Journal of Chromatography A最新文献_第5页

Carboxyl hybrid monolithic column in-tube solid-phase microextraction coupled with UPLC-QTRAP MS/MS for the determination of amphetamine-type stimulants 羧基杂化整体柱管内固相微萃取与 UPLC-QTRAP MS/MS 联用测定苯丙胺类兴奋剂。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-10-22 DOI: 10.1016/j.chroma.2024.465464

Ling-yu Zhao , Mian Qin , Tian Zheng , Guo-ping Wu , Teng Lu

A carboxyl functionalized organic-inorganic hybrid monolithic column (TMOS-co-CES) was applied as in-tube solid-phase microextraction (SPME) sorbent combining with ultra-performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometer for separation and analyzation of seven typical amphetamine-type stimulants (ATSs), including amphetamine (AM), methamphetamine (MAM), cathinone, methcathinone, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine and 3,4-methylenedioxyethylamphetamine. The application potential of TMOS-co-CES material to ATSs was preliminarily confirmed by computational simulation by using cathinone as a representative. The influences of various SPME parameters and analytical performance were investigated systematically. As matched with the results of computational simulation, TMOS-co-CES column could capture ATSs under milder near neutral pH condition with high extraction efficiency basing on the adsorption mechanism explained as a mixed mode of electrostatic and hydrophobic interactions. Seven target trace ATSs in spiked sewage, pond water and urine could be rapidly and conveniently separated and enriched by the proposed TMOS-co-CES in-tube SPME method under the optimized conditions with good accuracy, repeatability and resistance to matrix interference. Moreover, AM and MAM had been successfully detected in real urines of suspected drug abusers by TMOS-co-CES in-tube SPME method, which indicated that the proposed method had good application feasibility for drug monitoring. The mild extraction condition and ideal method performance further made the TMOS-co-CES in-tube SPME method more potential in applications for forensic analysis and drug abuse.

应用羧基功能化有机-无机杂化整体柱（TMOS-co-CES）作为管内固相微萃取（SPME）吸附剂，结合超高效液相色谱-三重四极杆/线性离子阱质谱仪，分离分析了七种典型的苯丙胺类兴奋剂（ATSs）、包括苯丙胺（AM）、甲基苯丙胺（MAM）、卡西酮、甲卡西酮、3,4-亚甲二氧基苯丙胺、3,4-亚甲二氧基甲基苯丙胺和 3,4-亚甲二氧基乙基苯丙胺。以卡西酮为代表，通过计算模拟初步证实了 TMOS-co-CES 材料在苯丙胺类兴奋剂中的应用潜力。系统研究了各种 SPME 参数对分析性能的影响。与计算模拟结果相一致，TMOS-co-CES 柱在较温和的近中性 pH 条件下，基于静电和疏水相互作用混合模式的吸附机理，能以较高的萃取效率捕获苯丙胺类兴奋剂。在优化的条件下，采用TMOS-co-CES管内SPME方法可以快速、方便地分离和富集污水、池塘水和尿液中的7种目标痕量苯并咪唑类兴奋剂，具有良好的准确性、重复性和抗基体干扰性。此外，TMOS-co-CES管内SPME法成功地检测了吸毒嫌疑人真实尿液中的AM和MAM，表明该方法在毒品监测中具有良好的应用前景。TMOS-co-CES试管内SPME法的萃取条件温和、方法性能理想，使其在法医分析和药物滥用方面的应用更具潜力。

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引用次数: 0

Separation of nucleobases, nucleosides, nucleotides and oligonucleotides by hydrophilic interaction liquid chromatography (HILIC): A state-of-the-art review 亲水作用液相色谱法（HILIC）分离核碱基、核苷、核苷酸和寡核苷酸：最新进展综述。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-10-22 DOI: 10.1016/j.chroma.2024.465467

Yong Guo

The polar nature of nucleobases, nucleosides and nucleotides makes hydrophilic interaction chromatography (HILIC) a good choice of technology for separation. Both naturally occurring and modified nucleosides and nucleotides have been successfully separated in HILIC. A wide range of stationary phases with different retention and selectivity are suitable for the separation of nucleobases, nucleosides and nucleotides; and a sufficient knowledge base is also available to guide method development. Although oligonucleotides are significantly different from nucleotides in terms of polarity and charges, HILIC has been shown to be a viable alternative to ion-pairing reversed-phase liquid chromatography (IP-RPLC). Only a few polar stationary phases have been shown to provide satisfactory performance; however, the requirements for the mobile phase composition including organic solvent, mobile phase pH and salt concentration are sufficiently understood. This review provides a comprehensive evaluation of the chromatographic conditions with a historical perspective on adopting and developing HILIC for the separation of nucleobases, nucleosides, nucleotides and oligonucleotides. The areas for more research and potential directions for future development activities are identified and discussed.

