Journal of chromatography open最新文献_第4页

Comparative study of pesticide analysis in river water by gas chromatography/mass spectrometry screening and standard methods 气相色谱/质谱筛选法与标准法分析河水中农药的比较研究

IF 3.2

Journal of chromatography open

Pub Date : 2025-11-01 DOI: 10.1016/j.jcoa.2025.100285

Norihiro Kobayashi , Yuko Tsuchiya , Sumomo Nakamura , Kenta Nohara , Takako Yamazaki , Tomoko Oda , Teruaki Kinoshita

This study entailed a comparative analysis of the standard method (notification method) and the screening method based on gas chromatography/mass spectrometry (GC/MS) for detecting 168 pesticides. To clarify the qualitative and quantitative accuracy of the GC/MS screening method, the occurrence of pesticides in river water samples was determined using both methods. The lowest concentration in the calibration curves for 155 pesticides was 0.01 mg/L, corresponding to a limit of quantification (LOQ) of 0.01 μg/L in river water after accounting for the 1000-fold concentration factor from sample pretreatment. Except for two cases wherein the chromatogram showed interference peaks, both methods yielded consistent identification results. The quantitative values obtained by the screening method were 0.52–1.45 times (quantitative error ranging from −48% to +45%) those obtained by the notification method. The quantitative error associated with the screening method decreased significantly with increasing quantitative values. Calibration curves for each pesticide were prepared five times throughout the study period. Upon comparing with the initial calibration curve, the changes in these calibration curve slopes generally vary between −50% and +100% for each pesticide. Quantitative accuracy could be ensured by comprehensively maintaining the instrument conditions, even during prolonged use. This indicates that the quantitative errors of the screening method are controllable, although they are not equivalent to those of the notification method. Therefore, the GC/MS screening method can be effectively utilized for water quality management. To avoid underestimation of pesticide concentrations, the GC/MS screening method values may be multiplied by a safety factor of 2.

对168种农药的标准检测方法（通报法）和气相色谱/质谱（GC/MS）筛选方法进行了对比分析。为了明确GC/MS筛选方法的定性和定量准确性，采用两种方法对河流水样中农药的出现情况进行了测定。155种农药的校准曲线最低浓度为0.01 mg/L，考虑样品前处理的1000倍浓度因子，河流水体的定量限为0.01 μg/L。除两例色谱出现干扰峰外，两种方法鉴定结果一致。筛选法得到的定量值是通报法的0.52 ~ 1.45倍（定量误差范围为- 48% ~ +45%）。随着定量值的增加，与筛选方法相关的定量误差显著降低。在整个研究期间，每种农药的校准曲线制备了5次。与初始校准曲线比较，每种农药的校准曲线斜率的变化通常在- 50%到+100%之间。即使在长时间使用期间，也可以通过全面维护仪器条件来确保定量准确性。这表明，筛选方法的定量误差是可控的，尽管它们不等同于通知方法的定量误差。因此，GC/MS筛选方法可以有效地用于水质管理。为避免农药浓度的低估，GC/MS筛选方法的值可乘以2的安全系数。

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引用次数: 0

Comment on ‘From multimodal liquid chromatography to supercritical fluid chromatography: Mapping chiral separation of the major organic ultraviolet filters’ (JCO 8 (2025) 100251. https://doi.org/10.1016/j.jcoa.2025.100251) - peak assignment for cis- and trans-homosalate 对“从多模态液相色谱到超临界流体色谱：绘制主要有机紫外过滤器的手性分离图谱”（JCO 8(2025) 100251）的评论。https://doi.org/10.1016/j.jcoa.2025.100251) -顺式和反式homosalate的峰分配

IF 3.2

Journal of chromatography open

Pub Date : 2025-11-01 DOI: 10.1016/j.jcoa.2025.100277

Daniel Bury, Katharina E. Ebert, Holger M. Koch

引用次数: 0

Microplastics in salt: A critical review of contamination, analytical methodologies, and health implications 盐中的微塑料：对污染、分析方法和健康影响的批判性审查

