Analytical and Bioanalytical Chemistry最新文献

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Ag NPs loading and ultraviolet irradiation strategies for enhancing the performance of WO3/Ti3C2TX composites in detecting 2-heptanone. WO3/Ti3C2TX复合材料中Ag NPs的负载和紫外辐照策略对2-庚酮检测性能的提高。
IF 3.8 2区 化学
Analytical and Bioanalytical Chemistry Pub Date : 2025-10-13 DOI: 10.1007/s00216-025-06143-0
Jinfu Zhang, Pei Li, Helei Yang, Zhiguo Zhu, Hua Zhou, Zhenhe Wang, Xia Sun
{"title":"Ag NPs loading and ultraviolet irradiation strategies for enhancing the performance of WO<sub>3</sub>/Ti<sub>3</sub>C<sub>2</sub>T<sub>X</sub> composites in detecting 2-heptanone.","authors":"Jinfu Zhang, Pei Li, Helei Yang, Zhiguo Zhu, Hua Zhou, Zhenhe Wang, Xia Sun","doi":"10.1007/s00216-025-06143-0","DOIUrl":"https://doi.org/10.1007/s00216-025-06143-0","url":null,"abstract":"<p><p>As a typical volatile organic compound (VOC), 2-heptanone detection is critical in food spoilage monitoring, chemical production safety control, and environmental pollutant tracking. However, developing a 2-heptanone gas sensor with high sensitivity at room temperature remains challenging. This study prepared WO<sub>3</sub>/Ti<sub>3</sub>C<sub>2</sub>T<sub>X</sub> MXene composites (WT-50) via a solvothermal method and constructed a ternary composite Ag/WO<sub>3</sub>/Ti<sub>3</sub>C<sub>2</sub>T<sub>X</sub>-50 (AgWT-50) by loading Ag nanoparticles. The gas-sensing properties of WT-50, AgWT-50, and WT-50 excited by ultraviolet light toward 2-heptanone were investigated. AgWT-50 exhibits a high response of 4.62 to 55.04 ppm 2-heptanone at room temperature, with excellent selectivity and stability. The UV-irradiated WT-50 (WT-50Z) demonstrates more significant performance enhancement, with a response of 6.54, which is twice that of WT-50 (3.25), and notably improved selectivity. Mechanistic studies reveal that the performance improvements of AgWT-50 and WT-50Z originate from increased oxygen vacancies induced by Ag nanoparticle loading and UV-induced high-energy hot electrons and elevated photogenerated carrier concentration, respectively. Finally, the fabricated sensor was successfully applied to evaluate the freshness of salmon, establishing a food quality monitoring model based on gas-sensing responses. This study provides a new strategy for developing room-temperature high-performance gas sensors, showing significant application potential in food quality control, public health protection, and environmental safety fields.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145278665","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
Deciphering the formation of biogenic nanoparticles and their protein corona: State-of-the-art and analytical challenges. 破译生物纳米颗粒及其蛋白质冠的形成:最新的和分析的挑战。
IF 3.8 2区 化学
Analytical and Bioanalytical Chemistry Pub Date : 2025-10-12 DOI: 10.1007/s00216-025-06144-z
Andrés Suárez Priede, Miguel Gómez-Sánchez, Paula García-Cancela, Jörg Bettmer, Paula Díez
{"title":"Deciphering the formation of biogenic nanoparticles and their protein corona: State-of-the-art and analytical challenges.","authors":"Andrés Suárez Priede, Miguel Gómez-Sánchez, Paula García-Cancela, Jörg Bettmer, Paula Díez","doi":"10.1007/s00216-025-06144-z","DOIUrl":"https://doi.org/10.1007/s00216-025-06144-z","url":null,"abstract":"<p><p>Biogenic synthesis of nanoparticles (NPs) using biological organisms such as plants, fungi, and bacteria offers a sustainable, green alternative to conventional chemical synthesis. These green methods involve biological matrices mediating metal ion reduction to form NPs capped by complex biomolecular coronas. These protein coronas critically affect NP stability, biological identity, and functionality, including notable therapeutic potentials. Despite advancements, the dynamic and heterogeneous nature of in situ biogenic NP formation remains insufficiently understood, as most studies emphasize synthetic production using biological extracts combined with metal precursors. Moreover, characterization of biogenic NPs requires a suite