Journal of Chromatography A最新文献_第6页

Multiresidue determination of alkylamines and alkylamides in meat by liquid chromatography high-resolution mass spectrometry and implications for food safety 液相色谱-高分辨率质谱法测定肉类中烷基胺和烷基酰胺的多残留及其对食品安全的影响。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-12-19 DOI: 10.1016/j.chroma.2025.466642

Ling Liu , Yizhe Zhu , Zitao Chai , Ruifen Zheng , Zhiqiang Zeng , Caiming Tang

This study developed a rapid and reliable liquid chromatography high-resolution mass spectrometry (LC-HRMS) method for the simultaneous determination of 8 alkylamines and 12 alkylamides in meat products. Sample preparation and instrumental conditions were optimized to achieve efficient extraction and accurate quantification. Meat samples were extracted with methanol-acetonitrile mixture (1:1, v/v) using vortex-ultrasonication for 15 min, followed by evaporation and reconstitution prior to analysis. The mobile phases were ultrapure water containing 0.1 % formic acid and acetonitrile, and a gradient elution program was employed. Mass spectrometric analysis was performed in positive electrospray ionization mode with full scan and data-dependent acquisition. Quantification was carried out using an internal standard method. The limits of quantification were 5 ng/g, and calibration curves showed good linearity. Recoveries ranged from 85.2 % to 103.0 % with relative standard deviations (RSDs) of 0.3–8.0 %, and matrix effects ranged from 61.7 % to 109.6 % with RSDs of 0.2–10.3 %. The method was successfully applied to meat samples collected from local markets, with concentrations of individual alkylamines and alkylamides ranging from below the detection limit to 13,105.0 ng/g. Migration experiments indicated that alkylamines and alkylamides could transfer from plastic materials into meat, with migration extent increasing with the increase of contact time and temperature. Hydrophobic alkylamides migrated more rapidly in early stage, while some alkylamines continued to migrate at low temperatures, indicating that meat characteristics and contact conditions could significantly affect the migration. The developed method is suitable for the determination of alkylamines and alkylamides in meat products, and can provide a reference approach for assessing the potential migration and exposure risks of alkylamines and alkylamides.

本研究建立了一种快速可靠的液相色谱-高分辨率质谱（LC-HRMS）同时测定肉制品中8种烷基胺和12种烷基酰胺的方法。优化了样品制备和仪器条件，以实现高效提取和准确定量。肉类样品用甲醇-乙腈混合物（1:1,v/v）涡流超声提取15min，蒸发重构后分析。流动相为含0.1%甲酸和乙腈的超纯水，采用梯度洗脱程序。质谱分析在正电喷雾电离模式下进行，具有全扫描和数据依赖采集。采用内标法进行定量。定量限为5 ng/g，校准曲线线性良好。加样回收率为85.2% ~ 103.0%，相对标准偏差为0.3 ~ 8.0%；基质效应为61.7% ~ 109.6%，相对标准偏差为0.2 ~ 10.3%。该方法成功应用于从本地市场收集的肉类样本，个别烷基胺和烷基酰胺的浓度从低于检出限至13,105.0 ng/g不等。迁移实验表明，烷基胺和烷基酰胺可以从塑料材料转移到肉中，迁移程度随着接触时间和温度的增加而增加。疏水烷基胺在早期迁移速度较快，而部分烷基胺在低温下仍在迁移，说明肉类特性和接触条件对迁移有显著影响。该方法适用于肉制品中烷基胺和烷基酰胺的检测，可为评估烷基胺和烷基酰胺的潜在迁移和暴露风险提供参考方法。

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引用次数: 0

Decoding diastereomeric and impurity profiles of phosphorothioated siRNAs via 2D anion-exchange chromatography coupled with ion-pair reversed phase liquid chromatography mass spectrometry 通过二维阴离子交换色谱和离子对反相液相色谱质谱法解码磷酸化sirna的非对映异构体和杂质谱。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-12-18 DOI: 10.1016/j.chroma.2025.466639

Quang-Dong Bui , Willy Verluyten , Bart Noten , Tiny Deschrijver , Sebastiaan Eeltink

