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A comprehensive review of advances in analytical chromatography for the characterization of therapeutic biomacromolecule and bioparticle. 综述了分析色谱法用于治疗性生物大分子和生物颗粒表征的研究进展。
IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Pub Date : 2026-03-03 DOI: 10.1016/j.chroma.2026.466864
Navratan Soni, Mukul Yadav, David Paul

The explosive growth of therapeutic biomacromolecules and bioparticles, such as monoclonal antibodies, nucleic acid therapeutics, viral vectors, lipid nanoparticles, and extracellular vesicles, has led to a critical need for advanced analytical & chromatographic techniques to resolve their structural, compositional, and physicochemical heterogeneity. Conventional analytical approaches are often inadequate for the characterization of important quality attributes, such as size and charge variants, post-translational modifications, conformational integrity, and particle-level heterogeneity, etc., in these complicated systems. This review discusses recent advances in some of the modern analytical chromatographic approaches for the separation and characterization of such complex biological systems, with high-end detection platforms such as mass spectrometry, multi-angle light scattering, and ion mobility spectrometry. Key developments in size-exclusion, ion-exchange, hydrophobic interaction, hydrophilic interaction, reverse-phase, affinity, hydrodynamic chromatography, and field-flow fractionation are critically discussed based on selected recent primary research studies. Comparative insights are provided to highlight the analytical competence, limitations, and applicability of each technique to different classes of biomolecules. Collectively, this review aims to be a decision-oriented guide for scientists and industrial practitioners seeking suitable analytical chromatographic strategies for characterizing emerging therapeutic biomacromolecules and bioparticles.

治疗性生物大分子和生物颗粒的爆炸性增长,如单克隆抗体、核酸疗法、病毒载体、脂质纳米颗粒和细胞外囊泡,导致了对先进的分析和色谱技术的迫切需求,以解决其结构、组成和物理化学的异质性。在这些复杂的系统中,传统的分析方法往往不足以表征重要的质量属性,如大小和电荷变化、翻译后修饰、构象完整性和粒子水平异质性等。本文综述了一些用于分离和表征复杂生物系统的现代分析色谱方法的最新进展,包括高端检测平台,如质谱法、多角度光散射法和离子迁移谱法。本文根据最近的主要研究,对尺寸排除、离子交换、疏水相互作用、亲水相互作用、反相、亲和、水动力色谱和场流分馏等方面的关键进展进行了批判性的讨论。提供了比较见解,以突出每种技术对不同类别生物分子的分析能力,局限性和适用性。总的来说,这篇综述的目的是为科学家和工业从业者寻找合适的分析色谱策略来表征新兴的治疗性生物大分子和生物颗粒提供决策导向的指南。
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引用次数: 0
Eco-friendly sugarcane bagasse-based biochar alginate beads as green sorbents for rapid and highly efficient benzoylurea insecticides extraction in tea samples 以甘蔗渣为基础的生物炭藻酸酯微球作为绿色吸附剂,快速高效地提取茶叶样品中的苯甲脲类杀虫剂。
IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Pub Date : 2026-02-22 Epub Date: 2026-01-10 DOI: 10.1016/j.chroma.2026.466701
Kittiya Sakhaem , Sujittra Aintharaprasert , Dararat Saenkam , Phatchara Rattanaphonsaen , Wannipha Khiaophong , Yanawath Santaladchaiyakit , Jitlada Vichapong
In this work, an environmentally method was proposed for the trace determination of benzoylureas by high performance liquid chromatography system after micro-solid phase extraction method. Sugarcane bagasse-based biochar alginate beads as were employed as sorbent material. The synthesized material was characterized. The univariate optimization approach was performed to determine optimum conditions for both preparation of sugarcane bead adsorbents and micro-solid phase extraction procedure. Under optimal conditions, the limit of detection was found to be in the range of 1.0 – 2.0 μg L–1 and the linearity was obtained between 3.0 and 400 μg L–1 with coefficient of determination greater than 0.99. The applicability of the investigated method was evaluated with recovery studies by spiking experiments in tea samples. The acceptable recovery results between 72.1 and 121.1 % by applying matrix matching calibration showed that the proposed analytical approach is feasible for the determination of benzoylurea insecticides in tea matrices.
