IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-05-10 Epub Date: 2026-03-07 DOI: 10.1016/j.chroma.2026.466886

Olga Vyviurska , Rocio Vidal Pellegrino , František Dugovič , Dominika Sklenárová , Ivan Špánik

In recent years, the application of flow-modulated comprehensive two-dimensional gas chromatography (FM-GC × GC) has significantly increased, particularly for profiling complex food volatilomes. However, the full potential of this technique is often hindered by the complexity of instrumental optimisation, which is critical for achieving high-resolution separation across a wide variety of analytes in diverse samples. This work addresses this challenge by developing a predictive strategy to optimise FM-GC × GC conditions for the separation of a wide variety of volatile compounds. The efficiency of a local model based on peak parameters was tested across four different column setups, monitoring its correlation to the separation of 22 critical coeluting pairs. Using a Doehlert experimental design and a General Linear Model (GLM) approach, robust predictive models (R² > 0.80) were established and validated. Although the predictive models are confined to the tested experimental space, the underlying strategy and observed general behaviours provide a transferable framework for other setups. The use of a multiresponse optimisation strategy coupled to a global resolution metric, the Fraction of Resolved Peaks (FRP), successfully improved the separation of coelutions, particularly for specific column configurations. The effectiveness of this workflow was ultimately demonstrated by its successful application to the complex volatilomes of wine, honey, cascara coffee tea, and masala tea.

近年来，流量调制综合二维气相色谱法（FM-GC × GC）在分析复杂食品挥发物方面的应用显著增加。然而，该技术的全部潜力往往受到仪器优化的复杂性的阻碍，这对于在不同样品中实现各种分析物的高分辨率分离至关重要。这项工作通过开发一种预测策略来优化各种挥发性化合物分离的FM-GC × GC条件，从而解决了这一挑战。基于峰值参数的局部模型的效率在四种不同的柱设置中进行了测试，并监测了其与22个关键coeloling对分离的相关性。采用Doehlert实验设计和一般线性模型（GLM）方法，建立并验证了鲁棒预测模型（R²> 0.80）。虽然预测模型仅限于测试的实验空间，但潜在策略和观察到的一般行为为其他设置提供了可转移的框架。使用多响应优化策略与全局分辨率度量相结合，即分解峰的分数（FRP），成功地提高了分离度，特别是对于特定的柱配置。该工作流程的有效性最终通过其成功应用于葡萄酒，蜂蜜，卡斯卡拉咖啡茶和马沙拉茶的复杂挥发物而得到证明。

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引用次数: 0

Archaea synthesize heterochiral phospholipid membranes as revealed by chiral analysis of archaeols 古菌的手性分析表明，古菌可合成杂手性磷脂膜。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-05-10 Epub Date: 2026-03-01 DOI: 10.1016/j.chroma.2026.466853

Walter Hofmann , Andrea Palyzová , Jan Jansa , Nika Pende , Simon K.-M.R. Rittmann , Tomáš Řezanka

This study comprehensively characterizes structural diversity of archaeol lipids in selected archaeal genera, integrating available genomic information with advanced lipidomic and stereochemical analyzes. Study of genomes from six archaeal genera revealed the presence of key enzymes involved in glycerophosphate biosynthesis, namely glycerol-1-phosphate dehydrogenase and glycerol-3-phosphate dehydrogenase. Their coexistence in some of the studied strains suggests the ability of these organisms to synthesize both enantiomeric forms of glycerol phosphates. Shotgun lipidomic profiling confirmed the presence of saturated and unsaturated archaeols, including extended forms (C20–C25), hydroxyarchaeols, and tetraether lipids, especially in the species Haloferax volcanii, Methanopyrus kandleri, and Sulfolobus acidocaldarius. Using on-line 2D LC-MS/MS, a specific molecular species of archaeol (20:3–25:4-AR) with seven double bonds was identified in H. volcanii, while bis-extended archaeol (C25–C25) was not detected. Chiral HPLC of a commercial archaeol standard resolved four isomers, with the (R)-2,3-di-O-phytanyl-sn-glycerol stereoisomer being the most abundant (> 80 %). In four of our archaeal strains a minor S enantiomer was present at concentrations of 6.8–13.9 % relative to the main R isomer, and its presence coincided with the presence of both glycerol phosphate dehydrogenases in the respective genomes. The distribution of these isomers across the studied strains supports the coexistence of both R- and S- enantiomers of archaeols in some, but not all, archaeal lineages. These findings highlight the stereochemical and structural complexity of archaeal membrane lipids and provide new insights into their biosynthetic diversity.

