Analytica Chimica Acta最新文献

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Cytokine profiling in COVID-19 patients by using ion mobility-mass spectrometry-based parallel reaction monitoring 基于离子迁移-质谱平行反应监测的COVID-19患者细胞因子谱分析
IF 5.7 2区 化学
Analytica Chimica Acta Pub Date : 2025-05-20 DOI: 10.1016/j.aca.2025.344227
Ling Yan , Chenrui Yuan , Runhou Zhou , Li Zhong , Kelvin Kai-Wang To , Na Liu , Xin Diao , Guangshan Xie , Hongzhi Zhao , Haijiang Wu , Lin Zhu , Zhiwei Chen , Zongwei Cai
{"title":"Cytokine profiling in COVID-19 patients by using ion mobility-mass spectrometry-based parallel reaction monitoring","authors":"Ling Yan ,&nbsp;Chenrui Yuan ,&nbsp;Runhou Zhou ,&nbsp;Li Zhong ,&nbsp;Kelvin Kai-Wang To ,&nbsp;Na Liu ,&nbsp;Xin Diao ,&nbsp;Guangshan Xie ,&nbsp;Hongzhi Zhao ,&nbsp;Haijiang Wu ,&nbsp;Lin Zhu ,&nbsp;Zhiwei Chen ,&nbsp;Zongwei Cai","doi":"10.1016/j.aca.2025.344227","DOIUrl":"10.1016/j.aca.2025.344227","url":null,"abstract":"<div><div>Cytokine therapy, a non-antigen-specific strategy, has led to several FDA-approved drugs. Given the role of dysregulated cytokine expression in diseases such as COVID-19, accurate quantification is critical in both clinical and research settings. While antibody-based assays offer high sensitivity, their reliance on specific antibodies limits multiplexing and increases analytical complexity. Conversely, mass spectrometry methods like multiplexed reaction monitoring provide higher throughput but lack the sensitivity to detect physiological cytokine levels and the resolution to distinguish structural isomers. Thus, a new MS-based approach is needed that integrates high sensitivity with the ability to resolve structurally similar cytokines. We developed an ion mobility-mass spectrometry (IM-MS)-based parallel reaction monitoring (PRM) method to establish the first Cytokine Ion Mobility Peptide (CIMP) databank and enable high-throughput cytokine profiling in serum samples from COVID-19 patients. By introducing ion mobility as an additional gas-phase separation dimension alongside liquid chromatography, the method enhances analyte resolution based on structural differences, facilitating the separation of isomers within the ion mobility trap. The incorporation of ion mobility as a complementary separation parameter enables the distinction of homologous cytokines and structural isomers (e.g., IFNA1/IFNA2, IFNL1/IFNL3, and peptide isomers), which remains challenging for conventional antibody-based assays. The method achieved a limit of detection of 62.9 fmol/L and a limit of quantification of 210 fmol/L across 31 cytokines, demonstrating greater sensitivity than traditional multiple reaction monitoring (MRM) approaches and enabling quantification at physiological concentration levels, assuming comparable background signal across platforms. The IM-MS-PRM method offers a multiplexed, high-throughput, and adaptable platform that eliminates the need for multiple assays while delivering excellent reproducibility. It enables accurate and sensitive cytokine quantification from minimal volumes of COVID-19 patient serum. Combined with the CIMP databank, this approach allows precise differentiation between early and late severe COVID-19 cases, supporting improved diagnostic and therapeutic decision-making.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344227"},"PeriodicalIF":5.7,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144104253","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Low-background and label-free loop-mediated isothermal amplification for rapid detection of foodborne pathogens using amplicon-templated copper nanoclusters 利用扩增子模板铜纳米团簇快速检测食源性病原体的低背景和无标记环介导等温扩增
IF 5.7 2区 化学
Analytica Chimica Acta Pub Date : 2025-05-20 DOI: 10.1016/j.aca.2025.344222
Wenyu Du , Shuanglong Wang , Yining Luo , Xiaoyu Tong , Yin Chen , Zhipeng Fang , Junzhuo Shan , Daofeng Liu , Haiyan Ni , Weihua Lai , Shan Shan