Phosphorothioate (PS) modifications are widely used in RNA-based therapeutic oligonucleotides (ONs), forming diastereomers that enhance ON stability, bioavailability, and cellular uptake. This study presents a strategy for profiling PS-ONs, including both duplexes and the respective single sense and antisense-strand components using anion-exchange chromatography (AEX). The impact of varying PS number and position, ribose modifications, and base compositions in PS-modified pentamer ONs was demonstrated by AEX analysis. Retention behavior was thoroughly characterized using the Boardman and Patrick model. Diastereomers displayed consistent conformations with a similar number of charges involved in adsorption-desorption, though each could be distinguished by unique surface-charged areas. Parameters, including pH, column temperature, counter- and displacing ions, and particle size, were systematically evaluated to optimize diastereomer separations. The optimized method programming a multistep negative gradient led to a baseline separation of 8 diastereomers from a 21-mer ON with 3 PS modifications. Diastereomer profiling of a N-acetylgalactosamine-conjugated duplex ON and palmitoyl-amide-modified small interfering RNA was performed via multiple heart-cut AEX-IP-RPLC-MS 2D analysis. Unlike non-conjugated ONs, the presence of non-ionic conjugates leads to suppression into only two diastereomer peaks during the ¹D AEX chromatograms. Each small-interfering RNA diastereomer fraction was denatured during the ²D IP-RPLC analysis leading to the separation of the antisense and sense strands, allowing qualitative impurity profiling for each strand in subsequent MS coupling.

硫代磷酸酯（PS）修饰广泛应用于基于rna的治疗性寡核苷酸（ON），形成非对映体，增强ON的稳定性、生物利用度和细胞摄取。本研究提出了一种利用阴离子交换色谱（AEX）分析PS-ONs的策略，包括双链和各自的单义和反义链成分。通过AEX分析证明了不同PS数和位置、核糖修饰和碱基组成对PS修饰的五聚体ONs的影响。使用Boardman和Patrick模型对留存行为进行了彻底的表征。非对映体在吸附-解吸过程中具有相似数量的电荷，但它们的构象是一致的，每一种都可以通过独特的表面带电区域来区分。系统地评估了包括pH、柱温、反离子和置换离子以及粒径在内的参数，以优化非对映体的分离。优化后的方法规划了一个多步负梯度，通过3个PS修饰，从21聚合体的ON中分离出8个非对映体。通过多重心脏切割aex - ip - hplc - ms 2D分析，对n -乙酰半乳糖胺偶联双ON和棕榈酰酰胺修饰的小干扰RNA进行非对映体分析。与非共轭的离子不同，非离子共轭物的存在导致在1D AEX色谱中只有两个非对映体峰被抑制。在二维IP-RPLC分析过程中，每个小干扰RNA非对映体部分被变性，导致反义链和义链分离，允许在随后的MS偶联中对每条链进行定性杂质分析。

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引用次数: 0

Computer-aided fabrication of molecularly imprinted COFs for enantioselective extraction of dihydroquercetin from vine tea 计算机辅助制备分子印迹COFs对映选择性提取藤茶中二氢槲皮素。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-12-18 DOI: 10.1016/j.chroma.2025.466637

Yanlong Chen , Xingyuan Zhang , Juanqiong Ma , Na Yang , Jincheng Su , Zhiyong Xie , Fenglian Chen , Xiao Lin , Jing Gong , Qiongfeng Liao

Efficient separation and enrichment of bioactive flavonoid enantiomers from complex natural matrices remain a major challenge in analytical and life sciences. However, the enantioselectivity of adsorbents for flavonoid extraction remains limited because they lack complementary recognition sites. Herein, molecularly imprinted covalent organic frameworks (MI-COFs) were constructed based on a computer-aided design, which formed well-defined imprinting cavities serving as high-affinity recognition sites. These cavities impart precise and selective recognition toward flavonoid enantiomers, enabling efficient extraction of (2R,3R)-dihydroquercetin (DMY) from vine tea. The MI-COFs exhibited a high adsorption capacity (105 mg/g), excellent selectivity (imprinting factor, 2.7), and rapid adsorption kinetics. The MI-COFs were successfully applied as adsorbents for the targeted extraction of DMY from real vine tea samples, achieving high recoveries (86.8–89.2 %) and an enantiomeric excess of 98 %, with excellent reproducibility. This work demonstrates that rational chiral functionalization of MI-COFs enables precise and selective recognition of target enantiomers. Moreover, it provides a robust and versatile platform for the enantioselective separation and purification of chiral natural products, with broad applicability in food and pharmaceutical analysis.