本研究综合了已有的基因组信息和先进的脂质组学和立体化学分析，全面表征了选定古菌属中古醇脂质的结构多样性。对6个古细菌属基因组的研究发现，存在参与甘油磷酸生物合成的关键酶，即甘油-1-磷酸脱氢酶和甘油-3-磷酸脱氢酶。它们在某些研究菌株中的共存表明这些生物有能力合成两种对映体形式的甘油磷酸。散弹枪脂质组学分析证实了饱和古醇和不饱和古醇的存在，包括扩展形式（C20-C25），羟基古醇和四醚类脂质，特别是在Haloferax volcanii， Methanopyrus kandleri和Sulfolobus acidocalarius物种中。利用在线二维LC-MS/MS，在H. volcanii中鉴定出具有7个双键的古酚（20:3-25:4-AR），而未检测到双延伸古酚（C25-C25）。手性高效液相色谱法测定了4种异构体的含量，其中(R)-2,3-二- o -植烷- n-甘油立体异构体含量最多（约80%）。在我们的四株古细菌菌株中，相对于主要的R异构体，存在一个次要的S对映体，其浓度为6.8- 13.9%，其存在与各自基因组中磷酸甘油脱氢酶的存在一致。这些异构体在研究菌株中的分布支持了古菌R-和S-对映体在一些（但不是全部）古菌谱系中共存。这些发现突出了古细菌膜脂的立体化学和结构复杂性，并为其生物合成多样性提供了新的见解。

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引用次数: 0

Chiral derivatization reagents for enantioselective LC-MS/MS analysis of amino acids with analyte-specific fragmentation 用于氨基酸对映选择性LC-MS/MS分析的手性衍生化试剂

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-05-10 Epub Date: 2026-02-28 DOI: 10.1016/j.chroma.2026.466851

Tatsuya Sakamoto, Kana Ishikura, Mayu Onozato, Takeshi Fukushima

Accurate enantioselective analysis of amino acids by liquid chromatography-tandem mass spectrometry (LC–MS/MS) remains challenging, as existing derivatization strategies often compromise either chromatographic resolution or structural discrimination in tandem mass spectrometry. In this study, we developed novel chiral derivatization reagents, (R)- and (S)-Oqic, based on a 1,3-oxazinoquinoline-4-one scaffold, for the simultaneous determination of amino acid enantiomers via LC–MS/MS. The reagents reacted rapidly with amino acids under mild basic conditions to form their chiral derivatives, enabling the simultaneous separation of 37 amino acids (18 pairs of amino acid enantiomers and Gly) on a conventional ODS column within 16 min. The resulting derivatives exhibited unique fragmentation patterns, yielding characteristic fragment ions at m/z 190 and [M + H − 171], with intensity ratios dependent on the tagged amino acid, thereby facilitating reliable analyte discrimination. The method was validated and subsequently applied to the analysis of commercially available fermented dairy products, revealing the presence of d-Ala, d-Ser, d-Asp, d-Glu, and d-Arg in yogurt and a probiotic beverage. The detection of sweet-tasting d-amino acids (d-Ala, d-Ser, and d-Arg) suggests their potential contribution to the sensory properties of fermented foods. Overall, the developed Oqic-based method provides a powerful tool for elucidating bacterial metabolism and food flavor profiles.