核碱基、核苷和核苷酸的极性使亲水相互作用色谱（HILIC）成为分离技术的最佳选择。天然核苷和核苷酸以及经过修饰的核苷和核苷酸均已在 HILIC 中成功分离。具有不同保留和选择性的多种固定相都适用于核碱基、核苷和核苷酸的分离，而且有足够的知识基础来指导方法的开发。虽然寡核苷酸在极性和电荷方面与核苷酸有很大不同，但 HILIC 已被证明是离子配对反相液相色谱（IP-RPLC）的可行替代方法。只有少数极性固定相能提供令人满意的性能；不过，人们对流动相组成（包括有机溶剂、流动相 pH 值和盐浓度）的要求已经有了充分的了解。本综述从采用和发展 HILIC 分离核酸、核苷、核苷酸和寡核苷酸的历史角度，对色谱条件进行了全面评估。本文还确定并讨论了需要进一步研究的领域以及未来开发活动的潜在方向。

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引用次数: 0

An integrated strategy for deciphering quality markers of Terminaliae Belliricae Fructus based on a three-dimensional characteristic model 以三维特征模型为基础的解密贝母果质量标记的综合策略。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-10-22 DOI: 10.1016/j.chroma.2024.465465

Yi-Han Xu, Xin-Yue Chen, Juan Chen

Terminalia bellirica (Gaertn.) Roxb. is an ethnomedicinal plant that has been utilized in Tibetan and traditional Chinese medicine (TCM). Nevertheless, its quality standard officially listed in the Chinese Pharmacopoeia does not include any content determination of the indicator components of Terminaliae Belliricae Fructus, which constrains the effective quality evaluation of medicinal material and related products. In this paper, a three-dimensional “content-pharmacokinetics-pharmacology” network strategy was developed to identify the quality markers (Q-markers) of Terminaliae Belliricae Fructus in terms of “measurability”, “traceability” and “effectiveness”. Chromatographic fingerprint analysis was performed to outline its chemical contour, and identify the differential components of 17 batches of Terminaliae Belliricae Fructus combined with multivariate statistics analysis and UPLC-QTOF-MS analysis. Serum pharmacochemistry analysis was implemented on rats, and 25 prototype components absorbed into the blood were identified. By network pharmacology analysis, a component-disease-target-pathway network was constructed, thus validating the effectiveness of the chemical components of Terminaliae Belliricae Fructus. Afterwards, the above screened candidate components were put into construction of three-dimensional "radar chart". According to the calculated regression area (

R A

) and coefficient of variation (

C V

) values, the potential Q-markers was determined, followed by “specificity” evaluation. Ultimately, ellagic acid (EA), chebulagic acid (CHA), gallic acid (GA), chebulinic acid (CA), corilagin (CO) and chebulanin (CH) were specified as the Q-markers of Terminaliae Belliricae Fructus. Owing to high content, good pharmacokinetic property, high pharmacological activities and specificity. The screened Q-markers could offer a scientific foundation for the quality control of Terminaliae Belliricae Fructus, and the proposed strategy is demonstrated to be reliable and feasible for deciphering Q-markers of TCM.

蝙蝠蛾属植物（Terminalia bellirica (Gaertn.) Roxb.）是一种民族药用植物，在藏医和传统中医学中均有应用。然而，《中国药典》正式收载的药材质量标准中并没有对蝙蝠葛的指标成分进行含量测定，这制约了药材及相关产品的有效质量评价。本文从 "可测性"、"可追溯性 "和 "有效性 "三个方面，建立了 "含量-药代动力学-药理学 "三维网络策略，以确定鸡枞的质量标志物（Q-markers）。通过色谱指纹图谱分析，勾勒出其化学轮廓，并结合多元统计分析和 UPLC-QTOF-MS 分析，确定了 17 个批次的鸡冠花的不同成分。对大鼠进行血清药理分析，确定了吸收入血的 25 种原型成分。通过网络药理学分析，构建了 "成分-疾病-靶点-通路 "网络，从而验证了鸡冠花化学成分的有效性。随后，将上述筛选出的候选成分构建成三维 "雷达图"。根据计算出的回归面积（RA）和变异系数（CV）值，确定潜在的 Q 标记，然后进行 "特异性 "评估。最终，鞣花酸（EA）、诃子鞣花酸（CHA）、没食子酸（GA）、诃子鞣花酸（CA）、柯里拉京（CO）和诃子鞣花宁（CH）被确定为鸡冠花的 Q 标志物。所筛选出的 Q 标记物具有含量高、药代动力学特性好、药理活性高和特异性强等特点。所筛选的Q标记物可为中药材的质量控制提供科学依据。