{"title":"Low-background and label-free loop-mediated isothermal amplification for rapid detection of foodborne pathogens using amplicon-templated copper nanoclusters","authors":"Wenyu Du ,&nbsp;Shuanglong Wang ,&nbsp;Yining Luo ,&nbsp;Xiaoyu Tong ,&nbsp;Yin Chen ,&nbsp;Zhipeng Fang ,&nbsp;Junzhuo Shan ,&nbsp;Daofeng Liu ,&nbsp;Haiyan Ni ,&nbsp;Weihua Lai ,&nbsp;Shan Shan","doi":"10.1016/j.aca.2025.344222","DOIUrl":"10.1016/j.aca.2025.344222","url":null,"abstract":"<div><h3>Background</h3><div>Loop-mediated isothermal amplification (LAMP) is a simple, low-cost, and instrument-free assay, which is highly adaptable for the detection of foodborne pathogens. However, current methods have a high background, making it difficult to achieve sensitive on-site detection.</div></div><div><h3>Results</h3><div>Herein, LAMP-CuNCs assay with a low background signal was established. LAMP amplicons were used as the templates for the synthesis of copper nanoclusters (CuNCs), and LAMP results were determined by the fluorescence intensity of the amplicons-CuNCs. The stability of LAMP amplicons templated CuNCs was improved by the addition of 1.5 g/mL fructose, which effectively prolonged the fluorescence lifetime. The detection limit of <em>Salmonella</em> DNA was 756 pg/μL, and the sensitivity and specificity of this method were 12/12 and 12/12, respectively. This method could detect <em>Salmonella</em> at a minimum concentration of 1910 CFU/mL in spiked salmon samples.</div></div><div><h3>Significance</h3><div>The study provided a method that can quickly obtain results within 16 min for detection of genomic DNA and visual inspection under a 365 nm UV flashlight. In addition, this method could also be used to detect <em>Listeria monocytogenes</em>, <em>Vibrio parahaemolyticus</em>, and <em>Escherichia coli</em>.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344222"},"PeriodicalIF":5.7,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144097265","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A fully automated, high-throughput electro-extraction and analysis workflow for acylcarnitines in human plasma and mouse muscle tissues 人血浆和小鼠肌肉组织中酰基肉碱的全自动、高通量电萃取和分析工作流程
IF 5.7 2区 化学
Analytica Chimica Acta Pub Date : 2025-05-20 DOI: 10.1016/j.aca.2025.344224
Yupeng He , Paul Miggiels , Amy Harms , Yvonne Rijksen , Renata M.C. Brandt , Wilbert P. Vermeij , Bert Wouters , Thomas Hankemeier
{"title":"A fully automated, high-throughput electro-extraction and analysis workflow for acylcarnitines in human plasma and mouse muscle tissues","authors":"Yupeng He ,&nbsp;Paul Miggiels ,&nbsp;Amy Harms ,&nbsp;Yvonne Rijksen ,&nbsp;Renata M.C. Brandt ,&nbsp;Wilbert P. Vermeij ,&nbsp;Bert Wouters ,&nbsp;Thomas Hankemeier","doi":"10.1016/j.aca.2025.344224","DOIUrl":"10.1016/j.aca.2025.344224","url":null,"abstract":"<div><h3>Background</h3><div>The labor-intensive and time-consuming nature of sample preparation poses significant challenges for bioanalysis, especially for large-scale samples characterized by limited volumes/mass, and low analyte abundance. Additionally, manual sample processing can compromise reproducibility. To overcome these limitations, automation and high-throughput methodologies are essential, highlighting the need for an automated, high-throughput sample preparation and analysis workflow.</div></div><div><h3>Results</h3><div>This study presents a fully automated, high-throughput electro-extraction (EE) platform integrated with a CTC PAL3 autosampler and liquid chromatography–mass spectrometry analyzer. The integrated platform underwent qualification, followed by optimization of EE parameters using a Design of Experiment approach. Ten acylcarnitines were selected as model analytes. The optimization models exhibited strong fits (p &lt; 0.006, R<sup>2</sup> &gt; 0.91). The optimized platform achieved an enrichment factor of up to 400 (an extraction recovery of up to 99 %) in designed academic samples, and was effectively implemented and evaluated using 20 μL of spiked human plasma samples. To test clinically relevant materials, the platform was utilized to study the effects of muscle tissue isolation speed on acylcarnitine stability, and to examine acylcarnitine abundance across muscle types in progeria (sarcopenia) mouse muscle. We found that the speed of muscle isolation does not affect measured levels of acylcarnitines, and detected higher acylcarnitine abundances are consistent with literature.</div></div><div><h3>Significance</h3><div>This study provides an automated, high-throughput, and cost-effective workflow enabling extraction and analysis of 120 samples per day, with a cost of &lt;0.1 Euro per sample. It presents a significant stride towards the creation of fully-automated, high-throughput bioanalysis workflows for large-scale studies involving biomass limited samples in the foreseeable future.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344224"},"PeriodicalIF":5.7,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144097266","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Analytical quality control in targeted lipidomics: Evaluating the performance of commercial plasma as a surrogate for pooled study samples 靶向脂质组学的分析质量控制:评估商业血浆作为合并研究样本的替代品的性能
