Journal of chromatography open最新文献

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An improved underivatized, cost-effective, validated method for six short-chain fatty organic acids by high-performance liquid chromatography

Journal of chromatography open

Pub Date : 2024-12-03 DOI: 10.1016/j.jcoa.2024.100193

Esther A. Olonimoyo , Naresh Kumar Amradi , Stephanie Lansing , Akua A. Asa-Awuku , Candice M. Duncan

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 ⁻¹ 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.

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引用次数: 0

Global retention models in reversed-phase liquid chromatography. A tutorial 反相液相色谱中的全局保留模型。教程

Journal of chromatography open

Pub Date : 2024-11-01 DOI: 10.1016/j.jcoa.2024.100192

P. Peiró-Vila, J.R. Torres-Lapasió, M.C. García-Alvarez-Coque

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.

为含有数百种成分的复杂样品开发液相色谱方法是一项重大挑战，尤其是在没有标准品或标准品未知的情况下，如药用植物等天然产品。即使可以获得所有标准品，优化实验条件以实现有效分离也需要大量耗时的实验，这在现实世界中往往是不切实际的。为了克服这些挑战，我们最近引入并验证了一种基于全局保留模型的新方法。这种方法不仅成功地应用于复杂的样品，也应用于有标准样品的简单样品。全局保留模型区分了特定于溶质的保留参数和描述色谱柱与溶剂特征的参数，这些参数在整组分析物中是共享的。这些共用参数来自于在训练设计中对实验进行跟踪的化合物子集的色谱数据。一旦建立了初始模型，就可以对其进行扩展，以包括训练集之外的其他分析物，从而大大减少了进一步进行大量实验的需要。本教程全面介绍了全局模型的背景，并逐步解释了这种新方法。为了说明该方法的实际应用，本教程还提供了一个涉及大量不同化合物的示例，使用为本教程创建的一套 MATLAB 函数来展示全局保留模型的实现。

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引用次数: 0

Editorial on “Advances in enantioseparations” virtual special issue

Journal of chromatography open

Pub Date : 2024-11-01 DOI: 10.1016/j.jcoa.2024.100186

Salvatore Fanali, Bezhan Chankvetadze

引用次数: 0

Knox-Saleem kinetic performance limits in liquid chromatography—A contemporary tutorial 液相色谱中的诺克斯-萨利姆动力学性能极限--当代教程

Journal of chromatography open

Pub Date : 2024-11-01 DOI: 10.1016/j.jcoa.2024.100184

Leonid M. Blumberg

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:

•
The static operations (isothermal isobaric GC, isocratic isothermal isobaric LC).
•
The columns packed with discrete particles.
•
The columns were optimized to deliver the smallest plate height.

Additionally, currently obsolete parameters and notations were used complicating comprehension of the original study.

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.

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 S cannot be achieved however much time is available.” Similar statement was also previously known from Giddings (1962): “critical pressure, p_c, the inlet pressure below which a [required, LB] separation can never be obtained”.

本文对 Knox 和 Saleem 于 1969 年评估的动力学性能极限进行了重新评估。最初的研究发表于 55 年前，并未涉及当代色谱法的几个关键特征。资料来源假定色谱分析具有以下特征：-静态操作（等温等压气相色谱、等压等温等压液相色谱）。本教程主要侧重于液相色谱，将 Knox-Saleem 的原始研究扩展到梯度洗脱液相色谱、任意结构的色谱柱（开放式、填料式、柱阵列、整体式等）以及次优操作，所有这些都用现代符号表示。本研究基于之前发布的与结构无关的色谱柱动力学性能基本方程。本文得出的结论是，只要分析时间可以接受，在任何压力下（无论多低）都可以实现任何分离性能（无论多高）。这似乎与诺克斯-萨利姆（Knox-Saleem）的说法相矛盾，他认为 "存在临界压力，在此压力之下，无论有多少时间，都无法达到分离度 S"。Giddings （1962 年）也有类似的说法："临界压力，pc，入口压力，低于该压力将永远无法获得[所需的，LB]分离"。

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引用次数: 0

Light-emitting diode-based absorbance detectors for flow-through analysis in analytical chemistry: A tutorial 基于发光二极管的吸光检测器，用于分析化学中的流动分析：教程

Journal of chromatography open

Pub Date : 2024-11-01 DOI: 10.1016/j.jcoa.2024.100191

Leo Lebanov , Ibraam Emad Mikhail , Brett Paull

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).

