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Recent developments in the use of electrokinetic methods for rapid cell viability assessments and separations 使用电动方法快速评估和分离细胞活力的最新进展
Pub Date : 2024-10-16 DOI: 10.1016/j.jcoa.2024.100185
Blanca H. Lapizco-Encinas
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.
在临床分析、医疗保健、药物开发和食品安全等越来越多的领域中,快速细胞活力评估至关重要。事实证明,电动(EK)方法是分析细胞(包括活力评估)的可靠平台。本文讨论的是介电泳和电泳这两种电动力学现象的应用,它们可以根据细胞的活力状态来区分细胞,还可以将细胞分类并分离成有活力和无活力的细胞,以便进行进一步的分析。文中介绍了每种 EK 方法的工作原理,然后是简要的历史概述和对 2015 年至 2024 年间发表的最新报告的详细分析。结语包括对这篇综述文章内容的总结,并对基于 EK 的系统在根据细胞活力状态评估和分离细胞方面的预期进展提出了未来展望。
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引用次数: 0
Chiral and achiral analysis of chiral flavonoids with liquid and supercritical fluid chromatography – A review 利用液相色谱和超临界流体色谱对手性黄酮类化合物进行手性和非手性分析--综述
Pub Date : 2024-10-15 DOI: 10.1016/j.jcoa.2024.100183
Laurine Réset, Clément De Saint Jores, Caroline West
Flavonoids have been the topic of numerous studies for decades because they possess varied interesting bioactivities including e.g. 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.
几十年来,黄酮类化合物一直是众多研究的主题,因为它们具有各种有趣的生物活性,例如抗氧化和抗癌特性。特别是一些类黄酮具有手性特征,这是因为它们的苷元上存在一个或两个手性碳原子。它们包括黄烷、异黄烷、黄烷酮、黄烷壬醇、黄烷醇和呋喃壬醇。此外,在连接到苷元根部的碳水化合物基团上还可以观察到其他手性中心,但本文不考虑这些手性中心。不过,由于立体异构体通常具有不同的生物活性,针对这些特定类黄酮的分析方法应有助于更好地了解它们的作用模式和生物合成途径。在本综述中,我们研究了在液相(LC)和超临界相(SFC)中以非手性和手性模式分析手性类黄酮的色谱分析方法。报告中介绍了一维和二维方法,还研究了不同的检测模式。需要注意的是,本综述并不力求全面,而是展示当前方法的多样性和主要特点。
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引用次数: 0
A simplified tutorial on charged aerosol detection: Understanding the basics, optimization, and troubleshooting 带电气溶胶检测简明教程:了解基础知识、优化和故障排除
Pub Date : 2024-10-06 DOI: 10.1016/j.jcoa.2024.100181
Wesley W. Barnhart, Muhammad Qamar Farooq, Imad A. Haidar Ahmad
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.
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.
带电气溶胶检测器(CAD)测量沉积在气溶胶颗粒上的总电荷,产生与分析物质量成比例的信号,适用于带或不带发色团的化合物。CAD 的一个显著优点是,在没有真品标准的情况下,也能对多种非挥发性化合物进行定量,因为此类分析物的响应因子是一致的。CAD 还是帮助检测和/或定量紫外吸收差或无紫外吸收的化合物的重要工具。在本教程中,将演示 CAD 的基本原理及其使用、故障排除和维护,以确保正确使用 CAD。CAD 的成功操作包括优化功率函数值 (PFV),以获得更宽的动态范围并提高响应的一致性。在采用梯度分析方法时,使用反梯度(柱后混合)可实现更精确的定量。此外,还将介绍几种故障排除策略,包括诊断反梯度泵有机溶剂输送和确定反梯度泵与系统泵之间的体积匹配/不匹配,以及操作计算机辅助分析仪的重要方面。最后,为了确保可靠的结果,需要长期监控计算机辅助分析仪的性能,以了解其工作是否充分或是否需要维护。
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引用次数: 0
In vial thin-film solid-phase microextraction using silver nanoparticles as coating for the determination of phenols in waters 使用银纳米颗粒涂层的瓶内薄膜固相微萃取法测定水体中的酚类物质
Pub Date : 2024-10-06 DOI: 10.1016/j.jcoa.2024.100182
Alejandro Rodríguez-González , Ana I. Jiménez-Abizanda , Verónica Pino , Adrián Gutiérrez-Serpa
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 versus 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-1, 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.