本文建立了微固相萃取法后高效液相色谱法测定苯甲酰脲的环境分析方法。采用甘蔗渣基生物炭海藻酸盐微球作为吸附材料。对合成材料进行了表征。采用单因素优化方法确定甘蔗头吸附剂的制备工艺和微固相萃取工艺的最佳条件。在最佳条件下,该方法的检出限在1.0 ~ 2.0 μ L-1范围内,线性关系在3.0 ~ 400 μ L-1之间,测定系数大于0.99。通过在茶叶样品中进行加穗试验,对方法的适用性进行了评价。采用基质匹配校准,回收率在72.1 ~ 121.1%之间,表明该分析方法对茶基质中苯甲脲类杀虫剂的测定是可行的。
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引用次数: 0
Development of an arrow solid-phase microextraction GC–MS/MS method for the determination of 69 odorants in water 箭型固相微萃取-气相色谱-质谱联用/质谱联用方法测定水中69种气味剂。
IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Pub Date : 2026-02-22 Epub Date: 2026-01-10 DOI: 10.1016/j.chroma.2026.466703
FeiFei Dai , Ruoyu Zhang , Dandan Nie , Shuqing Ma , Yurong Qin
A quantitative method for determining 69 odorants in water was developed using arrow-type headspace solid-phase microextraction (SPME) coupled with gas chromatography-tandem mass spectrometry (GC–MS/MS). Key extraction parameters, including extraction and desorption temperatures and times, NaCl addition, fiber type, and rotation speed, were systematically optimized. Under the optimized conditions, target compounds were efficiently enriched, separated on a polar chromatographic column, detected in selected reaction monitoring (SRM) mode, and quantified using external calibration. The method demonstrated high sensitivity, with limits of detection (LODs) ranging from 0.015 to 75 ng/L, and 55 compounds exhibiting LODs below 10 ng/L. All analytes showed excellent linearity (R2 > 0.995) within their respective ranges. Precision was satisfactory, with relative standard deviations (RSDs) between 1.10 % and 17.85 %, including 59 compounds with RSDs <10 %. Average recoveries at three spiking levels ranged from 80 % to 120 %. This automated and environmentally friendly method offers high sensitivity and accuracy, meeting the analytical requirements for complex odorants in water.
建立了箭型顶空固相微萃取(SPME) -气相色谱-串联质谱(GC-MS/MS)联合测定水中69种气味剂的方法。对提取和解吸温度、次数、NaCl加入量、纤维类型、转速等关键提取参数进行了系统优化。在优化的条件下,目标化合物被高效富集,在极性色谱柱上分离,在选择的反应监测(SRM)模式下检测,并通过外部定标进行定量。该方法具有较高的灵敏度,检出限(lod)范围为0.015 ~ 75 ng/L, 55个化合物的lod低于10 ng/L。所有分析物在各自的范围内均具有良好的线性(R2 > 0.995)。精密度满意,相对标准偏差(rsd)在1.10% ~ 17.85%之间,有rsd的化合物59个
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引用次数: 0
Polyetheretherketone (PEEK)-based open tubular ion chromatography for perchlorate detection 聚醚醚酮(PEEK)基开管离子色谱法检测高氯酸盐
IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Pub Date : 2026-02-22 Epub Date: 2026-01-07 DOI: 10.1016/j.chroma.2026.466700
Jiafeng Pang , Zihan Zeng , Hui Zeng , Min Zhang , Weixiong Huang
Open tubular ion chromatography (OTIC) offers a lightweight, low-pressure and efficient platform for on-site ion analysis. Polyetheretherketone (PEEK) is an attractive column substrate because of its mechanical strength, chemical resistance and thermal stability, yet conventional sulfuric-acid sulfonation limits ion-exchange capacity and requires long preparation times. Here, a mixed methanesulfonic and sulfuric acid reagent followed by acetone rinsing was used to streamline the sulfonation process, producing a roughened inner surface with higher functional group density. The optimized 25 μm i.d. PEEK capillaries achieved a cation-exchange capacity of 2.5 ± 0.1 peq/mm2, roughly eight times higher than that from single-acid treatment. The latex-coated columns had an anion-exchange capacity of 20.0 ± 0.8 peq/mm2 and enabled baseline separation of perchlorate within 5 min using 6 mM sodium salicylate as the eluent. When integrated with a nonsuppressed OTIC system and electromembrane extraction, the method exhibited high reproducibility (RSD < 3%), a quantitation limit of 0.2 μM, and recoveries of 87.6–114.9% in environmental samples, confirming its reliability and sensitivity for perchlorate analysis.