发光二极管（LED）的发展在化学分析领域的许多最新进展中发挥了重要作用。发光二极管体积小、功耗低、半单色性强，是用于现场分析、环境监测和工业应用（如过程分析技术 (PAT) 和连续实时分析）的便携式光度测量设备的理想光源。本教程概述了基于 LED 的吸光度检测器的关键部件，包括光源、光纤、流动池和光检测器，并对其进行了重要比较。详细讨论了 LED 在此类简单检测器中应用的基本方面，以及集成多个 LED 的多波长检测器的开发。教程还详细介绍了评估和鉴定基于 LED 的吸光度探测器的不同方法。最后，本教程介绍了基于 LED 的光度检测器在气体传感、流动注射分析 (FIA) 以及离子色谱法、液相色谱法和毛细管区带电泳 (CZE) 等分离技术中的一些选定应用。

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引用次数: 0

Considerations for method development and method translation in capillary liquid chromatography: A tutorial 毛细管液相色谱方法开发和方法转换的注意事项：教程

Journal of chromatography open

Pub Date : 2024-11-01 DOI: 10.1016/j.jcoa.2024.100190

Eliza K. Hanson, Samuel W. Foster, Christopher Piccolo, James P. Grinias

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.

高效液相色谱法仍然是化学分析中应用最广泛的测量技术之一。与分析级液相色谱相比，毛细管液相色谱使用窄直径色谱柱，流速较低，其流动相消耗量更少，与质谱检测联用时灵敏度更高，因此继续得到广泛应用。本教程就将分析级分离转化为毛细管级分离的最关键方面提供了实用的见解。在使用内径≤ 0.3 毫米的色谱柱进行分离时，将考察泵系统、检测器的选择以及柱外效应可能导致的性能损失。此外，还从固定相支持选项和一般商业可用性两方面详细介绍了在此直径范围内的色谱柱选择。介绍了这些不同因素对有效开发/转化流速低于 10 µL/min 的液相色谱方法的影响，为读者在自己的分析工作流程中实施这些策略提供了依据。

引用次数: 0

Editorial on “Recent Advances in Pollutants Analysis” 关于 "污染物分析的最新进展 "的社论

Journal of chromatography open

Pub Date : 2024-11-01 DOI: 10.1016/j.jcoa.2024.100159

Salvatore Fanali , Bezhan Chankvetadze

引用次数: 0

Tutorial on modelling chromatographic surrogation of biological processes 生物过程的色谱代用建模教程

Journal of chromatography open

Pub Date : 2024-11-01 DOI: 10.1016/j.jcoa.2024.100189

Elisabet Fuguet , Martí Rosés

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.

在药理学、毒理学和环境科学中，通过理化模型准确模拟生物分区系统对于了解物质的 ADMET 特征至关重要。直接在生物系统中进行实验耗时长、成本高，而且在伦理和实践方面都具有挑战性，因此开发可靠的理化模型至关重要。这些模型有助于预测化合物在生物体内的行为，减少动物试验，简化药物发现和风险评估。色谱系统具有多功能性，只需改变流动相和固定相或伪固定相的性质，就能提供大量不同的分区系统，因此在模拟生物或环境过程方面具有特别的意义。理化系统在模拟生物过程中的有效性通常是通过与生物数据的经验相关性来评估的。然而，使用共同的模型（如亚伯拉罕溶解模型）对物理化学和生物系统进行表征，只需比较模型的系统常数，就能确定替代特定生物或环境过程的最佳物理化学系统。本教程演示了如何比较、预测和提高理化系统替代生物或环境系统的效率，而无需先前的经验相关性。以皮肤渗透为例，介绍色谱代用和案例研究。