IF 3.2

Journal of chromatography open

Pub Date : 2025-11-01 DOI: 10.1016/j.jcoa.2025.100276

Cristina Grazia De Nido , Diego Centonze , Carmen Palermo , Javier González-Sálamo , Javier Hernández-Borges

Microplastic pollution has emerged as a growing environmental concern due to the rapid and widespread distribution of these particles, their entry into the food chain, and their potential implications for human health. Among food products, salt has gained attention as a relevant indicator of microplastic contamination, given its widespread consumption and direct environmental exposure during production. This review provides a comprehensive overview of current knowledge on the occurrence of microplastics in commercial salt, with a particular focus on sample pretreatment protocols, analytical techniques employed, and the diverse morphotypes in which microplastics are found, factors that are critical for accurate identification and quantification. Although research in this field is still evolving, existing studies offer valuable insights into the extent of contamination and serve as useful tools for environmental monitoring. Using salt as a model matrix, this review also reflects on the broader dietary and ecological implications of microplastic pollution, highlighting the need for improved methodologies and sustainable strategies to mitigate this emerging threat.

微塑料污染已成为日益严重的环境问题，原因是这些颗粒的迅速和广泛分布、进入食物链以及对人类健康的潜在影响。在食品中，盐作为微塑料污染的相关指标引起了人们的关注，因为盐的广泛消费和生产过程中的直接环境暴露。这篇综述提供了目前关于商品盐中微塑料的知识的全面概述，特别关注样品预处理方案，所采用的分析技术，以及发现微塑料的各种形态，这些因素对准确鉴定和定量至关重要。虽然这一领域的研究仍在不断发展，但现有的研究对污染程度提供了有价值的见解，并可作为环境监测的有用工具。本综述以盐为模型矩阵，还反映了微塑料污染对饮食和生态的更广泛影响，强调需要改进方法和可持续战略来减轻这一新出现的威胁。

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引用次数: 0

Vacuum-assisted headspace solid-phase microextraction for volatile profiling of avocado puree: Application to post-harvest ripening 真空辅助顶空固相微萃取牛油果泥挥发性分析：在收获后成熟中的应用

IF 3.2

Journal of chromatography open

Pub Date : 2025-10-18 DOI: 10.1016/j.jcoa.2025.100274

Angeliki Pateraki , Breno Jorge Pollo , Fabio Augusto , Elefteria Psillakis

Vacuum-assisted headspace solid-phase microextraction (Vac-HS-SPME) was developed and applied for the first time to monitor free volatile emissions during post-harvest ripening of Hass and Fuerte avocados. The parameters of extraction time and temperature were optimized using 24 analytes identified in unripe Hass puree. Through this optimization, the advantages of vacuum conditions were confirmed by comparing Vac-HS-SPME with conventional headspace solid-phase microextraction (HS-SPME). Vacuum conditions improved the extraction of sesquiterpenes and enabled the unique detection of octanal and (Z)-2-octen-1-ol under milder conditions. Under optimal conditions (30 min at 40 °C), Vac-HS-SPME successfully revealed cultivar-specific and ripening-related changes in volatile profiles. At the unripe stage, Fuerte showed higher relative abundances of sesquiterpenes compared to Hass, while (E)-2-heptenal, hexyl acetate and β-bisabolene were detected exclusively in unripe Hass. Ripening was associated with a marked reduction in sesquiterpenes, alcohols, and higher molecular weight aldehydes. The decline of sesquiterpenes is likely driven by the increasing oil content of the mesocarp during ripening, as lipophilic compounds preferentially remain in the lipid matrix rather than partitioning into the headspace. Aldehydes such as hexanal and (E)-2-hexenal became dominant at the ripe stage, and both cultivars displayed similar profiles. Overall, this study demonstrates that Vac-HS-SPME is a powerful and robust method for monitoring volatile changes in avocado ripening, with potential applications in harvest, storage, and quality management.