IF 5.7 2区 化学
Analytica Chimica Acta Pub Date : 2025-05-20 DOI: 10.1016/j.aca.2025.344225
Alanah Grant-St James , Aude-Claire Lee , Alex J. Lee , Julien Wist , Ferdous Sohel , Kok Wai Wong , Bu B. Yeap , Ruey Leng Loo , Amanda Henry , Daniella Susic , Emad El-Omar , Jeremy K. Nicholson , Elaine Holmes , Luke Whiley , Nicola Gray
{"title":"Analytical quality control in targeted lipidomics: Evaluating the performance of commercial plasma as a surrogate for pooled study samples","authors":"Alanah Grant-St James ,&nbsp;Aude-Claire Lee ,&nbsp;Alex J. Lee ,&nbsp;Julien Wist ,&nbsp;Ferdous Sohel ,&nbsp;Kok Wai Wong ,&nbsp;Bu B. Yeap ,&nbsp;Ruey Leng Loo ,&nbsp;Amanda Henry ,&nbsp;Daniella Susic ,&nbsp;Emad El-Omar ,&nbsp;Jeremy K. Nicholson ,&nbsp;Elaine Holmes ,&nbsp;Luke Whiley ,&nbsp;Nicola Gray","doi":"10.1016/j.aca.2025.344225","DOIUrl":"10.1016/j.aca.2025.344225","url":null,"abstract":"<div><h3>Background</h3><div>Pooled quality control (PQC) samples are the gold standard for data quality monitoring in metabolic phenotyping studies. Typically composed of equal parts from all study samples, PQCs can be challenging to generate in large cohorts or when sample volumes are low. As an alternative, externally sourced matrix-matched surrogate QCs (sQC) have been proposed. This study evaluates the performance of sQCs against PQCs for assessing analytical variation, data pre-processing, and downstream data analysis in a targeted lipidomics workflow.</div></div><div><h3>Results</h3><div>Plasma samples (n = 701) from the Microbiome Understanding in Maternity Study, along with PQC (n = 80) and sQC (n = 80) samples, were analyzed using a lipidomics assay targeting 1162 lipids. QC samples were injected throughout acquisition, and data pre-processing was performed using each strategy. For simplicity, a subset (n = 381) of the study samples was used to assess differences in downstream statistical analyses.</div><div>Both QC approaches demonstrated high analytical repeatability. While PQC and sQC compositions differed, use of PQCs retained less than 4 % more lipid species during pre-processing. Univariate analysis identified more statistically significant lipids with PQC-based pre-processing, but multivariate model performance was similar between datasets.</div></div><div><h3>Significance</h3><div>This study provides a comprehensive comparison of QC strategies and emphasizes the importance of careful QC workflow selection. While PQCs offer advantages, sQCs serve as a suitable alternative for quality assessment and pre-processing. Their commercial availability also supports use as intra- and inter-laboratory long-term references, aiding data harmonization across studies and laboratories.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1365 ","pages":"Article 344225"},"PeriodicalIF":5.7,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144104252","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Utilizing the total phosphorus content of lipid extracts as a normalization strategy in quantitative lipidomics studies 利用脂质提取物的总磷含量作为定量脂质组学研究的规范化策略
IF 5.7 2区 化学
Analytica Chimica Acta Pub Date : 2025-05-20 DOI: 10.1016/j.aca.2025.344228
Johannes Scholz , Anna Gremme , Julia Hillebrand , Jasper Baldauf , Lennart J. Bendheuer , Jonas Berreiter , Anne C. Sehnal , Julia Bornhorst , Heiko Hayen
