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A critical review and analysis of thermodynamic and kinetic effects on extraction of medical devices by organic solvents as a sample preparation step in devices’ chemical characterization 综述和分析了有机溶剂萃取医疗器械作为样品制备步骤在器械化学表征中的热力学和动力学影响
IF 3.2 Pub Date : 2026-01-18 DOI: 10.1016/j.jcoa.2026.100309
By Jianwei Li
The extraction of medical devices by organic solvents as a sample preparation step is perhaps the most critical process in chemical characterization of medical devices, as the decision of solvent choice determines not only the resulting extractables profiles (e.g., the number, molecular weight, and concentration of extractables), but also the degree of analytical challenges in identification and quantification, when performing instrumental analysis of extracts. Both concentration and chemical identities of all extractables are used in subsequent toxicological risk assessment, which is required to support regulatory submission and approval of medical devices. There is currently a considerable debate on which solvent(s) should be used to balance the desired extraction and clinical relevance to biological tissue exposure due to scientific and regulatory consequences. The purpose of this article is intended to streamline solvent selection in chemical characterization, particularly on the rational development of a semipolar solvent to stimulate or exaggerate biological (storage) fatty tissues. A comprehensive review and analysis of solvent extraction of polymer materials from thermodynamic and kinetic perspectives is provided first. The solvent-material interactions (swelling) and their consequences on kinetics and thermodynamics are subsequently elaborated. The conclusions of thermodynamic and kinetic properties, together with solvent-material interactions, are used to establish solvent similarity criteria between semipolar solvents and fatty tissues. Finally, solvent solubility, degree of material swelling by solvents, diffusion coefficients in device material, partition coefficient between material and solvent, and solvent compatibility with instrumental analysis are used as the criteria to establish representative solvents to fatty tissues in chemical characterization studies. Blood simulating solvents are well established and not discussed in the article.
用有机溶剂提取医疗器械作为样品制备步骤可能是医疗器械化学表征中最关键的过程,因为溶剂选择的决定不仅决定了所得到的可提取物谱(例如,可提取物的数量、分子量和浓度),而且还决定了在对提取物进行仪器分析时,在鉴定和定量方面的分析挑战程度。所有萃取物的浓度和化学特性都用于随后的毒理学风险评估,这是支持向监管机构提交和批准医疗设备所必需的。由于科学和监管的后果,目前对于应该使用哪种溶剂来平衡所需的提取和生物组织暴露的临床相关性存在相当大的争论。本文旨在简化化学表征中溶剂的选择,特别是半极性溶剂的合理开发,以刺激或夸大生物(储存)脂肪组织。本文首先从热力学和动力学的角度对高分子材料的溶剂萃取进行了综述和分析。随后阐述了溶剂-物质相互作用(溶胀)及其对动力学和热力学的影响。热力学和动力学性质的结论,连同溶剂-材料相互作用,用于建立半极性溶剂和脂肪组织之间的溶剂相似标准。最后,以溶剂溶解度、材料被溶剂溶胀程度、器件材料中的扩散系数、材料与溶剂的分配系数以及溶剂与仪器分析的相容性作为标准,建立脂肪组织在化学表征研究中的代表性溶剂。血液模拟溶剂已经很好地建立,本文中没有讨论。
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引用次数: 0
Estimating non-specific aquatic toxicity for the fathead minnow using surrogate chromatographic models 用替代色谱模型估计黑头鲦鱼的非特异性水生毒性
IF 3.2 Pub Date : 2026-01-15 DOI: 10.1016/j.jcoa.2026.100307
Sanka N. Atapattu , Colin F. Poole
In the assessment of aquatic toxicity, the fathead minnow (Pimephales promelas), a small fish species, is commonly used as an indicator. A major challenge in environmental risk assessment is predicting the aquatic toxicity of tens of thousands of emerging chemical contaminants and their metabolites, especially when no experimental data exist in the public domain or there is no means to generate new information. In this work the correlation of reversed-phase liquid chromatography and micellar electrokinetic chromatography retention factors to estimate fathead minnow toxicity was explored. We identified several surrogate chromatographic systems to estimate aquatic non-specific toxicity for the fathead minnow. We identified the reversed-phase liquid chromatography system comprising the XTerra MS C18 10% tetrahydrofuran-water binary solvent system and the micellar electrokinetic chromatography system utilizing the surfactant hexadecyltrimethylammonium bromide with prediction errors of 0.231–0.287 and 0.141–0.179 log units as suitable surrogate chromatographic systems to estimate non-specific aquatic toxicity for the fathead minnow.