of bioanalytical techniques, each offering diverse advantages but also inherent limitations, requiring a comprehensive understanding of their features to critically select the optimal combination of strategies to obtain a full descriptive picture of the studied NPs. This review critically discusses current biogenic synthesis methods alongside the complementary bioanalytical strategies employed to elucidate NP formation, corona composition, and their biological implications. By highlighting the strengths and weaknesses of available techniques, the review aims to identify key challenges and future directions necessary to advance the safe and effective development of green nanotechnologies.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145273445","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 novel approach to determination of amino acids and cyclic heptapeptides using imprinted proteins. 一种利用印迹蛋白测定氨基酸和环七肽的新方法。
IF 3.8 2区 化学
Analytical and Bioanalytical Chemistry Pub Date : 2025-10-11 DOI: 10.1007/s00216-025-06103-8
Kirill Yu Presnyakov, Polina M Ilicheva, Ivan A Reshetnik, Mikhail V Pozharov, Pavel S Pidenko, Natalia A Burmistrova
{"title":"A novel approach to determination of amino acids and cyclic heptapeptides using imprinted proteins.","authors":"Kirill Yu Presnyakov, Polina M Ilicheva, Ivan A Reshetnik, Mikhail V Pozharov, Pavel S Pidenko, Natalia A Burmistrova","doi":"10.1007/s00216-025-06103-8","DOIUrl":"https://doi.org/10.1007/s00216-025-06103-8","url":null,"abstract":"<p><p>For the first time, imprinted proteins (IPs) were used as molecular recognition elements for determination of amino acids (arginine, Arg) and heptapeptides (microcystin-LR, MC-LR) in competitive solid-phase fluorescent assay (CSPA). Bovine serum albumin and ovalbumin were used as protein matrices for imprinting procedures. Preliminary simulation of the interaction of Arg and proteins by molecular docking and dynamic methods was used to predict optimal template concentration during IP synthesis. We developed an original method of increasing the affinity of IP binding sites by imprinting the Arg derivative (Arg-aniline) with greater accessibility of template amino groups. Silica nanoparticles modified with IPs have a high sorption capacity to Arg (7.8 mg g <math><mmultiscripts><mrow></mrow> <mrow></mrow> <mrow><mo>-</mo> <mn>1</mn></mrow> </mmultiscripts> </math> ). We have developed procedures for determination of Arg and MC-LR by using CSPA; the linear determination range for Arg is 0.7-10 ng mL <math><mmultiscripts><mrow></mrow> <mrow></mrow> <mrow><mo>-</mo> <mn>1</mn></mrow> </mmultiscripts> </math> (LoQ = 0.5 ng mL <math><mmultiscripts><mrow></mrow> <mrow></mrow> <mrow><mo>-</mo> <mn>1</mn></mrow> </mmultiscripts> </math> ), while for MC-LR it is 4-60 ng mL <math><mmultiscripts><mrow></mrow> <mrow></mrow> <mrow><mo>-</mo> <mn>1</mn></mrow> </mmultiscripts> </math> (LoQ = 2 ng mL <math><mmultiscripts><mrow></mrow> <mrow></mrow> <mrow><mo>-</mo> <mn>1</mn></mrow> </mmultiscripts> </math> ). The obtained analytical approach was tested for Arg determination in a biologically active supplement.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145273411","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
Anthocyanins extraction from Amazonian matrices using natural deep eutectic solvents: characterization and ecological impact. 用天然深共晶溶剂从亚马逊基质中提取花青素:表征和生态影响。
IF 3.8 2区 化学
Analytical and Bioanalytical Chemistry Pub Date : 2025-10-11 DOI: 10.1007/s00216-025-06100-x
Ianê Valente Pires, Antonio Manoel da Cruz Rodrigues, Carolina Turnes Pasini Deolindo, Rodrigo B Hoff, Luiza Helena Meller da Silva, Marleny D A Saldaña