{"title":"Utilizing the total phosphorus content of lipid extracts as a normalization strategy in quantitative lipidomics studies","authors":"Johannes Scholz ,&nbsp;Anna Gremme ,&nbsp;Julia Hillebrand ,&nbsp;Jasper Baldauf ,&nbsp;Lennart J. Bendheuer ,&nbsp;Jonas Berreiter ,&nbsp;Anne C. Sehnal ,&nbsp;Julia Bornhorst ,&nbsp;Heiko Hayen","doi":"10.1016/j.aca.2025.344228","DOIUrl":"10.1016/j.aca.2025.344228","url":null,"abstract":"<div><h3>Background</h3><div>Normalization is a crucial element of quantitative lipidomics studies, for which there is still no uniform recommended strategy. There are various approaches for normalizing samples, including referencing to the total volume or weight, to the DNA content or the protein content. In addition, samples can be normalized to the phosphorus content, but either not all phospholipid classes are included or a less sensitive colorimetric assay is used. <strong>It is therefore necessary to develop new ways of normalization that are both specific and sensitive to compensate for the biological sample variance and the variance from pre-analytical and analytical steps.</strong></div></div><div><h3>Results</h3><div>We present a tailored normalization method for lipid quantification which is based on the total phosphorus content (TPC) of lipid extracts. The TPC reflects the amount of phospholipids present in the sample, because polar phosphorus-containing compounds like DNA and phosphorylated sugars are separated due to the extraction procedure. In order to test the normalization strategy, the (phospho)-lipids in the model organism <em>C. elegans</em> were quantified using SFC-TIMS-MS/MS. Subsequently, a digestion method was developed to degrade the lipids present in the organic extract. This was used to determine the TPC via ICP-OES and ICP-MS/MS analysis. In particular, very low detection limits (LOQ = 0.3 μg L<sup>−1</sup>) can be achieved with the ICP-MS/MS method. The elemental and molecular information were then combined, and the samples were normalized to TPC. The normalization showed a significant improvement in the standard deviations compared to the initial concentrations as well as an improvement compared to the normalization based on the total protein content, which is very frequently used.</div></div><div><h3>Significance</h3><div>Our method shows a sensitive way to determine the TPC in total lipid extracts of various samples, exemplified for human plasma and nematode samples. The normalization minimizes the standard deviations in biological samples even in comparison with other normalization approaches, i.e. protein content, and can contribute to increasing the conclusiveness of quantitative lipidomics studies.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344228"},"PeriodicalIF":5.7,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144097269","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Controllable synthesis of chiral hierarchical porous Co(OH)2 and its application in rapid chiral recognition and separation 手性层叠多孔Co(OH)2的可控合成及其在快速手性识别与分离中的应用
IF 5.7 2区 化学
Analytica Chimica Acta Pub Date : 2025-05-20 DOI: 10.1016/j.aca.2025.344212
Jinhua Xu , Jinyu Zhang , Wenmin Zhang , Shiye Xie , Lan Zhang
{"title":"Controllable synthesis of chiral hierarchical porous Co(OH)2 and its application in rapid chiral recognition and separation","authors":"Jinhua Xu ,&nbsp;Jinyu Zhang ,&nbsp;Wenmin Zhang ,&nbsp;Shiye Xie ,&nbsp;Lan Zhang","doi":"10.1016/j.aca.2025.344212","DOIUrl":"10.1016/j.aca.2025.344212","url":null,"abstract":"<div><h3>Background</h3><div>Chiral pollutants present significant environmental and health concerns, with neurotoxic amino acid analogs like β-N-methylamino-L-alanine (BMAA) demonstrating enantiomer-specific bioaccumulation in aquatic ecosystems. Current analytical approaches for chiral environmental contaminants rely predominantly on chromatographic techniques that require extensive sample preparation (typically 24 h), limiting field deployment and high-throughput screening capabilities. Detection thresholds for these compounds (0.1–10 μg/L) necessitate sensitive methodologies that maintain stereochemical integrity. This study addresses these analytical challenges through the rational design of chiral cobalt hydroxide (CF–Co(OH)<sub>2</sub>) nanomaterials engineered for dual-mode detection and separation functionality.