在评估水生毒性时,通常使用一种小型鱼类——大头鲦鱼(Pimephales promelas)作为指标。环境风险评估的一个主要挑战是预测数以万计的新出现的化学污染物及其代谢物的水生毒性,特别是在公共领域没有实验数据或没有办法产生新信息的情况下。本文探讨了反相液相色谱法和胶束电动色谱法保留因子在黑头鲦鱼毒性评价中的相关性。我们确定了几种替代色谱系统来估计水对黑头鲦鱼的非特异性毒性。我们确定了由XTerra MS C18 10%四氢呋喃-水二元溶剂体系组成的反相液相色谱体系和使用表面活性剂十六烷基三甲基溴化铵的胶束电动色谱体系,其预测误差分别为0.231-0.287和0.141-0.179对数单位,作为预测黑头鱼非特异性水生毒性的合适替代色谱体系。
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引用次数: 0
Magnetic polyamidoamine dendrimer with thiol terminal groups for magnetic solid-phase extraction of selected organophosphorus pesticides followed by quantification through high-performance liquid chromatography-ultraviolet detection 以巯基为末端基团的磁性聚胺胺树状大分子,对选定的有机磷农药进行磁固相萃取,并采用高效液相色谱-紫外检测进行定量
IF 3.2 Pub Date : 2026-01-03 DOI: 10.1016/j.jcoa.2026.100306
Milad Ghani , Seyedeh Bentolhoda Hosseinian , Behrooz Maleki , Pouya Ghamari kargar
Herein, polyamidoamine-SH dendrimer@Fe3O4 (PAMAM-SH@Fe3O4) was synthesized using a simple, green, fast, cost-effective, and efficient method. Firstly, polyamidoamine dendrimer with SH terminal groups (PAMAM-SH) was prepared by the Michael addition method. Subsequently, PAMAM-SH was immobilized on the surface of Fe3O4 nanoparticles. The proposed PAMAM-SH@Fe3O4 material exhibits superior extraction efficiency compared to conventional sorbents due to its abundant functional groups and thiol modifications, enabling highly effective MSPE of organophosphorus pesticides in complicated matrices. The obtained PAMAM-SH@Fe3O4 nanocomposite was utilized as a sorbent for magnetic solid-phase extraction (MSPE) of four selected organophosphorus pesticides (OPPs), including diazinon, malathion, chlorpyrifos, and phosalone. The extracted analytes were then desorbed using methanol (as the appropriate eluent) and analyzed by high-performance liquid chromatography with ultraviolet detection (HPLC-UV). Under optimized condition, the method exhibited good linearity in the range of 0.10–500.00 µg L⁻¹ for the target analytes (corresponding coefficients of determination (R²) > 0.9923). The limits of detection (LODs) and quantification (LOQs) were in the ranges of 0.02–0.13 µg L⁻¹ and 0.08–0.42 µg L⁻¹, respectively. Inter- and intra-day relative standard deviations (RSDs) were between 1.60% and 5.90%. The enrichment factors (EFs) were determined to be 79.00, 84.00, 72.00, and 81.00 for diazinon, malathion, chlorpyrifos, and phosalone, respectively. The proposed method was successfully applied to real samples, including apples, pears, peaches, grapes, and agricultural wastewater, demonstrating its reliability and applicability for complex matrices.