开管离子色谱(OTIC)为现场离子分析提供了一种轻便、低压、高效的平台。聚醚醚酮(PEEK)因其机械强度、耐化学性和热稳定性而成为一种有吸引力的柱状底物,但传统的硫酸磺化限制了离子交换能力,并且需要较长的制备时间。在这里,使用混合的甲磺酸和硫酸试剂,然后使用丙酮漂洗,以简化磺化过程,产生粗糙的内表面,具有更高的官能团密度。优化后的25 μm i.d PEEK毛细血管的阳离子交换容量为2.5±0.1 peq/mm2,约为单酸处理的8倍。乳胶包覆柱的阴离子交换容量为20.0±0.8 peq/mm2,使用6 mM水杨酸钠作为洗脱液,可在5分钟内对高氯酸盐进行基线分离。结果表明,该方法具有较高的重现性(RSD为3%),定量限为0.2 μM,回收率为87.6-114.9%,具有较高的灵敏度和可靠性。
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引用次数: 0
Development of a green analytical method based on a Montmorillonite/Hydroxyapatite composite coupled with rotating disk sorptive extraction and GC–MS for monitoring steroid hormones in hospital wastewater 基于蒙脱土/羟基磷灰石复合材料-旋转圆盘吸附萃取-气相色谱-质谱联用技术监测医院废水中类固醇激素的绿色分析方法的建立
IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Pub Date : 2026-02-22 Epub Date: 2026-01-21 DOI: 10.1016/j.chroma.2026.466722
Maby Moll Martínez-Garzón , José Martin Posada-Lotero , Milton Hernando Rosero-Moreano , Elisabeth Restrepo-Parra , Francy Nelly Jiménez-García
Environmental concern regarding the presence of steroid hormones in hospital wastewater treatment plants underscores the need for effective monitoring and removal strategies. Even at trace levels, steroid estrogens exhibit strong biological activity and bioaccumulation potential, classifying them as endocrine-disrupting compounds. In this study, a Montmorillonite/Hydroxyapatite (MMT/HAp) composite was proposed as an environmentally friendly and low-cost alternative for the extraction of estrone (E1), 17β-estradiol (E2), 17α-ethinylestradiol (EE2), and estriol (E3). Sample preparation was carried out using a green analytical method based on rotating disk sorptive extraction. Considering the complexity of wastewater matrices, analytes were determined using gas chromatography coupled to mass spectrometry (GC–MS) in selective ion monitoring mode. A Doehlert experimental design was applied to optimize the extraction process, yielding the following optimal conditions: extraction time of 87 min, sample volume of 16 mL, and stirring speed of 1080 rpm. Hospital wastewater samples from Manizales (Caldas, Colombia) were analyzed, and concentrations of E1, E2, EE2, and E3 were 7.2, 0.1, 6.7, and 33.2 µg L⁻¹, respectively. Limits of detection ranged from 0.06 to 0.40 µg L⁻¹, and limits of quantification from 0.16 to 1.20 µg L⁻¹. Calibration curves for all analytes showed R² values above 0.98. Recovery values obtained through standard addition calibration ranged from 56 % to 90 %, despite significant matrix effects (–67 to 230). The MMT/HAp composite demonstrated comparable performance to the commercial HLB sorbent, confirming its potential for environmental applications.