液相色谱-串联质谱（LC-MS /MS）对氨基酸进行精确的对映选择性分析仍然具有挑战性，因为现有的衍生化策略通常会损害串联质谱的色谱分辨率或结构辨别。在这项研究中，我们开发了新的手性衍生试剂(R)-和(S)- oqic，基于1,3-恶嗪喹啉-4- 1支架，用于通过LC-MS /MS同时测定氨基酸对映体。该试剂与氨基酸在温和的碱性条件下快速反应形成手性衍生物，在常规ODS色谱柱上可在16 min内同时分离37种氨基酸（18对氨基酸对映体和Gly）。所得到的衍生物显示出独特的碎片模式，在m/z 190和[m + H−171]处产生特征碎片离子，其强度比取决于所标记的氨基酸，从而促进了可靠的分析物鉴别。该方法经过验证并随后应用于市售发酵乳制品的分析，揭示了酸奶和益生菌饮料中d-Ala， d-Ser, d-Asp， d-Glu和d-Arg的存在。甜味d-氨基酸（d-Ala， d-Ser和d-Arg）的检测表明它们对发酵食品的感官特性有潜在的贡献。总之，开发的基于oqic的方法为阐明细菌代谢和食物风味谱提供了一个强大的工具。

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引用次数: 0

Metal-organic framework MIL-101(Cr) functionalized β-cyclodextrin-modified magnetic multi-walled carbon nanotubes for efficient extraction of amphenicol antibiotics 金属有机骨架MIL-101（Cr）功能化β-环糊精修饰磁性多壁碳纳米管高效提取抗生素

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-05-10 Epub Date: 2026-03-06 DOI: 10.1016/j.chroma.2026.466882

Lin Lv , Hongmei Liu , Tao Song , Yan Zhao

Given the extensive use of amphenicol antibiotics and their potential adverse effects on human health, the development of simple and highly sensitive detection methods is essential to ensure food safety. In this work, a novel and highly efficient magnetic sorbent based on β-cyclodextrin-modified magnetic multi-walled carbon nanotubes functionalized with MIL-101(Cr) (Fe₃O₄@β-CD@MWCNTs@MIL-101(Cr)) was developed and combined with ultra-high-performance liquid chromatography-mass spectrometry (UHPLC-MS/MS) to achieve highly sensitive detection of three amphenicol antibiotics (chloramphenicol, thiamphenicol, and florfenicol) in honey samples. The key factors influencing extraction efficiency in the magnetic solid-phase extraction process were identified using the Plackett-Burman experimental design, whereas the optimal experimental conditions were determined through Box-Behnken design-based response surface methodology optimization. Under these optimized conditions, favorable linear relationships for amphenicol antibiotics were observed within the concentration range of 0.5–250 ng mL⁻¹ (R² ≥ 0.9951). The method exhibited detection limits of 0.04–0.07 μg kg⁻¹. Recovery rates ranged from 83.2% to 97.9%, with intra-day and inter-day precisions both below 7.2%. This method provides an efficient tool for monitoring amphenicol antibiotics in complex matrices.

鉴于氨霉素抗生素的广泛使用及其对人类健康的潜在不利影响，开发简单和高度敏感的检测方法对于确保食品安全至关重要。本研究基于MIL-101（Cr）功能化的β-环糊精修饰磁性多壁碳纳米管（Fe3O4@β-CD@MWCNTs@MIL-101(Cr)）制备了一种新型高效磁性吸附剂，并结合超高效液相色谱-质谱联用（UHPLC-MS/MS），实现了蜂蜜样品中氯霉素、硫霉素和氟苯尼考三种抗生素的高灵敏度检测。采用Plackett-Burman实验设计确定了磁固相萃取过程中影响萃取效率的关键因素，并采用基于Box-Behnken设计的响应面法优化确定了最佳实验条件。在此优化条件下，在0.5 ~ 250 ng mL−1的浓度范围内，抗生素用量呈良好的线性关系（R2≥0.9951）。方法检出限为0.04 ~ 0.07 μg kg−1。回收率为83.2% ~ 97.9%，日内、日间精密度均低于7.2%。该方法为复杂基质中抗生素的监测提供了一种有效的工具。

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引用次数: 0

Revisiting the definition and measurement of total accessible and hold-up volumes in liquid chromatography: Current understanding and advances 重新审视液相色谱中总可接近体积和持有体积的定义和测量：当前的理解和进展。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-05-10 Epub Date: 2026-02-27 DOI: 10.1016/j.chroma.2026.466849