</div></div><div><h3>Results</h3><div>A hierarchical porous α-Co(OH)<sub>2</sub> with tunable chirality (R/S/RS configurations) and morphologies (square, rough surface, snowflake, flower-like) via micelle-templated growth strategies. The materials demonstrated dual functionality: (1) Rapid colorimetric amino acid discrimination within 5 min with precision (RSD = 4.9 %, n = 6), validated through urinary <span>l</span>-tryptophan quantification (17.1 ± 0.4 μg/mL); (2) Ultrasensitive BMAA separation via SPE-HPLC-MS/MS with significantly improved detection limits (LOD = 0.02 μg/kg) and processing speed (144 × faster than conventional methods). The colorimetric detection mechanism exploits BMAA's ability to form cobalt-amine complexes that produce concentration-dependent yellow coloration, enabling visual detection at 50 μg/kg in freshwater samples. Field testing successfully detected BMAA in crucian carp (0.39 ± 0.03 μg/kg), confirming food-chain biomagnification with excellent recovery (90.1–102.7 %) across diverse matrices. The system's chiral specificity exhibited distinct affinity patterns (BMAA: R–Co(OH)<sub>2</sub>; DAB: S–Co(OH)<sub>2</sub>) with 91.4 % enantiomeric excess in just 10 min through configuration-specific “three-point binding” mechanisms (intramolecular binding energy: 18.7 kcal/mol).</div></div><div><h3>Significance</h3><div>This research establishes morphology-programmable chiral materials as a versatile analytical platform for rapid on-site environmental monitoring and high-throughput toxin analysis. The developed methodology directly addresses World Health Organization guidelines for algal toxin detection in drinking water while providing a generalizable approach for chiral pollutant discrimination in complex environmental and biological samples.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344212"},"PeriodicalIF":5.7,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144097270","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A versatile two-dimensional liquid chromatography coupled to high-resolution mass spectrometry platform for unraveling chromatographic profiles of large synthetic oligonucleotides 一种多功能二维液相色谱耦合高分辨率质谱平台,用于解开大型合成寡核苷酸的色谱图谱
IF 5.7 2区 化学
Analytica Chimica Acta Pub Date : 2025-05-20 DOI: 10.1016/j.aca.2025.344218
Bifan Chen, Bingchuan Wei, Lulu Dai, Jenny Wang, Dawen Kou, Kelly Zhang
{"title":"A versatile two-dimensional liquid chromatography coupled to high-resolution mass spectrometry platform for unraveling chromatographic profiles of large synthetic oligonucleotides","authors":"Bifan Chen,&nbsp;Bingchuan Wei,&nbsp;Lulu Dai,&nbsp;Jenny Wang,&nbsp;Dawen Kou,&nbsp;Kelly Zhang","doi":"10.1016/j.aca.2025.344218","DOIUrl":"10.1016/j.aca.2025.344218","url":null,"abstract":"<div><h3>Background</h3><div>Many gene expression-modulating therapeutics, as well as clustered regularly interspaced short palindromic repeats (CRISPR)-Cas9 gene editing technology have greatly transformed the field of biomedical research. A number of trials already in clinic well exemplify the potential of oligonucleotide-based therapeutics to address many disease areas. The quality and the integrity of the oligonucleotides are therefore crucial to ensure efficacy and ultimately patient safety, which often require thorough characterization. In general, these oligonucleotides are synthetically made by solid phase phosphoramidite chemistry, during which many possible undesired byproducts from incomplete or side reactions can be generated. However, the examination of the overall chromatographic profile on the large synthetic oligonucleotides from the intact level has been limited and challenging by direct coupling to mass spectrometry (MS). This is due not only to the low abundance and heterogeneity of impurities, but also to difficulties in separation. Furthermore, many oligonucleotide separation methods coupled online to MS greatly suffer from suboptimal sensitivity of the MS detection.</div></div><div><h3>Results</h3><div>Here, to address these challenges, we develop a versatile two-dimensional liquid chromatography-mass spectrometry (2DLC-MS) platform involving multiple heart-cut fractionation, adduct removal, and acquisition through wide window quadrupole isolation. Using a 100-mer long single guide ribonucleic acid (sgRNA) as the model compound, we showcased the in-depth analysis of the sgRNA IP-RPLC profile as well as HILIC profile at lower temperature.</div></div><div><h3>Significance</h3><div>Overall, by utilizing the 2DLC-MS platform, we were able to gain a major sensitivity boost to examine the chromatographic profiles of large synthetic oligonucleotides, enabling lot to lot comparison and understanding of impurity profiles.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344218"},"PeriodicalIF":5.7,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144104251","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A homogeneous mass-encoded strategy for mass spectrometric biosensing of multiplex proteins 多重蛋白质质谱生物传感的均匀质量编码策略