本文采用简单、绿色、快速、经济、高效的方法合成了聚酰胺胺- sh dendrimer@Fe3O4 (PAMAM-SH@Fe3O4)。首先,采用Michael加成法制备了具有SH末端基团的聚氨基胺树状大分子(PAMAM-SH);随后,PAMAM-SH被固定在Fe3O4纳米颗粒表面。与传统吸附剂相比,PAMAM-SH@Fe3O4材料由于其丰富的官能团和巯基修饰,具有更高的萃取效率,能够在复杂基质中高效地进行有机磷农药的MSPE。以PAMAM-SH@Fe3O4纳米复合材料为吸附剂,对四种有机磷农药(包括二嗪农、马拉硫磷、毒死蜱和磷沙酮)进行磁固相萃取。提取的分析物用甲醇(作为合适的洗脱液)解吸,用高效液相色谱-紫外检测(HPLC-UV)分析。在优化条件下,该方法在0.10 ~ 500.00µg L⁻¹范围内呈现良好的线性关系(相应的测定系数(R²)> 0.9923)。检测限(lod)和定量限(loq)分别在0.02-0.13µg L⁻¹和0.08-0.42µg L⁻¹之间。日内、日间相对标准偏差(rsd)在1.60% ~ 5.90%之间。二嗪农、马拉硫磷、毒死蜱和福沙酮的富集因子(EFs)分别为79.00、84.00、72.00和81.00。该方法成功应用于实际样品,包括苹果、梨、桃、葡萄和农业废水,证明了其对复杂基质的可靠性和适用性。
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引用次数: 0
Analytical approaches for the identification and quantitation of nitazenes: a review nitazene的鉴定和定量分析方法综述
IF 3.2 Pub Date : 2025-12-29 DOI: 10.1016/j.jcoa.2025.100305
Roberto Mandrioli , Michele Protti , Roberta Di Lecce , Laura Mercolini
Nitazenes, a class of high-potency novel synthetic opioids containing a benzimidazole moiety, are currently being reported across seized materials and drug-checking submissions, human biological matrices (postmortem and clinical/forensic) and community-level samples including wastewater. The analytical literature converges on a layered, matrix-oriented toolkit. Rapid presumptive strategies (vibrational fingerprints and ambient-ionization techniques) support triage in solids and field-adjacent contexts, while chromatographic separations coupled to mass spectrometry (HPLC-MS/MS/HRMS and less frequently GC–MS/MS/HRMS) deliver selectivity and structure-aware confirmation for closely related analogues. In human biofluids, both targeted triple-quadrupole panels and HRMS suspect screening workflows are present for identification; validated quantitative methods consistently address calibration model and range, sensitivity (LOD/LLOQ), precision and accuracy, selectivity, carry-over and matrix effects, often with explicit attention to isomer resolution. Cross-cutting issues recurring in the field include reference standard availability, isomeric/isobaric interferences, immunoassay cross-reactivity and the promise of miniaturised sampling formats. Organised by matrix and analytical objective, this review provides enough information to enable efficient extraction of details at the method level, while ensuring a comprehensive coverage of the most important topics.
Nitazenes是一类含有苯并咪唑部分的高效新型合成阿片类药物,目前在查获的材料和药物检查提交材料、人类生物基质(尸检和临床/法医)以及包括废水在内的社区样本中都有报告。分析文献集中在一个分层的、面向矩阵的工具包上。快速推定策略(振动指纹和环境电离技术)支持固体和现场邻近环境中的分类,而色谱分离耦合质谱(HPLC-MS/MS/HRMS和较少的GC-MS /MS/HRMS)为密切相关的类似物提供选择性和结构感知确认。在人体生物体液中,有针对性的三重四极杆面板和HRMS可疑筛选工作流程可供识别;经过验证的定量方法一致地处理校准模型和范围,灵敏度(LOD/LLOQ),精密度和准确度,选择性,携带和矩阵效应,通常明确关注同分异体分辨率。该领域反复出现的交叉问题包括参考标准的可用性、同分异构体/等压干扰、免疫测定交叉反应性和小型化采样格式的前景。通过矩阵和分析目标的组织,本综述提供了足够的信息,以便在方法层面上有效地提取细节,同时确保对最重要主题的全面覆盖。
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引用次数: 0
Comprehensive characterization of Xuebijing injection and comparative analysis of its systemic exposure in patients with severe pneumonia, sepsis, and acute pancreatitis 血必净注射液的综合表征及其在重症肺炎、脓毒症和急性胰腺炎患者全身暴露的比较分析
IF 3.2 Pub Date : 2025-12-23 DOI: 10.1016/j.jcoa.2025.100304
Mingxin Guo , Shuo Chen , Xia Wu , Zhiqiang Hu , Yanchun Chen , Baohu Jiang