医院废水处理厂中存在类固醇激素的环境问题突出表明,需要制定有效的监测和去除战略。即使在微量水平,类固醇雌激素也表现出很强的生物活性和生物积累潜力,将其归类为内分泌干扰化合物。本研究提出了蒙脱土/羟基磷灰石(MMT/HAp)复合材料作为一种环保、低成本的提取雌酮(E1)、17β-雌二醇(E2)、17α-炔雌二醇(EE2)和雌三醇(E3)的替代材料。采用旋转圆盘吸附萃取绿色分析方法制备样品。考虑到废水基质的复杂性,在选择性离子监测模式下,采用气相色谱-质谱联用(GC-MS)对分析物进行测定。采用Doehlert实验设计优化提取工艺,得到最佳提取条件:提取时间87 min,进样量16 mL,搅拌速度1080 rpm。医院废水样本马尼萨莱斯(卡尔达斯、哥伦比亚)进行了分析和浓度的E1, E2, EE2,和E3是7.2,0.1,6.7,和33.2µg L⁻¹,分别。检测范围为0.06 - 0.40µg L -毒血症,定量范围为0.16 - 1.20µg L -毒血症。所有分析物的校正曲线R²值均在0.98以上。尽管有显著的基质效应(-67至230),但通过标准添加校准获得的回收率从56%到90%不等。MMT/HAp复合材料表现出与商用HLB吸附剂相当的性能,证实了其在环境应用方面的潜力。
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引用次数: 0
Developing 2D mzCompare for single comprehensive two-dimensional chromatography time-of-flight mass spectrometry chromatograms: Substantial resolution enhancement in the context of statistical overlap theory 在统计重叠理论的背景下,开发单个综合二维色谱飞行时间质谱色谱图的二维mzCompare:大幅提高分辨率。
IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Pub Date : 2026-02-22 Epub Date: 2026-01-02 DOI: 10.1016/j.chroma.2025.466669
Wenjing Ma, Caitlin N. Cain, Robert E. Synovec
Accurate identification of all detectable analyte components in a single comprehensive two-dimensional (2D) gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS) chromatogram is a fundamental interest in the field. While commercial software tools intended for this purpose are available, the performance of these tools to generate an accurate peak table has generally not been validated. To address this, we developed a new algorithmic software approach called 2D mzCompare to generate accurate peak tables for GC × GC-TOFMS. Extending from our original method for one-dimensional GC–MS data, the 2D mzCompare algorithm discovers selective mass channels (m/z) for each analyte to resolve overlapping peaks and improve analyte identification, by leveraging the similarity in retention time and peak shape across m/z of the same analyte. The 2D mzCompare algorithm calculates the peak shape similarity between m/z at every modulation, followed by clustering and focusing steps, to generate a final peak table. To evaluate this software, we simulated realistic GC × GC-TOFMS data in the context of the statistical overlap theory (SOT), so the exact number and identities of analytes are known a priori. Utilizing an in-house mass spectrum library of similar compounds, GC × GC-TOFMS chromatograms were simulated with varying degrees of 2D chromatographic saturation (α2D). At low saturation factors (α2D = 0.01, 0.03, and 0.1), over 95% of the simulated components are found to be mathematically resolved singlets (pure analyte components) by 2D mzCompare. Meanwhile, approximately 62% were found at α2D = 1, exceeding predictions made by SOT. Application of 2D mzCompare computationally reduces the 2D peak widths, resulting in an ∼12-fold reduction in α2D. The results of this research are simultaneously two-fold. First, we provide a new algorithmic approach, 2D mzCompare, to resolve overlapped analytes in GC × GC-TOFMS data, and second, we validate the accuracy of the software performance using SOT.