Judith Mollen , Gert Desmet , Deirdre Cabooter

The accurate determination of the retention factor, and particularly, the determination of the mobile phase volume that is needed for its computation, remains a fundamental, yet highly-debated topic in liquid chromatography. Two main approaches currently co-exist in literature: i) one based on the total accessible volume (= the total column volume accessible for solvent molecules after bonded phase coating) and ii) one based on the mobile phase volume that is accessible to unretained analytes (the hold-up volume). This review provides a clear graphical definition for both volumes and subsequently critically examines their use in current literature and reviews their methods of determination, emphasizing the need for careful experimental practice and standardized, universally accepted definitions. By comparing traditional experimental methods with findings from molecular dynamics simulations and Monte Carlo method studies, this review furthermore aims to clarify ambiguities and recommend best practices for future research. In addition, a comprehensive table linking the different names, symbols and definitions that have been used throughout literature to denote the different mobile phase volumes is provided, to help researchers navigate literature more easily.

保留因子的准确测定，特别是计算其所需的流动相体积的测定，仍然是液相色谱中一个基本的，但又备受争议的话题。目前文献中存在两种主要方法：i)一种基于总可接触体积（=键合相涂层后溶剂分子可接触的总柱体积），ii)一种基于未保留分析物可接触的流动相体积（保持体积）。这篇综述为这两卷提供了一个清晰的图形定义，随后批判性地检查了它们在当前文献中的使用，并回顾了它们的测定方法，强调需要仔细的实验实践和标准化，普遍接受的定义。通过比较传统的实验方法与分子动力学模拟和蒙特卡罗方法的研究结果，进一步澄清歧义，并为未来的研究提供最佳实践建议。此外，还提供了一个综合表，链接了整个文献中用于表示不同流动相卷的不同名称、符号和定义，以帮助研究人员更容易地浏览文献。

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引用次数: 0

Integrating natural deep eutectic solvents and ionic liquids as green mobile phase additives for enhanced selenium speciation analysis in food samples by liquid chromatography-atomic fluorescence spectrometry 结合天然深共晶溶剂和离子液体作为绿色流动相添加剂，液相色谱-原子荧光光谱法增强食品样品中硒的形态分析。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-05-10 Epub Date: 2026-02-28 DOI: 10.1016/j.chroma.2026.466844

María B. Botella , María N. Oviedo , Rodolfo G. Wuilloud

A study to evaluate the effects of natural deep eutectic solvent (NADES) and ionic liquids (ILs) on the separation of selenium (Se) species by reversed phase high performance liquid chromatography and detection by hydride generation atomic fluorescence spectrometry (RP-HPLC-HG-AFS) was performed in this work. The NADESs choline chloride:ethylene glycol and choline chloride:glycerol were applied as mobile phase additives for the separation of Se(IV), Se(VI), selenomethionine (SeMet) and Se-methylselenocysteine (SeMetSeCys). The effects of NADES composition, molar ratio, and concentration on chromatographic performance were systematically investigated, along with the influence of pH, buffer strength, and flow rate. The combined use of NADESs with the IL 1-hexyl-3-methylimidazolium chloride ([C₆mim]Cl) significantly enhanced the resolution of inorganic Se species. In addition, the effects of NADES and IL on the Se fluorescence signals obtained with the HG-AFS techniques were also studied using a multivariate technique for sensitivity optimization. The method achieved limits of detection of 1.59–2.78 µg L^-1, with relative standard deviations of 0.53–1.86 % for retention times and 1.23–1.72 % for peak areas. Finally, the proposed analytical method was successfully applied to Se speciation analysis in complex food samples, including nuts and Se-enriched garlic, yielding recoveries of 93.4–106 %.