This study aimed to investigate the chemical constituents of Xuebijing injection and compare differences in its systemic exposure components among patients with severe pneumonia, sepsis, and acute pancreatitis during the steady-state blood concentration phase. Using ultra-high-performance liquid chromatography-mass spectrometry, compounds were identified and analyzed based on retention time, accurate molecular weight, secondary mass spectrometry fragmentation patterns, and comparisons with reference standards and databases. A total of 55 chemical constituents were identified in Xuebijing injection, primarily flavonoids, organooxygen compounds, prenol lipids, and isobenzofurans. In patient plasma, 16 components were detected in severe pneumonia patients, comprising 7 prototypes, 6 Phase I metabolites, and 3 Phase II metabolites; 32 components were found in acute pancreatitis patients, including 12 prototypes, 10 Phase I metabolites, and 10 Phase II metabolites; and 24 components were identified in sepsis patients, consisting of 8 prototypes, 9 Phase I metabolites, and 4 Phase II metabolites. Acute pancreatitis patients exhibited the highest number of systemic exposure components, followed by sepsis and severe pneumonia patients. Hydroxysafflor yellow A, paeoniflorin, and neocnidilide glucuronidation were consistently detected at relatively high concentrations across all groups. This study demonstrates the utility of ultra-high-performance liquid chromatography-mass spectrometry for rapid profiling of the chemical composition of Xuebijing injection and its blood-exposed components, providing a reference for elucidating its pharmacodynamic material basis and mechanism of action.
本研究旨在研究血必净注射液的化学成分,比较其在重症肺炎、脓毒症和急性胰腺炎患者稳态血药浓度阶段全身暴露成分的差异。使用超高效液相色谱-质谱法,根据保留时间、精确分子量、二级质谱破碎模式以及与参考标准品和数据库的比较,对化合物进行鉴定和分析。从血痹净注射液中鉴定出55种化学成分,主要为黄酮类化合物、有机氧化合物、丙烯醇脂类和异苯并呋喃类。在重症肺炎患者血浆中检测到16种成分,包括7种原型物、6种I期代谢物和3种II期代谢物;在急性胰腺炎患者中发现32种成分,包括12种原型,10种I期代谢物,10种II期代谢物;在脓毒症患者中鉴定出24种成分,包括8种原型物、9种I期代谢物和4种II期代谢物。急性胰腺炎患者表现出最多的全身暴露成分,其次是败血症和严重肺炎患者。在所有组中,羟基红花黄A、芍药苷和新桂枝苷葡萄糖醛酸化均以相对较高的浓度检测到。本研究利用超高效液相色谱-质谱联用技术快速分析血必净注射液及其血暴露成分的化学成分,为阐明血必净注射液的药效学、物质基础和作用机制提供参考。
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引用次数: 0
Citizen science and analytical chemistry. Oxymoron or harmony of meaning? 公民科学和分析化学。矛盾修饰法还是意思和谐?
IF 3.2 Pub Date : 2025-12-20 DOI: 10.1016/j.jcoa.2025.100302
Giacomo Musile , Miryam Perrucci , Erika Maria Ricci , Antonio Maria Catena , Cristian D’Ovidio , Marcello Locatelli
Citizen science is rapidly emerging as a transformative force in analytical chemistry by opening research participation to non-specialists and expanding where and how data can be collected. This report explores how recent technological advances have made analytical tools simpler, smaller, and more affordable. These developments have enabled citizens and students to be engaged directly in environmental monitoring, food-quality assessment, and educational activities, often producing data comparable to those generated in laboratories. In addition, several emerging prototypes have been purposefully designed with citizen use in mind, anticipating future applications in participatory science. The discussion also addresses areas where citizen science could play a growing role, including biomedical and forensic analysis, while recognizing challenges related to data reliability, ethics, and validation. Overall, this report highlights how accessible technologies, supported by artificial intelligence and digital communication, are transforming analytical chemistry into a more inclusive and collaborative discipline, connecting scientific research with everyday life.