从复杂的天然基质中高效分离和富集生物活性类黄酮对映体仍然是分析和生命科学的主要挑战。然而，由于缺乏互补的识别位点，吸附剂对黄酮类化合物提取的对映选择性仍然有限。本文基于计算机辅助设计构建了分子印迹共价有机框架（MI-COFs），形成了明确的印迹空腔，作为高亲和力的识别位点。这些空腔对黄酮类对映体具有精确和选择性的识别，能够有效地从藤茶中提取(2R,3R)-二氢槲皮素（DMY）。MI-COFs具有较高的吸附量（105 mg/g）、优良的选择性（印迹因子2.7）和快速的吸附动力学。实验结果表明，该吸附材料可用于葡萄茶样品中DMY的定向提取，回收率高达868 ~ 89.2%，对映体残留量高达98%，重现性好。这项工作表明，MI-COFs的合理手性功能化能够精确和选择性地识别目标对映体。此外，它为手性天然产物的对映选择分离和纯化提供了一个强大而通用的平台，在食品和药物分析中具有广泛的适用性。

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引用次数: 0

Biophysical characterisation of mRNA structure and its impact on integrity analysis by liquid chromatography and capillary gel electrophoresis methods mRNA结构的生物物理特征及其对液相色谱和毛细管凝胶电泳方法完整性分析的影响

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-12-17 DOI: 10.1016/j.chroma.2025.466625

Mayada Elgohary , Alexandra L.J. Webb , Joseph C. Ward , Andal Murthy , Jack Hutchinson , James Button , George Thom , Philip Newton , Emmelie Hammarvid , Anna D. Baran , Juhi Patel , Hannah N. Turney , Mark J. Dickman , Sara Trabulo , Eivor Örnskov

Messenger RNA (mRNA) integrity is a critical quality attribute (CQA) commonly assessed using liquid chromatography (LC) and capillary gel electrophoresis (CGE). The LC and CGE methods used for integrity tests are also used for stability studies for establishing product shelf-life for mRNA-based therapeutics. Advances in sequence and structure engineering have demonstrated significant improvements in mRNA translatability and stability. However, the higher order structure (HOS) of mRNA remains poorly understood and it is difficult to correlate experimentally measured structures with their bioinformatically predicted conformations. Previous studies have shown that mRNA HOS can cause artefactual bands or peaks in CGE and LC analyses, leading to anomalous integrity readouts. In this study, we employed a range of biophysical methods to characterise mRNA HOS, aiming to clarify the origins of the additional peaks observed in CGE and LC analyses and to better comprehend the influences of predicted minimum free energy (MFE) and structural features on mRNA integrity, translatability, and stability. Our findings provide new method-related considerations for measuring mRNA integrity as well as insights into the effects of mRNA structure on stability under long term storage and forced degradation conditions.

信使RNA （mRNA）完整性是一项重要的质量属性（CQA），通常使用液相色谱（LC）和毛细管凝胶电泳（CGE）来评估。用于完整性测试的LC和CGE方法也用于稳定性研究，以确定基于mrna的治疗方法的产品保质期。随着序列和结构工程的发展，mRNA的可译性和稳定性得到了显著改善。然而，mRNA的高阶结构（HOS）仍然知之甚少，并且很难将实验测量的结构与其生物信息学预测的构象联系起来。先前的研究表明，mRNA HOS可以在CGE和LC分析中引起人为的波段或峰，导致异常的完整性读数。在这项研究中，我们采用了一系列生物物理方法来表征mRNA HOS，旨在澄清在CGE和LC分析中观察到的额外峰的起源，并更好地理解预测的最小自由能（MFE）和结构特征对mRNA完整性、可译性和稳定性的影响。我们的研究结果为测量mRNA完整性提供了新的方法相关考虑因素，并深入了解了mRNA结构在长期储存和强制降解条件下对稳定性的影响。

