosolized particles to produce a signal proportional to the mass of analyte present, which applies to compounds with or without a chromophore. A significant benefit of CAD is the ability to quantitate a wide range of non-volatile compounds in absence of their authentic standards due to uniform response factor for such analytes. CAD is also a valuable tool to help detect and/or quantitate compounds with poor or no UV absorption. These can include salts, impurities, and a variety of other types of analytes.</div><div>In this tutorial, fundamental principles of CAD and its utilization, troubleshooting, and maintenance will be demonstrated to ensure proper CAD usage. Successful operation of CAD includes optimizing power function value (PFV) to allow for a broader dynamic range and improve uniformity of response. The use of an inverse gradient (admixed post-column) enables more accurate quantitation, when employing a gradient analysis method. Several troubleshooting strategies, including diagnosing inverse gradient pump organic solvent delivery and determining volume match/mismatch between the inverse gradient and system pumps, will be presented along with important aspects of operating a CAD. Lastly, ensuring reliable results involves monitoring the performance of CAD over time to understand whether it is working sufficiently or if maintenance is required.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100181"},"PeriodicalIF":0.0,"publicationDate":"2024-10-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142533858","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}
Alejandro Rodríguez-González , Ana I. Jiménez-Abizanda , Verónica Pino , Adrián Gutiérrez-Serpa
{"title":"In vial thin-film solid-phase microextraction using silver nanoparticles as coating for the determination of phenols in waters","authors":"Alejandro Rodríguez-González , Ana I. Jiménez-Abizanda , Verónica Pino , Adrián Gutiérrez-Serpa","doi":"10.1016/j.jcoa.2024.100182","DOIUrl":"10.1016/j.jcoa.2024.100182","url":null,"abstract":"<div><div>A novel thin-film solid-phase microextraction (TF-SPME) device based on glass vials internally coated with silver nanoparticles (AgNPs) was developed for the first time, and used for determining five phenols in wastewater, bottled water, and irrigation water samples by high-performance liquid chromatography coupled to a photodiode array detector (HPLC-PDA). Different AgNPs were synthesized varying the ratio of metallic salt <em>versus</em> the reduction agent, and the pH of the synthesis. The preparation of the TF-SPME glass vial device was optimized in terms of the type of AgNPs used and the number of layers of AgNPs. Besides, the TF-SPME procedure was also optimized. The TF-SPME method was very simple, only requiring the addition of 18 mL of water and 5 min of agitation, followed by the disposal of the water and addition of the 750 µL as desorption solvent, and direct HPLC-PDA injection. The entire method showed adequate analytical performance, with limits of detection ranging from 3 to 8 μg·L<sup>-1</sup>, and intra-day and inter-day precision (as RSD), both evaluated with different vials and therefore showing inter-batch precision, with values between 8.70 and 16.4 %, and 6.0 and 19.7 %, respectively. The TF-SPME-HPLC-PDA procedure was compared with previous methods for the determination of phenols, both in terms of analytical performance and greenness assessments applying different metrics, showing clear advantages.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100182"},"PeriodicalIF":0.0,"publicationDate":"2024-10-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142440946","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":"Microchip gas chromatographic columns dedicated for space exploration: Stationary phase coating, setup optimization and evaluation of column performances","authors":"Arnaud Philippart , Valérie Peulon-Agasse , Malak Rizk-Bigourd , Audrey Boco-Simon , Gabin Bergerot , Guillaume Rioland , Arnaud Buch , Cyril Szopa , Pascal Cardinael","doi":"10.1016/j.jcoa.2024.100180","DOIUrl":"10.1016/j.jcoa.2024.100180","url":null,"abstract":"<div><div>This work is the first part of a project aiming to specifically design gas chromatographic microcolumns for space exploration. In particular, this study explored the functionalization and characterization of silicon/glass microchip gas chromatographic columns designed with a serpentine-shaped channel having an internal square cross-section. This microcolumn can be connected using a robust fluidic manifold with removable capillary connections to a conventional gas chromatograph or implemented in a prototype instrument for space exploration. First, benchtop gas chromatographic system was optimized in terms of injector liner volume, internal diameter (I.D.) of the capillary connections and data frequency of detection to ensure an optimal evaluation of column efficiency. Junction capillaries of 100 μm I.D., a liner of 1.2 mm I.D. and a detection acquisition frequency of 100 Hz were found to be the optimal set-up and parameters. Moreover, the stationary phase coating velocity was slowed-down to increase column efficiency by 100 %. Then, the performances of a square cross-section capillary column were compared with those of a conventional circular cross-section column. The coating efficiencies were estimated at 55 % and 42 % for circular and square internal cross-section geometries respectively, demonstrating that the square section geometry did not affect significantly the column performances. Stationary phase films of different thicknesses, from 0.032 to 0.260 µm, were coated on different microchips of the same production batch to assess the influence of film thickness on the chromatographic performances. Microchips performance was evaluated through Golay's plots, and some of the microchips were also studied by optical microscopy. The efficiency and retention capacity of our microchip column is shown to be highly dependent on the film thickness (9,000 plates.m<sup>-1</sup> with <em>k</em> = 0.12 for the thinnest film and up to almost 4,000 plates.m<sup>-1</sup> with <em>k</em> = 0.93 for the thickest film). Finally, the coating process repeatability was validated by producing three identical microchips with RSD of 4.8 % for the average number of theoretical plates.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"6 ","pages":"Article 100180"},"PeriodicalIF":0.0,"publicationDate":"2024-10-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142424864","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}