通过向非专业人士开放研究参与,扩大数据收集的地点和方式,公民科学正迅速成为分析化学领域的一股变革力量。本报告探讨了最近的技术进步如何使分析工具更简单、更小、更实惠。这些发展使公民和学生能够直接参与环境监测、食品质量评估和教育活动,经常产生可与实验室产生的数据相媲美的数据。此外,几个新兴的原型已经被有意地设计为公民使用,预测未来在参与性科学中的应用。讨论还讨论了公民科学可以发挥越来越大作用的领域,包括生物医学和法医分析,同时认识到与数据可靠性、伦理和验证相关的挑战。总体而言,本报告强调了在人工智能和数字通信的支持下,可获取的技术如何将分析化学转变为更具包容性和协作性的学科,将科学研究与日常生活联系起来。
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引用次数: 0
Study on enantioselective recognition of metofoline enantiomers with cyclodextrins using capillary electrophoresis, nuclear magnetic resonance spectroscopy and molecular modeling techniques 应用毛细管电泳、核磁共振波谱和分子模拟技术研究环糊精对甲托亚胺对映体的选择性识别
IF 3.2 Pub Date : 2025-12-18 DOI: 10.1016/j.jcoa.2025.100303
Ketevan Museridze , Ann Gogolashvili , Lali Chankvetadze , Giorgi Jibuti , Antonio Salgado , Barbara Sechi , Paola Peluso , Bezhan Chankvetadze
Compared to any other analytical technique, the main advantage of using capillary electrophoresis (CE) for studying enantioselective recognition mechanisms in intermolecular interaction is its higher sensitivity to detect weak noncovalent interactions. Furthermore, nuclear magnetic resonance (NMR) and molecular modeling proved to be very effective to complement CE for mechanistic purposes. On the other hand, multiple factors may impact selector-selectand geometries and binding energies affecting the overall enantiorecognition process. In this regard, the validation of computational tools to verify the reliability of proposed models is still a critical issue, and suitable experimental data sets are necessary for this purpose. In this study, we combined CE, NMR spectroscopy and molecular modeling with the aim of investigating the molecular bases of the enantioseparations of metofoline (MF) with β-cyclodextrin (CD), γ-CD, and heptakis(2,3-di-O-acetyl)-β-CD (HDA-β-CD). Based on this strategy and focusing on the reversal of migration order observed by using γ-CD [(R)-(S)] in place of β-CD [(S)-(R)], good agreement between experimental and theoretical data was obtained. The absolute configuration of MF enantiomers was assigned by comparison of experimental and computed chiroptical spectra.
与其他分析技术相比,毛细管电泳(CE)用于研究分子间相互作用对映体选择性识别机制的主要优点是其对弱非共价相互作用的检测灵敏度较高。此外,核磁共振(NMR)和分子模型被证明是非常有效的补充CE的机制目的。另一方面,多种因素可能影响选择器的选择,几何形状和结合能影响整个对映体识别过程。在这方面,验证计算工具以验证所提出模型的可靠性仍然是一个关键问题,为此需要合适的实验数据集。在本研究中,我们结合CE, NMR波谱和分子模型,目的是研究甲基叶酸(MF)与β-环糊精(CD), γ-CD和七烷基(2,3-二- o -乙酰基)-β-CD (HDA-β-CD)对映分离的分子基础。在此基础上,重点研究了用γ-CD [(R)-(S)]代替β-CD [(S)-(R)]观察到的迁移顺序反转,得到了实验数据与理论数据吻合较好的结果。通过比较实验和计算所得的红外光谱,确定了MF对映体的绝对构型。
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引用次数: 0
Preliminary characterization of wind turbine blade waste by solvolysis, microwave-assisted extraction, and comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry 通过溶剂溶解、微波辅助萃取和综合二维气相色谱-飞行时间质谱法对风力涡轮机叶片废弃物进行初步表征
IF 3.2 Pub Date : 2025-12-09 DOI: 10.1016/j.jcoa.2025.100301
Giulia Giacoppo , Charlotte Mase , Marco Piparo , Pierre Giusti , Caroline Mangote , Callum Branfoot , Luisa Pasti , Flavio Antonio Franchina , Marco Beccaria
The growth of renewable energy infrastructure highlights the urgent need for sustainable solutions to manage its end-of-life materials, including wind turbine blades (WTBs). These composite materials present significant challenges in recycling due to their complex heterogeneous structure and varied chemical composition. To depolymerize WTB composite materials, a solvolysis process was applied. The resulting chemical products underwent microwave-assisted extraction (MAE), using a mixture of n-hexane and methanol (10:3, v:v). The non-polar organic phase was subjected to analysis using comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry (GC×GC-ToFMS). On the basis of electron impact ionization mass spectral matching at 70 eV, linear retention index data, and molecular distribution on the two-dimensional space, >110 compounds were putatively identified, mainly composed by aromatic and heteroatom-containing species. To the best of our knowledge, this is the first time that the molecular composition of WTBs has been investigated by MAE-GC×GC–MS.