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引用次数: 0

Dual flow-path HPLC method for time-optimised quantification of physicochemically different metabolite classes in human serum samples using a single mass spectrometer 双流路高效液相色谱法用于单质谱仪对人血清样品中理化不同代谢物类别进行时间优化定量。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-12-17 DOI: 10.1016/j.chroma.2025.466636

Christian Faist , Edda Tacke , Thorsten Eierhoff , Alexander Oberhuber , Heiko Hayen

Biomedical studies often involve the analysis of a wide range of analytes. The varying physicochemical properties of these analytes frequently hinder their detection by a single method, making it necessary to employ different analytical instruments or chromatographic approaches. This process often requires considerable time. In this study, we present a time-optimised LC-MS-based approach using only one mass spectrometer, but utilisation of two orthogonal chromatographic techniques, namely hydrophilic interaction liquid chromatography (HILIC) and reversed phase (RP)-HPLC in parallel. The established method allowed short-chain fatty acids (SCFA) and amines (such as trimethylamine N-oxide and carnitine) to be recovered from one human serum sample. SCFA were derivatized to their corresponding 3-nitrophenylhydrazones for improved RP-HPLC separation and electrospray ionisation efficiency, whereas amines could be separated and detected in their native forms on a zwitterionic HILIC phase. The combination of RP and HILIC methods through a six-port valve was achieved with a dual split sampler, enabling re-equilibration of one chromatographic column during the separation step of the other method. This approach ensured optimal capacity use of the MS and resulted in a 37 % analysis time reduction compared to the analysis with both individual methods. Application to human serum samples confirmed the robustness and reproducibility of the method, with quantification results showing relative standard deviations ≤ 5.8 % for all analytes as well as stable retention times and chromatographic resolutions for both methods. By allowing the combination of any chromatographic columns and methods with only one detector, this setup is well suited for quantification of extensive sample batches applying customised chromatographic conditions, while ensuring the optimal separation performance for both methods as well as maintaining efficient detector utilisation.

生物医学研究通常涉及对大量分析物的分析。这些分析物的不同物理化学性质经常阻碍单一方法的检测，因此有必要采用不同的分析仪器或色谱方法。这个过程通常需要相当长的时间。在这项研究中，我们提出了一种时间优化的基于lc - ms的方法，仅使用一台质谱仪，但同时利用两种正交色谱技术，即亲水相互作用液相色谱（HILIC）和反相(RP)-HPLC。建立的方法允许从一个人血清样本中回收短链脂肪酸（SCFA）和胺（如三甲胺n -氧化物和肉碱）。SCFA被衍生为相应的3-硝基苯基腙，以提高RP-HPLC分离和电喷雾电离效率，而胺则可以在阴离子HILIC相上以其天然形式分离和检测。通过双分裂进样器，通过六端口阀实现RP和HILIC方法的结合，从而在另一种方法的分离步骤中实现一层色谱柱的再平衡。这种方法确保了质谱的最佳容量使用，与使用两种单独方法的分析相比，分析时间减少了37%。对人血清样品的应用证实了该方法的稳健性和重复性，定量结果显示所有分析物的相对标准偏差≤5.8%，两种方法的保留时间和色谱分辨率都稳定。通过允许任何色谱柱和方法的组合，只有一个检测器，这种设置非常适合于定量广泛的样品批次应用定制的色谱条件，同时确保两种方法的最佳分离性能，以及保持有效的检测器利用率。

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引用次数: 0

Dual-targeting immunoadsorbent employing a bispecific nanobody for the simultaneous removal of IL-6 and TNF-α from serum 双靶向免疫吸附剂采用双特异性纳米体同时去除血清中的IL-6和TNF-α。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-12-17 DOI: 10.1016/j.chroma.2025.466635