本文研究了天然深共晶溶剂（NADES）和离子液体（ILs）对反相高效液相色谱法分离硒（Se）和氢化物发生原子荧光光谱法（RP-HPLC-HG-AFS）检测的影响。采用NADESs氯化胆碱：乙二醇和氯化胆碱：甘油作为流动相添加剂分别分离硒（IV）、硒（VI）、硒代蛋氨酸（SeMet）和硒甲基硒半胱氨酸（SeMetSeCys）。系统地研究了NADES的组成、摩尔比和浓度对色谱性能的影响，以及pH、缓冲液强度和流速的影响。NADESs与IL - 1-己基-3-甲基咪唑氯（[C6mim]Cl）的联合使用显著提高了无机硒的分辨率。此外，还利用多元灵敏度优化技术研究了NADES和IL对HG-AFS技术获得的Se荧光信号的影响。方法的检出限为1.59 ~ 2.78µg L-1，保留时间的相对标准偏差为0.53 ~ 1.86%，峰面积的相对标准偏差为1.23 ~ 1.72%。最后，该方法成功地应用于坚果和富硒大蒜等复杂食品样品的硒形态分析，回收率为93.4 ~ 106%。

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引用次数: 0

Recent advances in greener alternative solvents for reversed-phase liquid chromatography in pharmaceutical analysis 药物分析中反相液相色谱绿色替代溶剂的研究进展

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-05-10 Epub Date: 2026-02-27 DOI: 10.1016/j.chroma.2026.466847

Haile Kassahun , Ann Van Schepdael , Erwin Adams

Reversed-phase liquid chromatography (RP-LC) is widely used in pharmaceutical analysis, often relying on traditional organic solvents which present significant environmental and health risks. As a result, the growing demand for sustainable analytical practices has led to the development of eco-friendly solvents for RP-LC. This review discusses recent developments in the application of greener alternative solvents, such as ethanol, glycerol, dimethyl carbonate, cyrene, acetone, propylene carbonate, ionic liquids, propylene glycol, deep eutectic solvents, and surfactants, in pharmaceutical analysis using RP-LC. The review also highlights the potential of these greener solvents to replace conventional ones in the analysis of pharmaceuticals. Overall, green solvents can achieve analytical performance comparable to traditional methods while significantly reducing environmental burden and health risks. The limitations and practical strategies to overcome the challenges are also discussed.

反相液相色谱法（RP-LC）在药物分析中应用广泛，通常依赖于传统的有机溶剂，存在重大的环境和健康风险。因此，对可持续分析实践日益增长的需求导致了RP-LC的环保溶剂的发展。本文综述了近年来乙醇、甘油、碳酸二甲酯、癸烯、丙酮、碳酸丙烯、离子液体、丙二醇、深度共晶溶剂和表面活性剂等绿色替代溶剂在RP-LC药物分析中的应用进展。这篇综述还强调了这些绿色溶剂在药物分析中取代传统溶剂的潜力。总体而言，绿色溶剂可以实现与传统方法相当的分析性能，同时显着减少环境负担和健康风险。并讨论了其局限性和克服挑战的实用策略。

引用次数: 0

Development of a magnetic core–shell adsorbent-based microextraction method for the determination of pesticide residues in edible vegetables 磁核-壳吸附微萃取法测定食用蔬菜中农药残留。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-05-10 Epub Date: 2026-02-23 DOI: 10.1016/j.chroma.2026.466839

Sina Mohammad Mehri , Mohammad Reza Afshar Mogaddam , Mir Ali Farajzadeh , Mahboob Nemati