本研究首次开发了一种新型薄膜固相微萃取(TF-SPME)装置,该装置基于内部涂有银纳米粒子(AgNPs)的玻璃瓶,并利用高效液相色谱-光电二极管阵列检测器(HPLC-PDA)测定了废水、瓶装水和灌溉水样品中的五种酚类物质。通过改变金属盐与还原剂的比例以及合成的 pH 值,合成了不同的 AgNPs。根据所使用的 AgNPs 类型和 AgNPs 层数,对 TF-SPME 玻璃瓶装置的制备进行了优化。此外,还优化了 TF-SPME 程序。TF-SPME 方法非常简单,只需加入 18 mL 水并搅拌 5 分钟,然后弃水并加入 750 µL 作为解吸溶剂,并直接进行 HPLC-PDA 进样。整个方法显示出良好的分析性能,检出限为 3 至 8 μg-L-1,日内和日间精密度(RSD)(均使用不同的样品瓶进行评估,因此显示出批次间精密度)分别为 8.70% 至 16.4%,6.0% 至 19.7%。TF-SPME-HPLC-PDA 程序与以前的酚类测定方法进行了比较,无论是在分析性能方面还是在采用不同指标进行绿色评估方面,都显示出明显的优势。
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引用次数: 0
Microchip gas chromatographic columns dedicated for space exploration: Stationary phase coating, setup optimization and evaluation of column performances 太空探索专用微型芯片气相色谱柱:固定相涂层、设置优化和色谱柱性能评估
Pub Date : 2024-10-05 DOI: 10.1016/j.jcoa.2024.100180
Arnaud Philippart , Valérie Peulon-Agasse , Malak Rizk-Bigourd , Audrey Boco-Simon , Gabin Bergerot , Guillaume Rioland , Arnaud Buch , Cyril Szopa , Pascal Cardinael
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-1 with k = 0.12 for the thinnest film and up to almost 4,000 plates.m-1 with k = 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.
这项工作是专门设计用于太空探索的气相色谱微柱项目的第一部分。特别是,这项研究探索了硅/玻璃微芯片气相色谱柱的功能化和表征,这种微芯片气相色谱柱设计成内部横截面为方形的蛇形通道。这种微型色谱柱可通过带有可拆卸毛细管接头的坚固流体歧管与传统气相色谱仪连接,或在用于太空探索的原型仪器中实施。首先,对台式气相色谱仪系统的进样器内衬体积、毛细管连接内径(I.D.)和检测数据频率进行了优化,以确保对色谱柱效率进行最佳评估。结果发现,内径为 100 μm 的连接毛细管、内径为 1.2 mm 的内衬和 100 Hz 的检测采集频率是最佳的设置和参数。此外,还降低了固定相的涂布速度,使色谱柱的效率提高了 100%。然后,比较了方形截面毛细管色谱柱与传统圆形截面色谱柱的性能。圆形和方形内部横截面的涂层效率分别为 55% 和 42%,这表明方形横截面对色谱柱的性能影响不大。在同一生产批次的不同微芯片上涂覆了 0.032 至 0.260 µm 不同厚度的固定相薄膜,以评估薄膜厚度对色谱性能的影响。微芯片的性能通过戈莱图进行评估,部分微芯片还通过光学显微镜进行了研究。结果表明,微芯片色谱柱的效率和保留能力与薄膜厚度密切相关(最薄的薄膜厚度为 9,000 板/米-1,k=0.12;最厚的薄膜厚度为 4,000 板/米-1,k=0.93)。最后,通过生产三个完全相同的微芯片,验证了镀膜工艺的可重复性,理论板平均数量的 RSD 为 4.8%。
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引用次数: 0
A method for suppressing pH excursion during elution in ion-exchange chromatography 一种抑制离子交换色谱法洗脱过程中 pH 值偏移的方法
Pub Date : 2024-09-23 DOI: 10.1016/j.jcoa.2024.100179
Raja Ghosh
A simple method for reducing pH excursion during salt-induced elution in cation exchange chromatography is presented in this paper. Connecting a preequilibrated anion exchange cartridge in series in front of the cation exchange device just prior to the elution step significantly reduced the transient decrease in pH that is typically observed during elution. The working principle of the proposed method is hypothesized. Bind and elute chromatography experiments showed that the suppression of pH excursion during elution of a monoclonal antibody from a cation exchange chromatography device resulted in significantly sharper and narrower eluted protein peaks. Improvement in pH control during elution would not only result in better reproducibility and efficiency in separation but would also ensure greater stability of pH sensitive proteins during their purification using ion exchange chromatography.