IF 5.7 2区 化学
Analytica Chimica Acta Pub Date : 2025-05-19 DOI: 10.1016/j.aca.2025.344219
Junjie Hu , Fei Liu , Yunlong Chen , Xinxin Xie , Huangxian Ju
{"title":"A homogeneous mass-encoded strategy for mass spectrometric biosensing of multiplex proteins","authors":"Junjie Hu ,&nbsp;Fei Liu ,&nbsp;Yunlong Chen ,&nbsp;Xinxin Xie ,&nbsp;Huangxian Ju","doi":"10.1016/j.aca.2025.344219","DOIUrl":"10.1016/j.aca.2025.344219","url":null,"abstract":"<div><h3>Background</h3><div>Protein kinases play important roles in fundamental biological processes. Aberrant activities may result in many diseases, thus the detection of multiplex kinase activities is important in clinical diagnosis. Recent progress has focused on the mass spectrometric biosensing technique to enable highly sensitive detection of multiplex targets. However, the application of the developed methods in multiplex enzyme analysis is greatly challenged due to the substrate immobilization on solid interfaces, which affect the contact between substrates and enzymes to reduce enzyme reaction efficiency.</div></div><div><h3>Results</h3><div>This work developed a homogeneous mass-encoded method for biosensing of multiplex proteins, which was performed using designed peptides containing the coding sequences and substrate regions. With the assistance of titanium dioxide coated magnetic beads (TiO<sub>2</sub>-MBs) to capture the phosphopeptide products, followed by trypsin to cleave the products for releasing the coding sequences, the kinase assays were achieved by submitting the supernatant for ultrahigh performance liquid chromatography-tandem mass spectrometric (UHPLC-MS/MS) analysis. Using protein kinase A (PKA) and human epidermal growth factor receptor 2 (HER2) as model targets, the peak area ratios of the coding sequences to the internal standards showed linear relations of 1.0–100 ng mL<sup>−1</sup> and 0.2–20 U mL<sup>−1</sup>, with the detection limits of 0.46 ng mL<sup>−1</sup> and 0.033 U mL<sup>−1</sup> for HER2 and PKA, respectively. The proposed strategy also demonstrated great practicability in inhibition analysis and kinase activity assays in cell lysates.</div></div><div><h3>Significance</h3><div>A homogeneous mass-encoded method for multiplex detection of kinase activities could simplify the assay procedure and reveal the enzyme activities with free substrates. The strategy enabled multiplex kinase activity assays with convenience, high sensitivity, and high specificity, demonstrating promising applications in clinical fields.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344219"},"PeriodicalIF":5.7,"publicationDate":"2025-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144097271","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Method development and validation for analysis of 74 per- and polyfluoroalkyl substances (PFAS) in food of animal origin using QuEChERSER method and LC-MS/MS 采用QuEChERSER法和LC-MS/MS法分析动物源性食品中74种全氟烷基和多氟烷基物质(PFAS)的方法开发和验证
IF 5.7 2区 化学
Analytica Chimica Acta Pub Date : 2025-05-19 DOI: 10.1016/j.aca.2025.344216
Kevin M. Stroski, Yelena Sapozhnikova
{"title":"Method development and validation for analysis of 74 per- and polyfluoroalkyl substances (PFAS) in food of animal origin using QuEChERSER method and LC-MS/MS","authors":"Kevin M. Stroski,&nbsp;Yelena Sapozhnikova","doi":"10.1016/j.aca.2025.344216","DOIUrl":"10.1016/j.aca.2025.344216","url":null,"abstract":"<div><h3>Background</h3><div>The detection of per- and polyfluoroalkyl substances (PFAS) in food is extremely important for ensuring safe food consumption however most analytical methods focus on only a small group of known analytes. <strong>The goal of this study was to develop and validate a new method for analysis of 74 PFAS ranging across 15 different groups including legacy PFAS, short-chain alternatives, precursors and breakdown products in beef, chicken, pork, catfish and eggs.