For the first time, a new magnetic core-shell adsorbent (synthesized from Fe₃O₄, mercaptoacetic acid, and hexamethylene diamine) was introduced for the effective extraction of pesticide residues from agricultural products, including cucumber, tomato, and zucchini. The structural and magnetic characteristics of the synthesized adsorbent were fully confirmed through a series of instrumental techniques such as Fourier transform infrared spectrometry, scanning electron microscopy, Brunauer-Emmett-Teller, thermogravimetric analysis, X-ray diffraction, transmission electron microscopy, energy dispersive X-ray, vibrating sample magnetometer, and zeta-potential analysis. The combination of dispersive micro solid phase extraction with dispersive liquid–liquid microextraction enabled a highly efficient two-step sample preparation protocol with minimal solvent consumption and rapid operation. Due to the magnetic nature of the adsorbent, phase separation was rapidly achieved using an external magnet, eliminating the need for repeated centrifugation and significantly reducing extraction time. The optimized procedure utilized only 3 mg of the sorbent and μL volumes of environmentally benign organic solvents, making the method green and cost-effective. Under the optimized conditions, the method achieved excellent analytical performance, including low detection limits (0.31–2.65 µg L⁻¹), wide linear ranges, good repeatability (relative standard deviations of 1.1–6.3%), high enrichment factors (225–480), and acceptable extraction recoveries (45–96%). The method was successfully applied to real agricultural matrices, and relative recoveries within the 80–120% range confirmed the absence of significant matrix effects. Altogether, this study highlighted a powerful and innovative analytical platform that offered high sensitivity, selectivity, and operational simplicity for the determination of pesticide residues in complex food samples.

以Fe₃O₄、巯基乙酸、己二胺为原料合成了一种新型磁性核壳吸附剂，用于黄瓜、番茄、西葫芦等农产品中农药残留的有效提取。通过傅里叶变换红外光谱、扫描电镜、布鲁诺尔-埃米特-泰勒、热重分析、x射线衍射、透射电镜、能量色散x射线、振动样品磁强计、ζ电位分析等一系列仪器技术，充分证实了合成吸附剂的结构和磁性。分散微固相萃取与分散液液微萃取相结合，实现了一种高效的两步制样方案，溶剂消耗少，操作快速。由于吸附剂的磁性，使用外部磁铁可以快速实现相分离，从而无需重复离心并显着缩短提取时间。优化后的方法只需要3 mg的吸附剂和μL的环保有机溶剂，使该方法具有绿色和经济效益。在优化条件下,该方法实现出色的性能分析,包括低检测范围(0.31 - -2.65µg L⁻¹),线性范围宽,可重复性好(相对标准偏差为1.1 -6.3%),高浓缩因素(225 - 480),和可接受的提取复苏(45 - 96%)。该方法成功地应用于实际农业基质中，相对回收率在80 ~ 120%范围内，证实该方法不存在明显的基质效应。总之，本研究突出了一个强大的和创新的分析平台，为复杂食品样品中农药残留的测定提供了高灵敏度、选择性和操作简便。

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引用次数: 0

Feed injection–enabled reversed phase liquid chromatography for simplified analysis of lipophilic drugs and formulations 进料进样反相液相色谱法用于亲脂性药物和制剂的简化分析

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-05-10 Epub Date: 2026-03-07 DOI: 10.1016/j.chroma.2026.466887

Daniel Foshag , Stephan Buckenmaier , Patrik Petersson

Strong sample solvents and lipidic excipients hamper reversed‑phase (RP) liquid chromatography (LC) analysis of lipid‑based pharmaceutical formulations by causing solvent mismatch, resulting in peak distortion and restricting the applicable injection volume, which ultimately reduces the sensitivity to detect impurities. In this work, we evaluated feed injection (FI) under gradient conditions for the analysis of sesame oil-based formulations dissolved in ethyl acetate (EtOAc) and integrated FI with two‑dimensional LC coupled to mass spectrometry (2D‑LC/MS) for impurity profiling. Findings were compared to conventional flow‑through injection (FTI) and sandwich injection, across injection volumes of 1–40 µL. FI at low feed flow fractions (≤ 5 % of mobile phase flow rate) provided ≥ 1:20 online dilution, sustaining column head focusing, and preserving peak shape and linearity across the full injection range. In contrast, higher feed flow fractions (≥ 20 % of the mobile phase flow rate, ≤ 1:5 dilution) resulted in severe fronting peaks and non-linear ultraviolet (UV) detector response. Finally, the ²D transfers resolved matrix‑ and Active Pharmaceutical Ingredient (API)‑related impurities without laborious offline reconstitution or dilution. This work extends the application field of FI from analyte diluents to complex lipid matrices, offering a robust, scalable workflow for pharmaceutical formulation analysis.