本文介绍了一种在阳离子交换色谱中减少盐诱导洗脱过程中 pH 值偏移的简单方法。在洗脱步骤之前,在阳离子交换装置前串联一个预平衡阴离子交换盒,可显著降低洗脱过程中通常会出现的 pH 值瞬时降低现象。现对拟议方法的工作原理进行假设。结合和洗脱色谱实验表明,抑制阳离子交换色谱装置洗脱单克隆抗体过程中的 pH 值偏移可使洗脱的蛋白质峰明显更清晰、更窄。改善洗脱过程中的 pH 值控制不仅能提高分离的重现性和效率,还能确保 pH 值敏感的蛋白质在使用离子交换色谱法纯化过程中具有更高的稳定性。
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引用次数: 0
Inverse gas chromatography fruitful and credible tool for materials characterization 反气相色谱法是富有成果的材料表征可靠工具
Pub Date : 2024-09-18 DOI: 10.1016/j.jcoa.2024.100177
Adam Voelkel, Beata Strzemiecka, Kasylda Milczewska, Katarzyna Adamska
Review contents the extensive insight into the last 10 years in the history of inverse gas chromatography (IGC). Although this technique seems to be well-known. Every year brings new proposals concerning the procedures enabling the deeper insights in the properties of the surfaces as well as the bulk of various materials. Meetings organized by the universities and commercial groups indicate the growing society of users. Different versions of IGC are most often used in following the changes of materials properties undergoing technological modifications and/or changes caused by the environment in which such material is applied.
The wide group of raw materials, minerals, pharmaceutical components, abrasive articles, cellulosic materials, bacteria biomass, ionic liquids, metal-organic frameworks (MOFs) as well as various hybrid materials were characterized by IGC. Here it is worth to indicate the properties of dentine and enamel during dental treatment or (on the other side) examination of the influence of various external parameters on the transport of gaseous compounds in different geologic materials. The advantages and challenges that arise during such experiments are presented and discussed.
回顾内容对反气相色谱法(IGC)过去 10 年的发展历程进行了广泛深入的剖析。尽管这项技术似乎已广为人知。但每年都有新的建议提出,这些建议有助于深入了解各种材料的表面和内部特性。由大学和商业团体组织的会议表明用户群体在不断扩大。不同版本的 IGC 最常用于跟踪材料特性在技术改造过程中的变化和/或由材料应用环境引起的变化。IGC 对多种原材料、矿物、药物成分、磨料、纤维素材料、细菌生物质、离子液体、金属有机框架 (MOF) 以及各种混合材料进行了表征。在此,值得指出的是牙科治疗过程中牙本质和珐琅质的特性,或(另一方面)研究各种外部参数对不同地质材料中气体化合物迁移的影响。本文介绍并讨论了此类实验中出现的优势和挑战。
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引用次数: 0
Evaluation of the presence of emerging contaminants in wastewater and seawater using automated solid-phase extraction and ultra-high-performance liquid chromatography coupled to tandem mass spectrometry 利用自动固相萃取和超高效液相色谱-串联质谱法评估废水和海水中新出现污染物的存在
Pub Date : 2024-09-17 DOI: 10.1016/j.jcoa.2024.100178
Julia Méndez-Catalán , Cristina Socas-Hernández , Gabriel Jiménez-Skrzypek , Javier Hernández-Borges , Javier González-Sálamo
The presence of emerging contaminants in water constitutes one of the main ways of human exposure to them, which can cause severe effects on health. In this sense, their adequate elimination through appropriate treatments plays a fundamental role, being necessary to monitor the effluents from wastewater treatment plants, as well as the areas close to their discharge. The aim of the present work has been the development and validation of an analytical methodology to determine 15 organic contaminants of emerging concern in wastewater as well as in seawater samples using an automated solid-phase extraction system and an ultra-high-performance liquid chromatography coupled to tandem mass spectrometry instrument. Matrix-matched calibration showed good linearity with determination coefficients ≥ 0.990. Likewise, matrix effect assessment showed a significant signal suppression in almost all the analytes demonstrating the need to consider such effect for a proper quantification of the analytes. Recovery values ranged from 74.7 to 109% with relative standard deviation values ≤ 20.5% for most analytes. Regarding seawater and wastewater samples, 11 of the target analytes were detected in, at least, one sample at concentrations from below limit of quantification of the method to 217 ± 92 ng l-1 in seawater and up to 2340 ± 107 ng l-1 in wastewater samples.