</strong></div></div><div><h3>Results</h3><div>The method was based on “quick, easy, cheap, effective, rugged, safe, efficient, and robust” (QuEChERSER) mega-method and LC-MS/MS analysis. Validation was performed at, above and below maximum levels set by the European Food Safety Authority (EFSA) in beef, chicken, pork, catfish, liquid egg, and powdered egg samples. Acceptable recoveries were obtained for 72 %–93 % of analytes using reagent only calibration curves across all matrices and concentrations tested. This increased to 84 %–97 % when using matrix matched calibration curves. Method performance was comparable (or better than) US Food and Drug Administration (FDA) and USDA Food Safety and Inspection Service (FSIS) methods. Further validation of the method with NIST standard reference materials (SRMs) 1946 and 1947 resulted in accuracies of 71 %–112 %. The validated method was applied to test catfish samples, and low levels of PFAS (0.020–2.24 ng/g wet weight) were measured in both farm raised and wild caught fish.</div></div><div><h3>Significance</h3><div>These results demonstrate the ability of this method to accurately measure a broad range of PFAS analytes in complex food matrices providing broad applicability and versatility to end users. To our knowledge, this is the largest current targeted method for analysis of PFAS in foods.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344216"},"PeriodicalIF":5.7,"publicationDate":"2025-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144097272","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Gold nanoparticle-assisted, label-free SELEX coupled with high-throughput NGS for generating highly sensitive and specific DNA aptamers targeting Aflatoxin B1 金纳米颗粒辅助,无标签SELEX结合高通量NGS生成高敏感和特异性的DNA适体靶向黄曲霉毒素B1
IF 5.7 2区 化学
Analytica Chimica Acta Pub Date : 2025-05-17 DOI: 10.1016/j.aca.2025.344201
Shazia Shareef, Hariprasad P.
{"title":"Gold nanoparticle-assisted, label-free SELEX coupled with high-throughput NGS for generating highly sensitive and specific DNA aptamers targeting Aflatoxin B1","authors":"Shazia Shareef,&nbsp;Hariprasad P.","doi":"10.1016/j.aca.2025.344201","DOIUrl":"10.1016/j.aca.2025.344201","url":null,"abstract":"<div><h3>Background</h3><div>Aflatoxin B<sub>1</sub> (AFB<sub>1</sub>) is a highly toxic fungal secondary metabolite that poses serious health risks to humans and animals, prompting the development of sensitive and specific detection technologies. Aptamer-based detection strategies offer a potential alternative to traditional detection methods. This study aimed to develop AFB<sub>1</sub>-specific aptamers using a gold nanoparticles-assisted SELEX (AuNP-SELEX) approach, eliminating the need for target immobilization. In this method, aptamers bound to AFB<sub>1</sub> detach from AuNPs while unbound or weakly bound sequences remain associated. The process was further strengthened using High-Throughput SELEX (HT-SELEX), enabling the efficient screening of large libraries for aptamers with minimal off-target binding.</div></div><div><h3>Results</h3><div>Successive rounds of SELEX led to the enrichment of high-affinity aptamers, which was monitored using a colorimetric AuNP-based assay. The top four aptamers- L2, CPMA1, L1, and L3, showed strong binding affinities with dissociation constants (<em>K</em><sub>d</sub>) of 1.24, 1.6, 2.55, and 5.26 nM, respectively. Circular dichroism spectroscopy confirmed conformational changes in the aptamers upon AFB<sub>1</sub> binding. A fluorescence assay using a FAM-labelled L2 aptamer and graphene oxide also achieved a detection limit of 0.53 nM.</div></div><div><h3>Significance</h3><div>This study demonstrates the effectiveness of the AuNP-assisted HT-SELEX platform as a rapid, visual, and refined method for selecting aptamers against small molecules like AFB<sub>1</sub>. The approach enhances detection sensitivity and specificity, offering a valuable tool for food safety monitoring and mycotoxin detection.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344201"},"PeriodicalIF":5.7,"publicationDate":"2025-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144067321","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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