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引用次数: 0

Highly pure measles virus generated by combination of salt-active nuclease treatment and heparin affinity chromatography 结合盐活性核酸酶处理和肝素亲和层析技术生成高纯度麻疹病毒。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-10-22 DOI: 10.1016/j.chroma.2024.465470

Viktoria Mayer , Florian Steiner , Alois Jungbauer , Patricia Pereira Aguilar

Highly purified virus preparations are essential for accurate activity and potency determination. This requires simple and efficient purification methods, especially in the early stages of research and development. While heparin affinity chromatography has been already successfully used for the purification of several enveloped viruses and virus-like particles, we extended its use to purification of very sensitive measles virus. The performance of heparin and heparin-like affinity chromatography was evaluated for the purification of recombinant measles virus, a large and labile enveloped virus used as vaccine or cancer therapy. Since DNA, particularly in the form of chromatin is a critical impurity in enveloped virus preparations, the effect of integration of an endonuclease (Benzonase® or M-SAN) treatment prior to chromatography was also investigated.

Both, Capto™ DeVirS (heparin-like) and Capto™ Heparin were able to capture measles viruses directly from clarified cell culture supernatant. Despite capturing 100 % of infectious measles virus, low recovery (8 %) was observed for Capto™ DeVirS. For Capto™ Heparin recoveries up to 85 % were observed. The combination of M-SAN with Capto™ Heparin enabled the production of highly purified measles virus with a yield of 62 % and a final purity of 10.2 ng dsDNA per dose (1 × 10⁵), outperforming the processes without endonuclease treatment with a yield of 18 %, and a purity of 66.7 ng dsDNA/dose or using Benzonase® with a yield of 38 % and a purity of 21.2 ng dsDNA/dose. As the developed method is simple and scalable it could also be integrated in a downstream process train for measles virus manufacturing.

高度纯化的病毒制剂对于准确测定活性和效力至关重要。这就需要简单高效的纯化方法，尤其是在研发的早期阶段。虽然肝素亲和层析法已成功用于纯化多种包膜病毒和类病毒颗粒，但我们将其应用扩展到了非常敏感的麻疹病毒的纯化。在纯化重组麻疹病毒时，我们对肝素和类肝素亲和层析的性能进行了评估，重组麻疹病毒是一种用于疫苗或癌症治疗的大型易变包膜病毒。由于 DNA（尤其是染色质形式的 DNA）是包膜病毒制剂中的重要杂质，因此还研究了在层析之前加入内切酶（Benzonase® 或 M-SAN）处理的效果。Capto™ DeVirS（类肝素）和 Capto™ Heparin 都能直接从澄清的细胞培养上清液中捕获麻疹病毒。尽管 Capto™ DeVirS 可捕获 100% 的传染性麻疹病毒，但其回收率较低（8%）。而 Capto™ Heparin 的回收率则高达 85%。将 M-SAN 与 Capto™ Heparin 结合使用，可生产出高度纯化的麻疹病毒，每剂量（1 × 105）的产量为 62%，最终纯度为 10.2 ng dsDNA，优于未经内切酶处理的工艺（产量为 18%，纯度为 66.7 ng dsDNA/剂量）或使用 Benzonase® 的工艺（产量为 38%，纯度为 21.2 ng dsDNA/剂量）。由于所开发的方法简单且可扩展，因此也可集成到麻疹病毒生产的下游工艺流程中。

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引用次数: 0

Constructing perfluorinated UiO-67 for enrichment of polycyclic aromatic hydrocarbons in seawater and seabed sediments 构建全氟 UiO-67 以富集海水和海底沉积物中的多环芳烃