真空辅助顶空固相微萃取技术（Vac-HS-SPME）首次被用于监测Hass和Fuerte鳄梨收获后成熟过程中的游离挥发物排放。以未熟哈斯果浆中鉴定的24种分析物为研究对象，对提取时间和温度参数进行了优化。通过优化，将真空-HS-SPME与传统顶空固相微萃取（HS-SPME）进行对比，证实了真空条件的优势。真空条件改善了倍半萜的提取，在较温和的条件下可以独特地检测辛烷和(Z)-2-辛烷-1-醇。在最佳条件下（40°C 30 min）， Vac-HS-SPME成功地揭示了挥发物谱的品种特异性和成熟相关变化。在未成熟阶段，富尔特的倍半萜相对丰度高于哈斯，而(E)-2-庚烯、乙酸己酯和β-双abolene仅在未成熟的哈斯中检测到。成熟与倍半萜、醇和高分子量醛的显著减少有关。倍半萜的下降可能是由于成熟过程中中果皮含油量的增加，因为亲脂化合物优先留在脂质基质中，而不是分配到顶空。醛类如己醛和(E)-2-己烯醛在成熟阶段成为优势，两个品种表现出相似的特征。总之，本研究表明，Vac-HS-SPME是一种监测鳄梨成熟过程中挥发物变化的强大而稳健的方法，在收获、储存和质量管理方面具有潜在的应用前景。

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引用次数: 0

Comprehensive two-dimensional gas chromatography analysis of volatiles on e-liquids and aerosol compounds produced during the heating process 综合二维气相色谱分析在加热过程中产生的电子液体和气溶胶化合物的挥发物

IF 3.2

Journal of chromatography open

Pub Date : 2025-10-18 DOI: 10.1016/j.jcoa.2025.100273

Glaucimar Alex Passos Resende , Sofia Madruga Marcondes Ferraz , Lucas Paines Bressan , Isadora de Oliveira , Thiago Nazario , Lucas Pessôa de Araujo , Leandro Wang Hantao

Electronic cigarettes (e-cigarettes) have gained global popularity, raising public health concerns due to the limited regulation and chemical complexity of e-liquids and their aerosols. This study presents the compositional analysis of volatile and semi-volatile organic compounds in 34 commercial e-liquid samples and their corresponding aerosols using headspace solid-phase microextraction (HS-SPME) and comprehensive two-dimensional gas chromatography coupled with mass spectrometry (GC×GC–MS). The HS-SPME method was optimized using a central composite design (CCD), which established the ideal extraction conditions. One hundred twenty-six compounds were identified in the e-liquids. Chemometric analysis revealed distinct flavor profiles. The occurrence of concerning aldehydes, including benzaldehyde and (E)-cinnamaldehyde, was confirmed in the samples. The study of compounds generated when the e-liquids were heated at various temperatures (190–270 °C) and durations (3–30 min) showed the formation of harmful and potentially harmful constituents (HPHCs), including furfural, glycidol, and diacetyl, under specific conditions. Principal component analysis (PCA) of the aerosol data revealed the impact of heating time on the volatilization of both major e-liquid components and lower-concentration flavoring compounds. Overall, this study demonstrated the potential of GC×GC–MS for characterizing e-liquids and enhanced our understanding of toxic compound formation during the heating of e-liquids.

电子烟（电子烟）在全球范围内受到欢迎，由于电子烟液体及其气溶胶的监管有限和化学复杂性，引起了公众对健康的担忧。本研究采用顶空固相微萃取（HS-SPME）和综合二维气相色谱-质谱联用技术（GC×GC-MS）对34种商用电子烟样品及其气溶胶中的挥发性和半挥发性有机化合物进行了成分分析。采用中心复合设计（CCD）对HS-SPME法进行了优化，建立了理想的提取条件。在电子液体中鉴定出126种化合物。化学计量分析显示出不同的风味特征。在样品中发现了苯甲醛和(E)-肉桂醛。对电子液体在不同温度（190-270℃）和时间（3-30分钟）下加热时产生的化合物的研究表明，在特定条件下，形成有害和潜在有害成分（HPHCs），包括糠醛，甘油和双乙酰。气溶胶数据的主成分分析（PCA）揭示了加热时间对电子烟主要成分和低浓度调味化合物挥发的影响。总的来说，这项研究证明了GC×GC-MS表征电子液体的潜力，并增强了我们对电子液体加热过程中有毒化合物形成的理解。