Xiangxuan Feng, Yaohui Wang, Yifan Wang, Jun Ren

The dysregulated overproduction of pro-inflammatory cytokines like interleukin-6 (IL-6) and tumor necrosis factor-alpha (TNF-α) is a hallmark of severe inflammatory diseases. Extracorporeal blood purification offers a promising therapeutic strategy, but current adsorbents often lack the specificity required for precise intervention. This study reports the development of a bispecific nanobody (bsNb)-based immunoadsorbent for the simultaneous and specific removal of IL-6 and TNF-α. The functional bsNb, produced in a prokaryotic system via tandem fusion, was covalently immobilized on Sepharose CL-6B matrix to prepare the affinity adsorbent. Comprehensive characterization confirmed its high saturation adsorption capacity (6.9 mg/mL for IL-6 and 2.2 mg/mL for TNF-α) and rapid binding kinetics. In a simulated hemoperfusion system using human serum, the adsorbent achieved removal efficiencies exceeding 85% for both cytokines across a range of pathophysiological concentrations. Crucially, the bsNb adsorbent effectively captured both targets simultaneously from a complex serum matrix. This work highlights the significant potential of bispecific nanobodies as robust and selective ligands for preparing targeted immunoadsorbents. The developed platform represents a superior alternative to non-specific adsorbents, paving the way for more precise and effective extracorporeal therapies against cytokine-driven inflammatory disorders.

促炎细胞因子如白细胞介素-6 （IL-6）和肿瘤坏死因子-α (TNF-α)的过度产生失调是严重炎症性疾病的标志。体外血液净化提供了一种很有前途的治疗策略，但目前的吸附剂往往缺乏精确干预所需的特异性。本研究报道了一种基于双特异性纳米体（bsNb）的免疫吸附剂的开发，用于同时和特异性去除IL-6和TNF-α。通过串联融合在原核系统中制备功能性bsNb，并将其共价固定在Sepharose CL-6B基质上制备亲和吸附剂。综合表征证实其具有较高的饱和吸附能力（IL-6为6.9 mg/mL， TNF-α为2.2 mg/mL）和快速的结合动力学。在使用人血清的模拟血液灌流系统中，吸附剂在病理生理浓度范围内对两种细胞因子的去除效率均超过85%。至关重要的是，bsNb吸附剂有效地从复杂的血清基质中同时捕获两个目标。这项工作强调了双特异性纳米体作为制备靶向免疫吸附剂的强大和选择性配体的巨大潜力。开发的平台代表了非特异性吸附剂的优越替代品，为更精确和有效的体外治疗细胞因子驱动的炎症性疾病铺平了道路。

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引用次数: 0

Ultrasensitive detection of neurotransmitter dopamine in human urine via fluorescent azamonardine formed with resorcinol 间苯二酚形成的荧光氮杂定超灵敏检测人尿中的神经递质多巴胺

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-12-16 DOI: 10.1016/j.chroma.2025.466633

Marianna Ntorkou , Paraskevas D. Tzanavaras , Constantinos K. Zacharis

This work presents a pre-column derivatization HPLC–spectrofluorimetric platform for the ultratrace quantification of endogenous dopamine (DA) in human urine. Under alkaline conditions, DA rapidly condenses with resorcinol to form a highly fluorescent azamonardine derivative (λ_ex/λ_em = 420/460 nm), whose emission properties provide excellent analytical sensitivity in complex biochemical matrices. The derivatization proceeds quickly and yields a product with fluorescence stability for up to 6 hours. Key derivatization parameters were optimized using a face-centered central composite design. Selectivity studies confirmed the method’s discriminative capability against major metabolic interferents (e.g., homovanillic acid), enabling accurate quantitation at low-ppb concentrations. Method validation was performed using accuracy profiles in accordance with FDA bioanalytical guidelines. The method exhibited linearity over 5–100 ng/mL with a limit of detection of 0.3 ng/mL. The method precision was less 3.5% in all cases. Environmental and operational performance were simultaneously assessed using the unified multicolor MA tool, demonstrating the method’s strong sustainability profile and practical feasibility. Application to authentic human urine samples further confirmed the system’s translational potential as a robust, high-performance analytical approach for clinical diagnostics, neurochemical studies, and broader bioanalytical applications.