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-10-21 DOI: 10.1016/j.chroma.2024.465463

Dongxue Li, Mengjie Qin, Xuejing Lou, Jiawen Zhu, Wende Ma, Ning Zhang, Minghua Lu

To investigate the ocean contamination caused by polycyclic aromatic hydrocarbons (PAHs), UiO-67/perfluorooctanoic acid (UiO-67/PFOA) was synthesized through solvent-assisted ligand incorporation method. The UiO-67/PFOA was then served as an adsorbent in headspace solid-phase microextraction (HS-SPME) technology for collecting and concentrating trace PAHs. The addition of the PFOA improved the hydrophobicity and stability of the UiO-67/PFOA coating, and the C-F functional group in UiO-67/PFOA could form the pseudo hydrogen bonding with the CH on the benzene ring of PAHs, which endowed the UiO-67/PFOA with 1.60–4.63 times enrichment performance for PAHs than UiO-67. Under optimal conditions, the wide linear ranges of PAHs (0.01–20 ng·mL⁻¹) with good coefficients of determination (R² ≥ 0.9950) and low limits of detection (LODs, 0.003–0.008 ng·mL⁻¹) were obtained. The recoveries of five PAHs from spiked seawater and seabed sediment by the developed method ranged from 81.14 % to 116.0 % with satisfactory results. This work provided a good adsorbent for the enrichment of trace PAHs in complicated environments and a new approach for the subsequent synthesis of adsorbents with good enrichment performance.

为研究多环芳烃（PAHs）对海洋的污染，采用溶剂辅助配体掺入法合成了UiO-67/全氟辛酸（UiO-67/PFOA）。然后将 UiO-67/PFOA 作为吸附剂用于顶空固相微萃取（HS-SPME）技术，以收集和富集痕量多环芳烃。PFOA的加入提高了UiO-67/PFOA涂层的疏水性和稳定性，UiO-67/PFOA中的C-F官能团可与多环芳烃苯环上的CH形成假氢键，使UiO-67/PFOA对多环芳烃的富集性能是UiO-67的1.60-4.63倍。在最佳条件下，多环芳烃的线性范围宽（0.01-20 ng-mL-1），测定系数（R2 ≥ 0.9950）和检出限（LODs，0.003-0.008 ng-mL-1）均较低。该方法对加标海水和海底沉积物中5种多环芳烃的回收率为81.14%～116.0%，结果令人满意。该研究为在复杂环境中富集痕量多环芳烃提供了一种良好的吸附剂，也为后续合成具有良好富集性能的吸附剂提供了一种新方法。

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引用次数: 0

Advances and challenges in non-targeted analysis: An insight into sample preparation and detection by liquid chromatography-mass spectrometry 非目标分析的进展与挑战：深入了解样品制备和液相色谱-质谱法检测。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-10-19 DOI: 10.1016/j.chroma.2024.465459

Vivek Mandal , Jinal Ajabiya , Nasir Khan , Rakesh K Tekade, Pinaki Sengupta

Unknown impurities, metabolites and harmful pollutants present in pharmaceutical products, biological and environmental samples, respectively are of high concern in terms of their detection and quantification. The targeted analysis aims to quantify known chemical entities, but it lacks the ability to identify unknown components present in a sample. Non-targeted analysis is an analytical approach that can be made applicable to various disciplines of science to effectively search for unknown chemical, biological, or environmental entities that can answer various baffling mysteries of research. It employs various high-end analytical techniques that can specifically screen out multiple unknown compounds from complex mixtures. Non-targeted analysis is also applicable for complex studies such as metabolomics to search unidentified metabolites of new chemical entities. This review critically discusses the current advancements in non-targeted analysis related to the analysis of pharmaceutical, biological, and environmental samples. Various steps like sample collection, handling, preparation, extraction, its analysis using advanced techniques like high-resolution mass spectrometry, liquid chromatography mass spectrometry, and lastly interpretation of the huge amounts of complex data obtained upon analysis of complex matrices have been discussed broadly in this article. Besides the advantages of non-targeted analysis over targeted analysis, limitations, bioinformatics tools, sources of error, and research gaps have been critically analyzed.