强样品溶剂和脂质赋形剂阻碍了反相（RP）液相色谱（LC）对脂质药物配方的分析，导致溶剂错配，导致峰畸变，限制了适用的进样量，最终降低了检测杂质的灵敏度。在这项工作中，我们评估了梯度条件下进料注射（FI）用于分析溶解在乙酸乙酯（EtOAc）中的芝麻油基配方，并将FI与二维LC - LC/MS （2D - LC/MS）相结合用于杂质分析。研究结果与传统的流式注射（FTI）和夹心注射进行了比较，注射量为1-40µL。低进料流量分数（≤5%流动相流量）的FI提供≥1:20的在线稀释，维持柱头聚焦，并在整个进样范围内保持峰形和线性。相比之下，较高的进料流量（≥20%的流动相流量，≤1:5的稀释度）导致了严重的前峰和非线性紫外（UV）检测器响应。最后，二维转移分解了基质和活性药物成分（API）相关的杂质，而无需费力的离线重构或稀释。这项工作将FI的应用领域从分析物稀释剂扩展到复杂的脂质基质，为药物配方分析提供了一个强大的、可扩展的工作流程。

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引用次数: 0

Analysis of bio-nano interactions by electrical asymmetric flow field-flow fractionation with multiple online detectors 生物纳米相互作用的电不对称流场-多在线检测器流分馏分析

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-05-10 Epub Date: 2026-03-05 DOI: 10.1016/j.chroma.2026.466879

Panida Punnabhum , Karim Daramy , Napaporn Roamcharern , Caterina Minelli , Yiwen Pei , Nelli Chourmouziadi Laleni , Yvonne Perrie , Zahra Rattray

Understanding bio-nano interactions and protein corona formation is critical for advancing nanomedicines towards clinical translation. However, conventional methods for nanoparticle analysis have limited utility for in situ analysis due to interference from unbound proteins present in bulk biological media. Electrical asymmetric flow field-flow fractionation (EAF4), which integrates AF4 with an applied electrical field, enables size and surface charge-based separation, and when coupled with online detectors, provides simultaneous measurement of particle size, electrophoretic mobility, and zeta potential, key parameters governing bio-nano interactions. Here, we report the first application of multiplexed EAF4 with online detection for evaluating biophysical changes occurring in polystyrene latex and silk nanoparticles, used as model nanomedicine systems, following exposure to serum under conditions that mimic the protein composition of cell culture media. Our findings reveal significant alterations in particle physical attributes, including particle size, shape factor, zeta potential, and electrophoretic mobility following exposure to protein-containing media. Furthermore, we demonstrate that EAF4 enables gentle fractionation of complex biological samples, providing comprehensive physicochemical profiling of diverse particulate and macromolecular species within nanoparticle–protein complexes. This work establishes EAF4 as a powerful analytical platform for resolving nano–bio interactions and guiding the rational design of next-generation nanomedicines.

了解生物纳米相互作用和蛋白质电晕的形成对于推进纳米药物走向临床翻译至关重要。然而，传统的纳米颗粒分析方法由于存在于散装生物介质中的未结合蛋白质的干扰，对原位分析的效用有限。电不对称流场-流分选（EAF4）将AF4与应用电场相结合，实现了基于尺寸和表面电荷的分离，当与在线检测器相结合时，可以同时测量粒径、电泳迁移率和zeta电位，这些都是控制生物纳米相互作用的关键参数。在这里，我们报告了多重EAF4在线检测的首次应用，用于评估在模拟细胞培养基蛋白质组成的条件下暴露于血清中发生的生物物理变化，这些变化被用作模型纳米药物系统。我们的研究结果揭示了暴露于含蛋白质介质后颗粒物理属性的显著变化，包括颗粒大小、形状因子、zeta电位和电泳迁移率。此外，我们证明EAF4能够温和地分离复杂的生物样品，提供纳米颗粒-蛋白质复合物中不同颗粒和大分子物种的全面物理化学分析。这项工作建立了EAF4作为一个强大的分析平台来解决纳米生物相互作用和指导下一代纳米药物的合理设计。

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引用次数: 0

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