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引用次数: 0

Rapid High Performance Liquid Chromatography methodologies for analytical characterization of biotherapeutic products 生物治疗产品分析表征的快速高效液相色谱方法

IF 3.2

Journal of chromatography open

Pub Date : 2025-10-16 DOI: 10.1016/j.jcoa.2025.100272

Anurag S. Rathore, Debasmita Chakraborty, Deepika Sarin

The last two decades have witnessed an increasing interest in rapid analytical methods amongst the biopharmaceutical industry. This interest has, in turn, resulted in advancements in analytical hardware, data analytics, and practices. In this article, we review major developments that have occurred over the last 6 years (2019–2025) in rapid chromatographic analysis of proteins, including monoclonal antibodies (mAbs), antibody-drug conjugates (ADCs), and other therapeutic proteins. Conventional high-performance liquid chromatography (HPLC) is vital for characterizing critical quality attributes (CQAs), but has limitations like long run times, manual handling, and low throughput. Recent developments in rapid HPLC have given a new direction to biopharmaceutical analysis by reducing analysis times from hours to minutes, while maintaining resolution and sensitivity. Key aspects of improvements that have been addressed in this review include chromatography equipment, column innovations, and advanced methodologies that have contributed towards the implementation of rapid HPLC methods in the biopharmaceutical industry. Furthermore, integrating process analytical technology (PAT) with rapid HPLC has made it possible to monitor CQAs in real-time, either inline or at-line, which is crucial for manufacturers engaged in continuous processing. The review also discusses data analytics and software-driven method development, which have significantly lowered experimental efforts and strengthened method reliability. The article focuses mainly on rapid HPLC-based analysis and does not include the mass spectrometry (MS) oriented faster analytical methods.

在过去的二十年中，生物制药行业对快速分析方法的兴趣日益浓厚。这种兴趣反过来又导致了分析硬件、数据分析和实践的进步。在本文中，我们回顾了过去6年（2019-2025）在蛋白质快速色谱分析方面的主要进展，包括单克隆抗体（mab）、抗体-药物偶联物（adc）和其他治疗性蛋白质。传统的高效液相色谱（HPLC）对于表征关键质量属性（cqa）至关重要，但存在运行时间长、人工处理和吞吐量低等局限性。快速高效液相色谱的最新发展为生物制药分析提供了新的方向，将分析时间从几小时减少到几分钟，同时保持分辨率和灵敏度。在这篇综述中提到的主要改进方面包括色谱设备、色谱柱创新和先进的方法，这些都有助于在生物制药工业中实现快速高效液相色谱方法。此外，将过程分析技术（PAT）与快速高效液相色谱（HPLC）相结合，使得在线或在线实时监测cqa成为可能，这对从事连续加工的制造商至关重要。本文还讨论了数据分析和软件驱动的方法开发，它们大大降低了实验工作量，增强了方法的可靠性。本文主要侧重于基于高效液相色谱的快速分析，不包括面向质谱（MS）的快速分析方法。

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引用次数: 0

Full comprehensive ion-pair-mediated anion exchange chromatography × ion-pair reversed-phase liquid chromatography fingerprinting of digested messenger ribonucleic acid drug substances 全综合离子对介导阴离子交换色谱法×离子对反相液相色谱法酶解信使核糖核酸原药的指纹图谱

IF 3.2

Journal of chromatography open

Pub Date : 2025-10-15 DOI: 10.1016/j.jcoa.2025.100271

Niklas Carstensen , Ryan Karongo , Anne Mengel , Michael Lämmerhofer

The growing interest in messenger RNA (mRNA) based therapeutics has increased the need for analytical method development to meet the desired standards for quality control of these novel drugs. The identity of the mRNA drug substance is usually confirmed via indirect approaches such as Sanger sequencing or next generation sequencing (NGS), or more direct approaches such as LC-MS/MS after digestion with specific RNases. These conventional bottom-up MS methodologies, however, usually require several partial digests with various RNases to get sufficient sequence coverage. In the present study, a comprehensive two-dimensional liquid chromatography (LC × LC) platform is presented, utilizing ion-pair-mediated anion exchange chromatography in the first dimension and ion-pair reversed-phase liquid chromatography in the second dimension and evaluated using the convex hull model for orthogonality determination. This platform can be employed for the fingerprinting of RNase T1 digested mRNA, enabling the distinction between different mRNAs based on the fingerprint of a full digestion with a single RNase. It could also be used to confirm its identity or help with sequencing efforts, when combined with high-resolution MS.