在一个全面的二维(2D)气相色谱-飞行时间质谱(GC × GC- tofms)色谱图中准确识别所有可检测的分析物成分是该领域的一个基本兴趣。虽然用于此目的的商业软件工具是可用的,但这些工具生成准确峰值表的性能通常尚未得到验证。为了解决这个问题,我们开发了一种新的算法软件方法,称为2D mzCompare,用于生成GC × GC- tofms的准确峰表。从一维GC-MS数据的原始方法扩展,二维mzCompare算法为每个分析物发现选择性质量通道(m/z),以解决重叠峰,并通过利用相同分析物在m/z上的保留时间和峰形的相似性来提高分析物识别。二维mzCompare算法计算每个调制下m/z之间的峰形相似性,然后进行聚类和聚焦步骤,以生成最终的峰表。为了评估该软件,我们在统计重叠理论(SOT)的背景下模拟了真实的GC × GC- tofms数据,因此分析物的确切数量和身份是先验的。利用内部类似化合物的质谱库,以不同程度的二维色谱饱和度(α2D)模拟GC × GC- tofms色谱图。在低饱和因子(α2D = 0.01, 0.03和0.1)下,通过2D mzCompare发现95%以上的模拟组分是数学上可分辨的单重态(纯分析物组分)。同时,在α2D = 1处发现了约62%,超出了SOT的预测。应用2D mzCompare计算减少了2D峰宽,导致α2D降低了约12倍。这项研究的结果是双重的。首先,我们提供了一种新的算法,2D mzCompare,来解决GC × GC- tofms数据中的重叠分析,其次,我们使用SOT验证了软件性能的准确性。
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引用次数: 0
Exploring adsorption–desorption kinetics and eddy dispersion in enantioselective hydrophilic interaction chromatography using teicoplanin-based chiral stationary phase 利用基于teicoplanin的手性固定相探索对映选择性亲水性相互作用色谱的吸附-解吸动力学和涡流分散
IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Pub Date : 2026-02-22 Epub Date: 2026-01-10 DOI: 10.1016/j.chroma.2026.466702
Chiara De Luca , Chiara Nosengo , Amirmohammad Faraji Shovey , Antonio Ricci , Martina Catani , Alberto Cavazzini , Fabrice Gritti , Simona Felletti
This research examined the kinetic behavior of two chiral probes (FMOC-Alanine and Haloxyfop) using a zwitterionic teicoplanin-based column and an aqueous-methanol mobile phase. More specifically, experimental results, supported by literature data measured using the same elution mode, indicate that the presence of a water layer adsorbed on the particle surface hinders analyte surface diffusion leading to localized adsorption. This shows cascading effects on longitudinal diffusion, solid–liquid mass transfer resistance and eddy dispersion, which become analyte-independent. The only difference in the measured plate heights is therefore given only by slow adsorption–desorption kinetics, confirming an important correlation between analyte structure and the extent of band broadening in chiral chromatography.
The findings reported in this study can be expanded to other molecules, suggesting that similar kinetic behavior could be expected if the same experimental conditions are maintained (e.g., same column manufacturer, silica particles, and elution mode). This would help accelerating the method development and the understanding of both the chiral recognition mechanism and the sources of band broadening occurring in chiral chromatography.
本研究使用两性离子teicoplanin基柱和水-甲醇流动相考察了两种手性探针(fmoc -丙氨酸和Haloxyfop)的动力学行为。更具体地说,使用相同洗脱模式测量的文献数据支持的实验结果表明,颗粒表面吸附的水层的存在阻碍了分析物表面的扩散,导致局部吸附。这显示了纵向扩散、固液传质阻力和涡流色散的级联效应,它们与分析物无关。因此,测量板高度的唯一差异仅由缓慢的吸附-解吸动力学给出,证实了手性色谱中分析物结构与波段拓宽程度之间的重要相关性。本研究报告的发现可以扩展到其他分子,表明如果保持相同的实验条件(例如,相同的色谱柱制造商,二氧化硅颗粒和洗脱模式),可以预期类似的动力学行为。这将有助于加快方法的发展和对手性识别机制和手性色谱中发生的带拓宽来源的理解。
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引用次数: 0
Efficient analysis of sodium chromate by combining phase-transfer headspace strategy and GC-TCD 相转移顶空策略与GC-TCD相结合的高效分析铬酸钠
IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Pub Date : 2026-02-22 Epub Date: 2025-12-24 DOI: 10.1016/j.chroma.2025.466657
Wei-Qi Xie, Ya-Yun Wang, Yi-Xan Gong
This study developed a gas-evolving phase-transfer strategy for precise sodium chromate quantification. The analytical approach utilized the chemical reaction between sodium chromate and oxalic acid to generate measurable carbon dioxide, which was subsequently quantified via headspace gas chromatography equipped with thermal conductivity detector (HS-GC-TCD). Experimental validation confirmed the method's exceptional analytical performance in sodium chromate determination. The developed phase transformation technique established a robust and efficient protocol for sodium chromate assessment while simultaneously creating a framework for extending this analytical paradigm to other gas-evolving compounds.