医药产品、生物和环境样品中分别存在的未知杂质、代谢物和有害污染物在检测和定量方面备受关注。靶向分析的目的是量化已知的化学实体，但缺乏识别样品中未知成分的能力。非目标分析是一种适用于各科学学科的分析方法，可以有效地寻找未知的化学、生物或环境实体，从而解答各种令人费解的研究谜题。它采用各种高端分析技术，可以从复杂的混合物中专门筛选出多种未知化合物。非靶向分析也适用于复杂的研究，如代谢组学，以搜索新化学实体的未识别代谢物。本综述深入探讨了与药物、生物和环境样本分析相关的非靶向分析的最新进展。本文广泛讨论了样品收集、处理、制备、提取等各个步骤，以及使用高分辨率质谱法、液相色谱质谱法等先进技术进行分析，最后对分析复杂基质时获得的大量复杂数据进行解读。除了非靶向分析相对于靶向分析的优势之外，还对其局限性、生物信息学工具、错误来源和研究空白进行了批判性分析。

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引用次数: 0

Determination of particle number concentration for biological particles using AF4-MALS: Dependencies on light scattering model and refractive index 使用 AF4-MALS 测定生物颗粒的数量浓度：与光散射模型和折射率有关。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-10-19 DOI: 10.1016/j.chroma.2024.465460

Christine L. Plavchak , Allison Z. Werner , Elizabeth Betz , Davinia Salvachúa , Gregg T. Beckham , S. Kim Ratanathanawongs Williams

Determining accurate counts and size distributions for biological particles (bioparticles) is crucial in wide-ranging fields, but current methods to this end are susceptible to bias from polydispersity in size. This bias can be mitigated by incorporating a separation step prior to characterization. For this reason, asymmetrical flow field-flow fractionation (AF4) with on-line multiangle light scattering (MALS) has become an important platform for determining particle size. AF4-MALS has also been increasingly used to report particle concentration, particularly for complex biological particles, yet the impact of light scattering models and particle refractive indices (RI) have not been quantitatively evaluated. Here, we develop an analysis workflow using AF4-MALS to simultaneously separate and determine particles sizes and concentrations. The impacts of the MALS particle counting model used to process data and the chosen RI value(s) on particle counts are systematically assessed for polystyrene latex (PSL) particles and bacterial outer membrane vesicles (OMVs) in the 20–500 nm size range. Across spherical models, PSL and OMV particle counts varied up to 13 % or 200 %, respectively. For the coated-sphere model used in the analysis of OMV samples, the sphere RI value greatly impacts particle counts. As the sphere RI value approaches the RI of the suspending medium, the model becomes increasingly sensitive to the light scattering signal-to-noise ratio ultimately causing erroneous particle counts. Overall, this work establishes the importance of selecting appropriate MALS models and RI values for bioparticles to obtain accurate counts and provides an AF4-MALS method to separate, enumerate, and size polydisperse bioparticles.

确定生物颗粒（生物微粒）的精确计数和粒度分布在多个领域都至关重要，但目前的方法容易受到粒度多分散性的影响。在表征之前加入分离步骤可以减轻这种偏差。因此，带有在线多角度光散射（MALS）的非对称流场-流动分馏（AF4）已成为确定粒度的重要平台。AF4-MALS 也越来越多地用于报告颗粒浓度，尤其是复杂生物颗粒的浓度，但光散射模型和颗粒折射率 (RI) 的影响尚未得到定量评估。在此，我们开发了一种使用 AF4-MALS 的分析工作流程，可同时分离并确定颗粒大小和浓度。我们系统地评估了用于处理数据的 MALS 粒子计数模型和所选 RI 值对 20-500 nm 尺寸范围内聚苯乙烯胶乳 (PSL) 粒子和细菌外膜囊泡 (OMV) 粒子计数的影响。在各种球形模型中，PSL 和 OMV 粒子数的变化分别高达 13 % 和 200 %。对于用于分析 OMV 样品的涂层球模型，球形 RI 值对颗粒计数有很大影响。当球形 RI 值接近悬浮介质的 RI 时，模型对光散射信噪比越来越敏感，最终导致错误的颗粒计数。总之，这项工作证明了为生物颗粒选择适当的 MALS 模型和 RI 值对获得精确计数的重要性，并提供了一种 AF4-MALS 方法来分离、列举和测定多分散生物颗粒的大小。

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引用次数: 0

Pore structure reconstruction to reveal the adsorption capacity limitation of current oligo-dT resins and guide new resin design 重建孔隙结构，揭示当前寡聚-dT 树脂的吸附能力限制，指导新树脂的设计