对基于信使RNA （mRNA）的治疗方法的兴趣日益增长，增加了对分析方法开发的需求，以满足这些新药质量控制所需的标准。mRNA原料药的身份通常通过间接方法（如Sanger测序或下一代测序（NGS））或更直接的方法（如特定RNases消化后的LC-MS/MS）来确认。然而，这些传统的自下而上的质谱方法通常需要几种不同rna的部分文摘来获得足够的序列覆盖。在本研究中，提出了一个综合的二维液相色谱（LC × LC）平台，利用离子对介导的阴离子交换色谱（第一维）和离子对反相液相色谱（第二维），并使用凸壳模型评估正交性。该平台可用于RNase T1酶切mRNA的指纹图谱，实现基于单个RNase全酶切的指纹图谱来区分不同的mRNA。当与高分辨率质谱相结合时，它也可以用来确认其身份或帮助测序工作。

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引用次数: 0

Rapid O-glycan release from glycoproteins using a monolith-based glycosidase microreactor 利用单块基糖苷酶微反应器快速从糖蛋白中释放o -聚糖

IF 3.2

Journal of chromatography open

Pub Date : 2025-10-09 DOI: 10.1016/j.jcoa.2025.100269

Bin Yang , Myriam Taverna , Cédric Y. Montanier , Zhengjin Jiang , N. Thuy Tran

Fast, efficient and simple selective O-glycan release methods are urgently needed for accurately analyzing O-glycans of therapeutic proteins or glycosylation-based biomarkers. In this study, a polymeric monolith-based microreactor with immobilized O-glycosidase inside a capillary has been developed. The photopolymerization of a poly (glycidyl methacrylate-co-poly (ethylene glycol) diacrylate) monolith in a capillary with tens of nanoliters volume (50 μm I.D. × 1 cm) was optimized. It exhibited a relatively high permeability (2.29 × 10^–13 m²), and good mechanical and chemical stabilities. Two different immobilization chemistries to attach O-glycosidase and several digestion protocols were tested and compared. We showed that Shiff base and Epoxy chemistries for O-glycosidase immobilization led to similar digestion efficiencies regarding the quantity of released O-glycans. The performance of the immobilized enzyme reactor (IMER) was assessed on asialofetuin used as a substrate for the release of O-glycans. In-IMER digestion was able to release 56 % of O-glycans in <3 s, while the enzyme in-solution digestion required at least one hour to achieve the same release efficiency. The capillary format monolith proves the route to fulfil on-line coupling between O-glycan release and glycan separation analysis.

快速、高效、简单的选择性o -聚糖释放方法是准确分析治疗蛋白或糖基生物标志物o -聚糖的迫切需要。本研究开发了一种毛细管内固定化o -糖苷酶的聚合物单体微反应器。优化了聚（甲基丙烯酸缩水甘油酯-共聚（乙二醇）二丙烯酸酯）单体在体积为几十纳升（50 μm I.D. × 1 cm）的毛细管中光聚合的条件。它具有较高的渗透率（2.29 × 10-13 m2）和良好的机械和化学稳定性。两种不同的固定化学附着o -糖苷酶和几种消化方案进行了测试和比较。我们发现，对于o -糖苷酶的固定化，shift碱和环氧化学反应导致了类似的消化效率，就释放的o -糖苷的数量而言。以asialofetuin为底物，对固定化酶反应器（IMER）的性能进行了评价。in- imer酶切法能在3秒内释放56%的o -聚糖，而溶液酶切法至少需要1小时才能达到相同的释放效率。毛细管格式整体柱证明了实现o -聚糖释放与聚糖分离分析在线耦合的途径。

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引用次数: 0

Chromatographic techniques in volcanic surveillance: from gases to dissolved species 火山监测中的色谱技术：从气体到溶解物质