本研究开发了一种用于精确定量铬酸钠的气相转移策略。分析方法利用铬酸钠和草酸之间的化学反应产生可测量的二氧化碳,随后通过配备热导检测器的顶空气相色谱(HS-GC-TCD)进行定量。实验验证了该方法在铬酸钠测定中具有优异的分析性能。开发的相变技术为铬酸钠的评估建立了一个强大而有效的协议,同时创建了一个框架,将这种分析范式扩展到其他气态化合物。
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引用次数: 0
Determination of 15 phthalates metabolites and 9 bisphenols in human serum by using high-performance liquid chromatography coupled with tandem mass spectrometry 高效液相色谱-串联质谱法测定人血清中15种邻苯二甲酸酯代谢物和9种双酚类物质
IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Pub Date : 2026-02-22 Epub Date: 2026-01-22 DOI: 10.1016/j.chroma.2026.466728
Yilin Liu , Juan Wen , Xu Zhang , Xiao Lin , Zhuangzhuang Feng , Dejun Bao , Xiaojian Hu , Ying Zhu
Endocrine disrupting chemicals (EDCs) are a class of emerging contaminants that have raised significant public health concerns. Human co-exposure to mixtures of specific EDCs, such as phthalate and bisphenols, and the associated health risks remain poorly understood. To support biomonitoring and epidemiological studies on these compounds, there is a critical need for sensitive and reliable methods for their quantification in human specimens. Herein, we developed and validated an analytical method based on ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) for the simultaneous determination of 15 phthalate metabolites and 9 bisphenols in human serum. A systematic comparison between liquid-liquid extraction (LLE) and high-efficiency matrix removal (HMR) clean-up approach revealed that HMR offered advantages in terms of extraction efficiency and matrix effect reduction, and was ultimately selected as the final clean-up method for this study. The developed method demonstrated satisfactory performance, with recoveries ranging from 81 % to 115 %, with the relative standard deviations (RSD) below 18 %. The calibration curves established using isotope-labeled internal standards exhibited good linearity, with correlation coefficients (R2) consistently above 0.997. The limits of detection (LODs) and limits of quantification (LOQs) were determined to be in the range of 0.01 ng/mL to 0.2 ng/mL and 0.04 ng/mL to 0.7 ng/mL, respectively. Both intra-day and inter-day precision were satisfactory, with RSDs values ranging from 4.2 % to 13 % and 6.9 % to 14 %, respectively. This sensitive analytical method was successfully applied to the determination of target analytes in human serum samples from 15 pregnant women, demonstrating its applicability for monitoring of these emerging contaminants in human serum.