本研究提出了一种柱前衍生化高效液相色谱-荧光光谱法超痕量定量人尿中内源性多巴胺（DA）的方法。在碱性条件下，DA与间苯二酚快速缩合形成高荧光的氮杂胺衍生物（λex/λem = 420/460 nm），其发射特性在复杂的生化基质中具有优异的分析灵敏度。衍生化过程进行得很快，产生的产物具有长达6小时的荧光稳定性。采用面心中心复合设计对关键衍生化参数进行优化。选择性研究证实了该方法对主要代谢干扰物（如同香草酸）的鉴别能力，能够在低ppb浓度下进行准确定量。根据FDA生物分析指南使用准确度谱进行方法验证。该方法在5 ~ 100 ng/mL范围内呈线性，检出限为0.3 ng/mL。方法精密度均小于3.5%。使用统一的多色MA工具同时评估环境和运营绩效，证明该方法具有强大的可持续性和实际可行性。对真实人类尿液样本的应用进一步证实了该系统作为临床诊断、神经化学研究和更广泛的生物分析应用的强大、高性能分析方法的转化潜力。

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引用次数: 0

Characterization of biomimetic chromatography columns based on plasma proteins through the Abraham solvation parameter model 利用亚伯拉罕溶剂化参数模型表征血浆蛋白的仿生色谱柱

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-12-16 DOI: 10.1016/j.chroma.2025.466631

A.L. Valdez-Micheo , M. Rosés , S. Amézqueta , E. Fuguet

Biomimetic chromatography is a valuable tool for studying drug interactions by mimicking biological environments. In this work, two liquid chromatography systems with stationary phases based on plasma proteins, human serum albumin (HSA) and α₁-acid glycoprotein (AGP), will be evaluated regarding the interactions that these stationary phases establish with neutral and ionized compounds.

The Abraham solvation parameter model has been used to characterize the chromatographic systems. The models obtained demonstrate that both columns present almost identical selectivity for neutral compounds, with very similar retention mechanisms. The volume of the compounds increases the retention, whereas a high hydrogen bond basicity reduces it. Contrarily, the columns show different selectivity for ionic compounds, especially for anions, which are specifically retained in the HSA column, whereas no or low retention is observed in the AGP column.

When the obtained models are compared to the models corresponding to other biomimetic chromatography systems, it has been observed that, despite the nature of the stationary phase, all them provide similar selectivity for neutral compounds. In concrete, the two evaluated systems present great similarity to other systems based on liquid chromatography or electrokinetic chromatography that use phosphatidylcholine as stationary phase.

仿生色谱是通过模拟生物环境来研究药物相互作用的一种有价值的工具。在这项工作中，将评估基于血浆蛋白，人血清白蛋白（HSA）和α 1 -酸糖蛋白（AGP）的两种固定相的液相色谱系统，以确定这些固定相与中性和电离化合物的相互作用。用亚伯拉罕溶剂化参数模型对色谱系统进行了表征。得到的模型表明，两种色谱柱对中性化合物的选择性几乎相同，保留机制非常相似。化合物的体积增加了保留，而氢键的高碱度则降低了保留。相反，这些柱对离子化合物表现出不同的选择性，特别是阴离子，它们在HSA柱中被特异性保留，而在AGP柱中没有或很少被保留。当得到的模型与其他仿生色谱系统对应的模型进行比较时，已经观察到，尽管固定相的性质，但它们都对中性化合物提供相似的选择性。具体而言，这两种评价体系与其他以磷脂酰胆碱为固定相的液相色谱或电动色谱体系有很大的相似之处。

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引用次数: 0

Screening of active ingredients from traditional Chinese medicine using two-dimensional liquid chromatography-mass spectrometry: A case study of screening neuraminidase inhibitors from Schizonepetae spica 二维液相色谱-质谱联用技术筛选中药有效成分——以荆芥中神经氨酸酶抑制剂筛选为例

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-12-16 DOI: 10.1016/j.chroma.2025.466632