可再生能源基础设施的发展凸显了对可持续解决方案的迫切需求,以管理其报废材料,包括风力涡轮机叶片(WTBs)。这些复合材料由于其复杂的非均相结构和多变的化学成分,在回收方面面临着重大挑战。采用溶剂解聚法对WTB复合材料进行解聚。用正己烷和甲醇(10:3,v:v)的混合物进行微波辅助萃取(MAE)。非极性有机相采用综合二维气相色谱-飞行时间质谱法(GC×GC-ToFMS)进行分析。根据70 eV下的电子碰撞电离质谱匹配、线性保留指数数据和二维空间上的分子分布,推定鉴定出110种化合物,主要由芳香族和杂原子组成。据我们所知,这是第一次通过MAE-GC×GC-MS研究wtb的分子组成。
{"title":"Preliminary characterization of wind turbine blade waste by solvolysis, microwave-assisted extraction, and comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry","authors":"Giulia Giacoppo ,&nbsp;Charlotte Mase ,&nbsp;Marco Piparo ,&nbsp;Pierre Giusti ,&nbsp;Caroline Mangote ,&nbsp;Callum Branfoot ,&nbsp;Luisa Pasti ,&nbsp;Flavio Antonio Franchina ,&nbsp;Marco Beccaria","doi":"10.1016/j.jcoa.2025.100301","DOIUrl":"10.1016/j.jcoa.2025.100301","url":null,"abstract":"<div><div>The growth of renewable energy infrastructure highlights the urgent need for sustainable solutions to manage its end-of-life materials, including wind turbine blades (WTBs). These composite materials present significant challenges in recycling due to their complex heterogeneous structure and varied chemical composition. To depolymerize WTB composite materials, a solvolysis process was applied. The resulting chemical products underwent microwave-assisted extraction (MAE), using a mixture of <em>n-</em>hexane and methanol (10:3, v:v). The non-polar organic phase was subjected to analysis using comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry (GC×GC-ToFMS). On the basis of electron impact ionization mass spectral matching at 70 eV, linear retention index data, and molecular distribution on the two-dimensional space, &gt;110 compounds were putatively identified, mainly composed by aromatic and heteroatom-containing species. To the best of our knowledge, this is the first time that the molecular composition of WTBs has been investigated by MAE-GC×GC–MS.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"9 ","pages":"Article 100301"},"PeriodicalIF":3.2,"publicationDate":"2025-12-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145789691","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Chromatography on monolithic supports for biological nanoparticles and large biomolecules: Recent developments and state-of-the-art 生物纳米颗粒和大分子的单片支撑层析:最新发展和最新技术
IF 3.2 Pub Date : 2025-12-08 DOI: 10.1016/j.jcoa.2025.100300
Tomislav Friganović , Lucija Dončević , Djuro Josić
Chromatography on monolithic supports combines convective flow through interconnected macropores with tunable surface chemistries, enabling high-flow, low-shear purification of large biomolecules and biological nanoparticles. Recent developments in stationary-phase design, such as brush-grafted surfaces, together with optimized elution protocols, have additionally advanced both resolution and capacity across a broad range of targets. Demonstrated applications include the high-resolution separation of adeno-associated virus (AAV) empty and full capsids, isolation of supercoiled plasmid DNA, and removal of double-stranded RNA impurities from mRNA therapeutics. Furthermore, the platform’s tolerance for complex matrices enables efficient purification of extracellular vesicles and direct recovery of biotherapeutics from undiluted blood plasma. Miniaturized monolithic columns enable rapid and robust on-line monitoring of industrial processes for current good manufacturing practice (cGMP) control. Ongoing progress in multimodal chemistries, continuous and multicolumn operations, and integrated analytics establishes chromatography on monolithic supports as a versatile and robust platform for the rapid, selective purification of large biomolecules and biological nanoparticles and efficient monitoring of industrial processes.