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引用次数: 0

Ion-pair reversed-phase chromatography analysis of oligonucleotides using ultra-short (20 x 2.1 mm) columns. Tutorial 使用超短（20 x 2.1 毫米）色谱柱对寡核苷酸进行离子对反相色谱分析。教程

Journal of chromatography open

Pub Date : 2024-10-23 DOI: 10.1016/j.jcoa.2024.100187

Szabolcs Fekete , Mateusz Imiołek , Matthew Lauber

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.

通过这项工作，我们介绍了在超短色谱柱（20 × 2.1 mm）上使用离子对反相液相色谱（IP-RPLC）分析寡核苷酸（ON，5 至 100 mer）的综合教程。我们探讨了离子配对（IP）剂对ON保留的影响，结果表明，虽然IP剂对绝对保留有显著影响，但对选择性的影响往往微乎其微。我们的发现强调了系统化方法开发（包括软件辅助保留建模）的实用性，可优化梯度陡度和温度，从而优化序列和长度变异的分辨率。我们建议使用低吸附色谱柱硬件，以最大限度地减少非特异性相互作用，这有利于提高方法的稳健性、峰形和回收率（尤其是较短杂质的回收率）。我们的研究结果证实了所谓的超短柱格式的实用性，并通过快速运行时间分离和高通量 ON 分析等实例加以证明。这项研究为开发稳健、可重现、高效的ONs IP-RPLC方法提供了实用指南，对研究新疗法、新测序和诊断试剂的分析人员都有帮助。

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引用次数: 0

Incorporating ultrashort-chain compounds into the comprehensive analysis of per- and polyfluorinated substances in potable and non-potable waters by LC-MS/MS 利用 LC-MS/MS 将超短链化合物纳入饮用水和非饮用水中的全氟和多氟化物的综合分析中

Journal of chromatography open

Pub Date : 2024-10-22 DOI: 10.1016/j.jcoa.2024.100188

Shun-Hsin Liang, Moubani Chakraborty, Justin A. Steimling

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.

超短链（USC）全氟烷基和多氟烷基物质（PFAS）是碳链长度短于 C4 的小型极性化合物。它们在环境水生系统中无处不在且含量很高，正在成为一个令人担忧的重大问题，其严重程度可与长链全氟烷基磺酸污染相关的既定问题相媲美。因此，必须同时分析水样中的 USC 和长链 PFAS，以全面评估和解决全氟辛烷磺酸污染问题。USC PFAS 的极性很高，这对 PFAS 分析中的标准色谱操作提出了挑战，主要原因是色谱保留时间不足。本研究开发了一种简单可靠的工作流程，用于同时分析饮用水和非饮用水中的 C1 至 C14 全氟烷基羧酸和磺酸以及其他类别的 PFAS。色谱分离采用极性嵌入式反相液相色谱柱，硬件上有惰性涂层。选择了三种不同的水基质（自来水、瓶装水、污水处理废水）进行方法评估，以证明所开发的工作流程适用于测量不同水样中的 45 种 PFAS 化合物。在 2 至 250 纳克/升的五个强化水平下，通过准确度和精密度分析，对稀释-检测工作流程进行了评估。在 100 纳克/升的样品中加入 18 种同位素标记的 PFAS 作为提取内标，以验证整个工作流程的准确性。由于反渗透水对所有分析物都很洁净，因此校准标准用反渗透水制备。不同分析物的校准范围各不相同，从 1 毫微克/升到 1000 毫微克/升不等。所有分析物和提取的内标在所有强化水平下的回收率为标称浓度的 70% 至 130%。方法的精确度令人满意，%RSD 值低于 20%。为了进一步证明所建立的工作流程适用于对各种水基质中的目标 PFAS 进行准确定量，还对从各种源水中收集的其他饮用水和非饮用水进行了测试。

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