IF 3.2

Journal of chromatography open

Pub Date : 2025-10-09 DOI: 10.1016/j.jcoa.2025.100270

María Asensio-Ramos

Volcanic systems release chemical species in gases, aerosols, and hydrothermal or surface waters, providing critical insights into magmatic degassing, hydrothermal processes, and surface interactions that inform hazard assessment. Among the many chromatographic techniques available, volcanic surveillance has primarily relied on a few approaches. Gas chromatography (GC) and liquid chromatography (LC) are essential for analyzing these emissions, ranging from detecting permanent gases and volatile organic compounds (VOCs) in volcanic plumes to quantifying anions, cations, and organic compounds in dissolved phases such as hydrothermal waters and ash leachates. Advances in miniaturized GC instrumentation and hyphenated methods such as GC-mass spectrometry (MS) and LC-MS enhance the analysis of trace species, providing detailed insights into volcanic activity. Despite challenges posed by matrix complexity and the reactivity of some species, chromatography remains a key tool for investigating volcanic emissions and the processes driving them. This review highlights chromatographic methods applied to volcanic surveillance and the study of volcanic processes.

火山系统在气体、气溶胶、热液或地表水中释放化学物质，为岩浆脱气、热液过程和地表相互作用提供了重要的见解，为危害评估提供了信息。在许多可用的色谱技术中，火山监测主要依赖于几种方法。气相色谱（GC）和液相色谱（LC）对于分析这些排放物至关重要，从检测火山羽流中的永久性气体和挥发性有机化合物（VOCs）到定量阴离子、阳离子和溶解相中的有机化合物，如热液水和灰渗滤液。小型气相色谱仪器和联用方法的进步，如气相色谱-质谱（MS）和LC-MS，增强了对痕量物种的分析，为火山活动提供了详细的见解。尽管基质复杂性和某些物质的反应性带来了挑战，色谱法仍然是研究火山喷发及其驱动过程的关键工具。本文综述了色谱法在火山监测和火山过程研究中的应用。

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引用次数: 0

Application of alrestatin chloride as a derivatizing reagent for the determination of amino acids, catecholamines and biogenic amines in urine 氯阿司他汀衍生试剂在测定尿液中氨基酸、儿茶酚胺和生物胺中的应用

IF 3.2

Journal of chromatography open

Pub Date : 2025-10-07 DOI: 10.1016/j.jcoa.2025.100268

A. Temerdashev , A. Azaryan , Dzh. Konshina , V. Konshin , M. Steshin , E. Gashimova , S.N. Atapattu , Y.-Q. Feng , Q.-F. Zhu

The feasibility of using alrestatin chloride as a derivatization reagent was evaluated. Selected amino acids, catecholamines, and biogenic amines were tested. Limits of detection (LOD), limits of quantification (LOQ), and key analytical performance parameters were determined. Depending on the analyte, the detection limit varied from 0.1 to 5 ng/ml, and the error did not exceed 15 %, which allows the effective use of alrestatin chloride as a derivatizing reagent and significantly exceeds FMOCCl and dansyl chloride in sensitivity. An important advantage established for these derivatives is that they are stable over a long period of time. A proposed interpretation of the amino acid derivative is presented, and optimal MRM transitions for quantitative and qualitative analysis are established. It is shown that, although the proposed derivatization approach provides high sensitivity, prolonged heating is required to ensure a complete derivatization reaction, which can negatively impact analyte stability.

评价了氯阿司他汀作为衍生化试剂的可行性。对选定的氨基酸、儿茶酚胺和生物胺进行了测试。确定了样品的检出限（LOD）、定量限（LOQ）和关键分析性能参数。根据分析物的不同，检测限在0.1 ~ 5ng /ml之间变化，误差不超过15%，可以有效地使用氯阿司他汀作为衍生化试剂，并且灵敏度明显超过FMOCCl和丹酰氯。这些衍生品的一个重要优势是它们在很长一段时间内都是稳定的。提出了一种氨基酸衍生物的解释，并建立了定量和定性分析的最佳MRM转换。结果表明，尽管提出的衍生化方法提供了高灵敏度，但需要长时间加热以确保完整的衍生化反应，这可能会对分析物的稳定性产生负面影响。

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引用次数: 0