水中新出现的污染物是人类接触这些污染物的主要途径之一,会对健康造成严重影响。从这个意义上说,通过适当的处理方法充分消除这些污染物起着至关重要的作用,因此有必要对污水处理厂的污水以及污水排放附近的区域进行监测。本研究的目的是开发和验证一种分析方法,利用自动固相萃取系统和超高效液相色谱耦合串联质谱仪测定废水和海水样本中新出现的 15 种有机污染物。基质匹配校准显示出良好的线性关系,测定系数≥ 0.990。同样,基质效应评估显示,几乎所有的分析物都存在明显的信号抑制现象,这表明在对分析物进行适当定量时需要考虑基质效应。大多数分析物的回收率在 74.7%至 109%之间,相对标准偏差值小于 20.5%。在海水和废水样品中,至少有一个样品检测到了 11 种目标分析物,其浓度从低于方法的定量限到 217 ± 92 ng l-1(在海水中),以及高达 2340 ± 107 ng l-1(在废水中)。
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引用次数: 0
Retention factor variation on wide range of mobile phase compositions in reversed-phase high-performance liquid chromatography; a short tutorial 反相高效液相色谱法中宽范围流动相组成的保留因子变化;简明教程
Pub Date : 2024-09-14 DOI: 10.1016/j.jcoa.2024.100176
Victor David , Serban C. Moldoveanu

Mobile phase composition remains the major experimental parameter influencing the separation process in reversed-phase high-performance liquid chromatography (RP-HPLC). Its influence on the retention of solutes is explained by the Hildebrand solubility parameter and solvophobic theory, which also considers molecular characteristics of the participants in a separation process. The main empirical dependences (linear and polynomial) between the retention factor and the composition of mobile phase (retention function) are discussed taking into consideration a wide range of mobile phase compositions. Two direct chromatographic indices are resulting from these equations: the extrapolated value of retention factor for zero organic content in mobile phase composition (log kw) and the solvent strength parameter (S), which for a linear retention function is its slope being constant over the entire mobile phase compositions. Another chromatographic index could result from the retention function for zero content of water in mobile phase, but this situation can be applied only for very hydrophobic solutes. For large domains of mobile phase composition, the retention function cannot be described by a single type of dependence. This explains the paradox of generating by extrapolation different logkwvalues for different organic components. For the mobile phase close to pure water the retention function is different from that at average water concentration.

流动相组成仍然是影响反相高效液相色谱分离过程的主要实验参数。希尔德布兰德溶解度参数和疏溶理论解释了流动相组成对溶质保留的影响,该理论还考虑了分离过程中参与者的分子特性。考虑到流动相组成的广泛范围,讨论了保留因子与流动相组成(保留函数)之间的主要经验依赖关系(线性和多项式)。从这些公式中可以得出两个直接的色谱指数:流动相组成中有机物含量为零时保留因子的推断值(log kw)和溶剂强度参数(S),对于线性保留函数而言,其斜率在整个流动相组成中保持不变。另一个色谱指标可能来自流动相中水含量为零时的保留因子,但这种情况仅适用于非常疏水的溶质。对于流动相组成的大范围,保留功能无法用单一类型的依赖关系来描述。这就解释了为什么不同的有机成分会通过外推法产生不同的对数kw值。对于接近纯水的流动相,保留功能与平均水浓度下的保留功能不同。
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引用次数: 0
Determination and identification of polyphenols in wine using mass spectrometry techniques 利用质谱技术测定和鉴定葡萄酒中的多酚
Pub Date : 2024-09-14 DOI: 10.1016/j.jcoa.2024.100175
Azamat Temerdashev , Sanka N. Atapattu , Geethi K. Pamunuwa

Mass spectrometry is crucial for analysing physicochemical and sensory properties, including colour, astringency, taste, and flavour, predicting ageing characteristics, and addressing stability issues in wine. Polyphenols are key chemical constituents in wine that are associated with health benefits and improve circulatory conditions. Advances in mass spectrometry ionisation techniques such as matrix-assisted laser desorption and ionisation and direct analysis in real-time offer high sensitivity for identifying important polyphenolic constituents in wine. High-resolution mass spectrometry, in combination with liquid chromatography, accurately identify and quantify polyphenolic compounds, even at low concentrations, and provides the possibility for further retrospective analysis and non-targeted analysis using statistical methods of data analysis. Ambient mass spectrometry techniques such as paper spray and low-temperature plasma allow solventless analysis, determining the geographical origin, authentication, and quality control of wine samples. This review will explore the potential benefits of using mass spectrometry to identify various polyphenols and polymeric polyphenols in wine, as well as recent developments and applications. Additionally, we will discuss determining antioxidant activity and total polyphenol content in wine.

质谱分析法对于分析葡萄酒的理化和感官特性(包括颜色、涩味、口感和风味)、预测陈酿特性和解决稳定性问题至关重要。多酚是葡萄酒中的主要化学成分,对健康有益并能改善循环系统状况。基质辅助激光解吸电离和实时直接分析等质谱电离技术的进步为鉴定葡萄酒中的重要多酚成分提供了高灵敏度。高分辨率质谱法与液相色谱法相结合,可准确鉴定和量化多酚类化合物,即使是低浓度的多酚类化合物,并可利用数据分析统计方法进行进一步的回顾性分析和非针对性分析。纸喷雾和低温等离子体等环境质谱技术可以进行无溶剂分析,确定葡萄酒样品的地理来源、认证和质量控制。本综述将探讨使用质谱技术鉴定葡萄酒中各种多酚和聚合多酚的潜在益处,以及最近的发展和应用。此外,我们还将讨论如何确定葡萄酒中的抗氧化活性和总多酚含量。
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引用次数: 0
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Journal of chromatography open
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