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-10-18 DOI: 10.1016/j.chroma.2024.465454

Liang-Zhi Qiao, Yuan-Zhi Tan, Shan-Jing Yao, Dong-Qiang Lin

In-depth knowledge of the pore structure of chromatographic resins is instrumental for better mechanistic understanding of adsorption performance, which can be translated into strategies to guide the design of new resins. Aiming to reveal the underlying reasons of low mRNA adsorption capacities of commercial oligo-dT resins, three-dimensional (3D) pore structure reconstruction was applied to relate key pore properties to the adsorption performance. The static 3D pore analysis revealed that the amount and connectivity of the accessible pores for 100 nm-sized mRNA reduced by over 90% and 46% compared with initial pore structure of resins, respectively, which led to discontinuous transport paths for mRNA. The dynamic simulations revealed that the strong hindrance of the firstly bound mRNA to the following mRNA molecules led to less than 10% of mRNA being able to penetrate into the resins with a depth of only 1–2 μm. Based on the digital material model, a virtual nanofiber-based macroporous resin was designed to explore its potential. Simulation results demonstrated that due to large pores and high connectivity, the new resin could allow over 91% of mRNA diffusion into the resin interior, showing great potential to improve the adsorption capacity of mRNA. This work provided a new method to evaluate the limitations of commercial oligo-dT resins and obtained some valuable guidance for the structure design of next-generation resins.

深入了解色谱树脂的孔结构有助于更好地从机理上理解其吸附性能，并将其转化为指导新树脂设计的策略。为了揭示商用寡聚-dT 树脂 mRNA 吸附能力低的根本原因，研究人员应用三维（3D）孔结构重构技术将关键孔性质与吸附性能联系起来。静态三维孔隙分析表明，与树脂的初始孔隙结构相比，100 nm 大小的 mRNA 可进入孔隙的数量和连通性分别减少了 90% 和 46% 以上，这导致 mRNA 的传输路径不连续。动态模拟结果表明，首次结合的 mRNA 对后续 mRNA 分子的强烈阻碍作用导致只有不到 10% 的 mRNA 能够穿透树脂，深度仅为 1-2 μm。在数字材料模型的基础上，设计了一种基于纳米纤维的虚拟大孔树脂，以探索其潜力。模拟结果表明，由于大孔和高连通性，新型树脂可使91%以上的mRNA扩散到树脂内部，在提高mRNA吸附能力方面显示出巨大潜力。这项工作为评估商用寡聚-dT 树脂的局限性提供了一种新方法，并为下一代树脂的结构设计提供了一些有价值的指导。

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引用次数: 0

On the fractionation of lignin oligomers by stepwise gradient reversed-phase liquid chromatography 用逐步梯度反相液相色谱法分馏木质素低聚物

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-10-18 DOI: 10.1016/j.chroma.2024.465458

Daniel Papp, Margareta Sandahl

With the increased interest in lignin valorization, the analytical challenge to separate a complex mixture of a vast number of phenolics has made chromatography an indispensable step in lignin analysis. High-resolution separations, such as gas chromatography, reversed-phase liquid chromatography and supercritical fluid chromatography have typically been targeting low-molecular-weight compounds, while larger lignin oligomers have received less attention. These compounds have proven to be difficult to separate due to the inherent complexity of the high-molecular-weight fraction of lignins, in fact, even high-resolving linear reversed-phase gradients elute them as one wide zone. To tackle this, in this study we show that a crude fractionation of lignin oligomers can be achieved by applying stepwise reversed-phase gradients. A commonly employed reversed-phase system with water:acetonitrile mobile phase is evaluated for this task. Special attention was devoted to uncovering the molecular level explanation of the retention phenomenon. Our results indicate that separation is mainly governed by reversed-phase retention phenomena without any major exclusion or viscosity-related effects, shown by great fits to linear retention models (R²_avg = 0.9599 for five different oligomers) and apparent differences in retentivity between different stationary phases. The influence of the gradient shape was demonstrated by the comparison of stepwise gradients with different number and frequency of steps, leading to the conclusion that gradients with a low number of steps yield fewer, but better resolved fractions, while finer multi-step gradients can be used to distinguish more fractions.