内分泌干扰物(EDCs)是一类新兴污染物,已引起重大的公共卫生问题。人类共同暴露于特定的EDCs混合物,如邻苯二甲酸酯和双酚,以及相关的健康风险仍然知之甚少。为了支持这些化合物的生物监测和流行病学研究,迫切需要在人类标本中建立敏感可靠的定量方法。在此,我们建立并验证了一种基于超高效液相色谱-串联质谱(UHPLC-MS/MS)同时测定人血清中15种邻苯二甲酸酯代谢物和9种双酚类物质的分析方法。通过对液液萃取(LLE)和高效基质去除(HMR)净化方法的系统比较,发现HMR在萃取效率和基质效应降低方面具有优势,最终选择了液液萃取作为本研究的最终净化方法。该方法回收率为81% ~ 115%,相对标准偏差(RSD)小于18%。采用同位素标记内标建立的标准曲线线性良好,相关系数(R2)均在0.997以上。检测限和定量限范围分别为0.01 ng/mL ~ 0.2 ng/mL和0.04 ng/mL ~ 0.7 ng/mL。日内和日内精密度均较好,rsd值分别为4.2% ~ 13%和6.9% ~ 14%。该灵敏的分析方法成功地应用于15例孕妇血清样品中目标分析物的测定,证明了该方法对监测这些新出现的人血清污染物的适用性。
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引用次数: 0
Comparative assessment of feature and component profiling workflow for supercritical fluid chromatography – high resolution mass spectrometry analysis 超临界流体色谱-高分辨率质谱分析的特征和组分分析工作流程的比较评估。
IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Pub Date : 2026-02-22 Epub Date: 2026-01-22 DOI: 10.1016/j.chroma.2026.466730
Samuele Pellacani , Giorgio Tomasi , Gerrit Renner , Selina Tisler
Supercritical fluid chromatography coupled to high-resolution mass spectrometry (SFCHRMS) is gaining attention for non-target screening (NTS), yet systematic evaluations of data-processing workflows remain scarce. Here, we present the first comprehensive comparison between a component-profile (CP) approach based on Region of Interest analysis combined with Component Detection Algorithm and Multivariate Curve Resolution (ROI-CODA-MCR) and a feature-profile (FP) workflow, MS-DIAL. Using extracted ion chromatograms (EICs) as ground truth, both workflows were optimized and benchmarked for standard detection, peak intensity reliability, blank filtering performance, and suspect screening for wastewater samples. Both detected a comparable number of standards (33–35 out of 37) but ROI-derived intensities closely matched EICs (average ratio ≈1, RSD = 5.8%), while MS-DIAL intensities deviated substantially (up to two orders of magnitude, RSD >200%). In non-target analysis, MS-DIAL produced ≈1000 features with many false positives, while ROI-CODA-MCR yielded ≈200 components with lower blank contributions and superior resolution of in-source fragments and adducts. MS-DIAL detected more suspect compounds, highlighting a higher risk of false negatives in the CP approach, particularly for low-intensity or sparse signals. Our results demonstrate that SFCHRMS datasets, often including intense background signals, challenge key assumptions underlying both FP and CP workflows and necessitate careful parameter optimization.
超临界流体色谱联用高分辨率质谱(SFCHRMS)在非目标筛选(NTS)中越来越受到关注,但对数据处理工作流程的系统评估仍然很少。在这里,我们首次全面比较了基于兴趣区域分析结合成分检测算法和多元曲线分辨率(ROI-CODA-MCR)的成分轮廓(CP)方法和特征轮廓(FP)工作流MS-DIAL。利用提取离子色谱(EICs)作为基础,对两个工作流程进行了优化,并对标准检测、峰值强度可靠性、空白过滤性能和废水样品的可疑筛选进行了基准测试。两者都检测到相当数量的标准(37个标准中有33-35个标准),但roi衍生强度与EICs非常匹配(平均比率≈1,RSD = 5.8%),而MS-DIAL强度偏差很大(高达两个数量级,RSD bb0 200%)。在非目标分析中,MS-DIAL产生了约1000个具有许多假阳性的特征,而ROI-CODA-MCR产生了约200个具有较低空白贡献和较高源内片段和加合物分辨率的成分。MS-DIAL检测到更多可疑化合物,突出了CP方法中假阴性的较高风险,特别是对于低强度或稀疏信号。我们的研究结果表明,SFCHRMS数据集通常包括强烈的背景信号,挑战了FP和CP工作流程的关键假设,需要仔细的参数优化。
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引用次数: 0
期刊
Journal of Chromatography A
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