单片支架上的色谱结合了通过相互连接的大孔的对流流动和可调节的表面化学性质,实现了大生物分子和生物纳米颗粒的高流量、低剪切纯化。固定相设计的最新发展,如刷接表面,以及优化的洗脱方案,在广泛的目标范围内进一步提高了分辨率和容量。演示的应用包括腺相关病毒(AAV)空衣壳和满衣壳的高分辨率分离,超卷曲质粒DNA的分离,以及mRNA疗法中双链RNA杂质的去除。此外,该平台对复杂基质的耐受性使细胞外囊泡的有效纯化和从未稀释的血浆中直接回收生物治疗药物成为可能。小型化整体柱能够快速和强大的在线监测工业过程的现行良好生产规范(cGMP)控制。在多模态化学、连续和多柱操作以及集成分析方面的持续进展,使单片支撑层析成为快速、选择性纯化大型生物分子和生物纳米颗粒以及有效监测工业过程的通用和强大平台。
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引用次数: 0
Development of simplified method for the detection of capsaicin using high performance liquid chromatography 高效液相色谱法测定辣椒素简便方法的建立
IF 3.2 Pub Date : 2025-11-28 DOI: 10.1016/j.jcoa.2025.100296
Jiang Huo , J. Heinrich Lieth , Qi Zhang , Pramod Pandey
Peppers are widely used for their pungency, and Scoville Heat Unit (SHU) is often used to measure the pungency of the peppers caused by compounds called capsaicinoids. Liquid Chromatography (LC) methods have emerged as effective tools for determining capsaicinoids. However, accurate extraction and quantification of capsaicin remain challenging. Here, we developed a simple, rapid, and robust high-performance liquid chromatography-ultraviolet detector (HPLC-UV) method for quantifying capsaicin in green Thai pepper (Bird’s eye chili). Capsaicin separation was achieved using a SiELC Newcrom R1 column (100 × 3.2 mm, 3 µm) under isocratic mobile phase consisting of 0.5 % formic acid in water and acetonitrile (30 %:70 %) at a flow rate of 0.4 mL/min. Detection of capsaicin was done at 220 nm and 280 nm wavelengths. Capsaicin extraction from pepper samples was evaluated at 20 min, 60 min, and 120 min intervals. Results showed that a 60-min extraction at 60 °C with orbital mixing 150 rpm was sufficient to recover the majority of the capsaicin from green Thai pepper. The method showed excellent linearity across 11 concentration levels (0.5 - 600 ppm) with an R2 value of 0.99. While capsaicin analysis has been investigated previously, this streamlined HPLC-UV method provides an accessible and effective alternative for improving capsaicin extraction and detection in green chili peppers.
辣椒因其辛辣而被广泛使用,史高维尔辣度单位(SHU)经常被用来衡量辣椒的辛辣程度,这种辣度是由辣椒素引起的。液相色谱法已成为测定辣椒素的有效方法。然而,辣椒素的准确提取和定量仍然具有挑战性。本文建立了一种简便、快速、可靠的高效液相色谱-紫外检测器(HPLC-UV)定量泰国青椒(鸟眼辣椒)中辣椒素的方法。采用SiELC Newcrom R1色谱柱(100 × 3.2 mm, 3µm)分离辣椒素,流动相为0.5%甲酸水溶液和乙腈(30%:70%),流速为0.4 mL/min。辣椒素的检测波长分别为220 nm和280 nm。辣椒样品中辣椒素的提取在20分钟,60分钟和120分钟的间隔进行评估。结果表明,在60°C条件下,以150转/分的转速进行60分钟的提取,可以回收泰国青椒中的大部分辣椒素。该方法在11个浓度水平(0.5 ~ 600 ppm)上线性良好,R2值为0.99。在前人研究辣椒素分析方法的基础上,建立了高效液相色谱-紫外分光光度法,为提高辣椒素的提取和检测水平提供了一种简便有效的方法。
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Journal of chromatography open
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