随着人们对木质素价值化的兴趣与日俱增，分离由大量酚类化合物组成的复杂混合物所带来的分析挑战使色谱法成为木质素分析中不可或缺的步骤。气相色谱法、反相液相色谱法和超临界流体色谱法等高分辨率分离法通常以低分子量化合物为目标，而较大的木质素低聚物则较少受到关注。由于木质素高分子量部分的固有复杂性，这些化合物已被证明难以分离，事实上，即使是高分辨线性反相梯度也会将它们洗脱为一个宽阔的区域。为了解决这个问题，我们在本研究中展示了通过使用阶跃反相梯度可以实现木质素低聚物的粗分馏。为完成这一任务，我们对常用的以水：乙腈为流动相的反相系统进行了评估。我们特别注意从分子水平上解释保留现象。我们的结果表明，分离主要受反相保留现象的支配，没有任何主要的排斥或粘度相关影响，这表现在线性保留模型的高度拟合（5 种不同低聚物的 R2avg = 0.9599）以及不同固定相之间保留率的明显差异。通过比较不同步数和频率的阶梯梯度，证明了梯度形状的影响，从而得出结论：低步数梯度产生的馏分较少，但分辨效果更好，而更精细的多步梯度可用于分辨更多馏分。

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引用次数: 0

Evaluating the detection of barbiturates in dried blood spots: A comparative analysis using gas chromatography-mass spectrometry, gas chromatography-tandem mass spectrometry, and liquid chromatography-tandem mass spectrometry with different extraction methods 评估干血斑中巴比妥酸盐的检测：使用气相色谱-质谱法、气相色谱-串联质谱法和液相色谱-串联质谱法与不同提取方法进行比较分析。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-10-18 DOI: 10.1016/j.chroma.2024.465434

Yujie Zhi , Jiayue Lu , Qiongying Zheng , Xinyu Cao , Min Lv , Qing Xu , Ping Xiang , Wei Liu , Bin Di , Xianyu Fan , Hang Chen

Rapid and accurate characterization and quantitation of blood barbiturates and their combination drugs are very important for the clinical treatment of acute barbiturate poisoning. A comparison of dried blood spot (DBS) and traditional liquid-liquid extraction (LLE) in the pre-treatment stage, as well as a comparison of gas chromatography-mass spectrometry (GC–MS), gas chromatography-tandem mass spectrometry (GC–MS/MS), and liquid chromatography-tandem mass spectrometry (LC-MS/MS) as instrumental analysis methods, revealed differences in the analysis results of barbiturates and their combination drugs under different conditions. Based on these findings, we introduce a DBS-GC–MS/MS method. The developed and validated method showed good selectivity, sensitivity (LOD: 0.1 μg mL⁻¹, LOQ: 0.2 μg mL⁻¹), linearity (R²>0.9992), trueness (<15 %, except for carbamazepine, at 29.4 %), and precision (<15 %). Recovery was also good for most target compounds, but significant matrix effects were evident. Compared with the LLE method, the DBS method has the benefits of easy sample collection, storage, and transport, as well as simple pre-treatment and reduced reagent and energy consumption. Compared to LC-MS/MS, GC–MS/MS requires no switching between positive and negative ion modes and uses the MRM detection mode, meaning that more information about the sample compounds can be obtained in less analysis time. Using actual sample analysis, we have demonstrated the advantages of the DBS-GC–MS/MS method for the qualitative and quantitative analysis of barbiturates and poisoning events due to combinations of these drugs. Comparison of the three instruments and the two treatment methods revealed their analysis characteristics. From the perspective of practical application, the broad practical value and advantages of DBS should be embraced in more applications, and future analytical laboratory development should continue to recognize GC–MS/MS as a useful supplement to LC-MS/MS.

快速准确地定性和定量血液中的巴比妥酸盐及其复方药物对急性巴比妥酸盐中毒的临床治疗非常重要。通过比较前处理阶段的干血斑（DBS）和传统的液液萃取（LLE），以及气相色谱-质谱（GC-MS）、气相色谱-串联质谱（GC-MS/MS）和液相色谱-串联质谱（LC-MS/MS）等仪器分析方法，发现巴比妥类药物及其复方药物在不同条件下的分析结果存在差异。基于这些发现，我们介绍了一种 DBS-GC-MS/MS 方法。所建立和验证的方法具有良好的选择性、灵敏度（LOD：0.1 μg mL-1, LOQ：0.2 μg mL-1）、线性度（R2>0.9992）、确证度（R2>0.9992）和定量限（R2>0.9992）。

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