Hongping Wang , Zhaozhou Lin , Quantao Ma

The traditional methods of screening active ingredients from traditional Chinese medicine (TCM) are primarily based on chemical separation followed by activity evaluation, which involve long experimental cycles and large workloads. However, identifying active ingredients in TCM based on the targets related to a disease results in significantly improved screening efficiency. In this study, we developed a method for screening active components using two-dimensional liquid chromatography coupled with mass spectrometry (2D LC-MS). Briefly, the TCM extract was co-incubated with the target to form target–ligand complexes. Then, the incubation solution was loaded onto a 1D size-exclusion chromatography column, where the target–ligand complexes were separated from the unbound free compounds. Subsequently, a 2D reversed-phase chromatography column was used to dissociate the target–ligand complexes. Chromatographic separation was further optimized to ensure separation of the released ligands and inactive target. Finally, the dissociated ligands were analyzed using high-resolution mass spectrometry for structural identification. As an example, we screened the neuraminidase inhibitors from Schizonepetae spica using the method developed in this study and successfully identified a total of 40 ligands. The proposed 2D LC-MS method can be used for screening other active ingredients in TCM, and the screening model for neuraminidase inhibitors established in this study can be used for screening neuraminidase inhibitors from other TCM.

传统的中药有效成分筛选方法主要是先化学分离后活性评价，实验周期长，工作量大。而基于疾病相关靶点识别中药有效成分，可显著提高筛选效率。在本研究中，我们建立了一种利用二维液相色谱-质谱联用（2D LC-MS）筛选活性成分的方法。简单地说，中药提取物与靶标共孵育形成靶配体复合物。然后，将培养液加载到一维尺寸排除色谱柱上，将目标配体配合物与未结合的自由化合物分离。随后，使用二维反相色谱柱解离目标配体复合物。进一步优化色谱分离，确保释放配体与无活性靶分离。最后，利用高分辨率质谱分析解离配体进行结构鉴定。以Schizonepetae spica神经氨酸酶抑制剂为例，采用本研究开发的方法对其进行了筛选，共鉴定出40个配体。所建立的二维LC-MS方法可用于筛选中药中其他有效成分，本研究建立的神经氨酸酶抑制剂筛选模型可用于筛选其他中药中的神经氨酸酶抑制剂。

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引用次数: 0

Why is the “cutting heads and tails” process used in the production of strong-flavor Baijiu? 为什么在酿造烈性白酒时要采用“削头削尾”的工艺？

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-12-16 DOI: 10.1016/j.chroma.2025.466634

Yuhao Xiang , Hongguang Shang , Shuangquan Xiang , Xianping Qiu , Jianshen Yu , Xianlin Ni , Tongwei Guan

"Cutting the head and tail", a critical process in strong-flavor Baijiu production, was investigated in this study using GC-IMS, GC–MS, and sensory analysis. The results revealed that head fraction contained the highest volatile organic compounds (VOCs) content, contributing to rich aromas. However, its high alcohol content introduced unpleasant spiciness and bitterness, while fusel oils and fatty acid ethyl esters impaired flavor and caused turbidity. Body fraction exhibited a balanced flavor with a pronounced grain aroma, making it ideal as a base liquor. The tail fraction had the lowest VOCs content and high organic acid levels, which made it unsuitable for direct use. The study also found variation in the alcohol content of tail fraction samples, suggesting this process may lead to waste. Mixing head and tail fractions improved flavor and reduced waste. This study provided an approach for resource utilization, offered scientific support for optimizing the "cutting head and tail" process.

采用气相色谱- ims、气相色谱-质谱分析、感官分析等方法，对烈性白酒生产中的关键工序“去头去尾”进行了研究。结果表明，头部馏分挥发性有机化合物（VOCs）含量最高，香气丰富。然而，其高酒精含量带来了令人不快的辛辣和苦味，而杂醇油和脂肪酸乙酯则损害了风味并引起浑浊。酒体呈现出平衡的风味和明显的谷物香气，使其成为理想的底酒。尾馏分挥发性有机化合物（VOCs）含量最低，有机酸含量较高，不宜直接利用。该研究还发现了尾部馏分样品中酒精含量的变化，表明这一过程可能导致浪费。混合头和尾馏分改善了风味，减少了浪费。本研究为资源利用提供了途径，为优化“头尾切割”工艺提供了科学依据。

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