{"title":"Anthocyanins extraction from Amazonian matrices using natural deep eutectic solvents: characterization and ecological impact.","authors":"Ianê Valente Pires, Antonio Manoel da Cruz Rodrigues, Carolina Turnes Pasini Deolindo, Rodrigo B Hoff, Luiza Helena Meller da Silva, Marleny D A Saldaña","doi":"10.1007/s00216-025-06100-x","DOIUrl":"https://doi.org/10.1007/s00216-025-06100-x","url":null,"abstract":"<p><p>This study investigated the effectiveness of natural deep eutectic solvents (NADES) as a green alternative to traditional organic solvents for the extraction of anthocyanins from three Amazonian matrices: açaí, mangosteen pericarp, and purple yam. High-intensity ultrasound-assisted extraction (HIUS) was evaluated by varying key processing parameters such as molar ratio, solid-to-liquid ratio (S/L), added water, extraction time, and ultrasound power. Results showed that both molar ratio and added water had a significant impact on extraction efficiency. The addition of water to NADES was crucial in reducing viscosity and enhancing anthocyanin solubility, thereby improving mass transfer. However, excessive water led to decreased extraction yields, likely due to the disruption of hydrogen bonds within the NADES system. The extraction time and ultrasound power proved to be critical factors, as prolonged extraction periods and high power resulted in the degradation of anthocyanins. This study concluded that NADES yielded promising results for anthocyanin extraction. The optimal anthocyanin extraction conditions for açaí (132.20 mg/100 g) were a 1:2 molar ratio, 1:120 S/L, 30% added water, 5 min extraction, and 600 W power. For mangosteen pericarp, the optimal anthocyanin extraction conditions (58.81 mg/100 g) were a 1:2 molar ratio, 1:120 S/L, 30% added water, 5 min, and 1200 W power. For purple yam, the optimal anthocyanin extraction conditions (25.95 mg/100 g) were a 1:3 molar ratio, 1:120 S/L, 20% added water, 5 min, and 1200 W power. Additionally, the NADES-extracted anthocyanins demonstrated good stability across a range of pH values. Liquid chromatography coupled with electrospray ionization and tandem mass spectrometry (LC-ESI-MS/MS) analysis revealed variability in phenolic profiles, while açaí and mangosteen pericarp showed diverse bioactive compounds, including isorhamnetin and epicatechin. Purple yam exhibited no detectable phenolics. Compared to conventional solvents, NADES extraction exhibited a lower environmental impact, as assessed by Ecoscale and Analytical GREEnness Metric (AGREE) tools.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145273476","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
Deciphering the binding strength of oil matrix through molecularly resolved release energy analysis using thermal slicing ramped pyrolysis GC-MS. 热切片斜坡热解气相色谱-质谱联用技术通过分子分辨释放能分析来破译油基质的结合强度。
IF 3.8 2区 化学
Analytical and Bioanalytical Chemistry Pub Date : 2025-10-10 DOI: 10.1007/s00216-025-06110-9
Kaijun Lu, Jianhong Xue, Zhanfei Liu
{"title":"Deciphering the binding strength of oil matrix through molecularly resolved release energy analysis using thermal slicing ramped pyrolysis GC-MS.","authors":"Kaijun Lu, Jianhong Xue, Zhanfei Liu","doi":"10.1007/s00216-025-06110-9","DOIUrl":"https://doi.org/10.1007/s00216-025-06110-9","url":null,"abstract":"<p><p>Recent advancements in analytical techniques have significantly furthered our understanding of the chemical composition of petroleum and its derivatives. However, there remains a missing link connecting the molecular structure with how specific compounds are bound within the sample matrix. Traditional approaches to study energetic characteristics of petroleum often rely on bulk property measurements (e.g., thermogravimetric analysis), therefore lacking the resolution needed to capture compound-specific interactions and structural information. In this work, we aim to fill the gap between compositional and energetic analyses by employing thermal slicing ramped pyrolysis gas chromatography mass spectrometry (TSRP-GC-MS). TSRP-GC-MS enables the analysis of temperature-dependent release patterns of pyrolyzates, linking molecular structures to energetic characteristics via computing the energy distributions for specific pyrolyzates. Results of the photodegradation experiments demonstrate that as the photodegradation proceeds, the energy required to disrupt the matrix and to release n-alkanes increased from ca. 90 kJ/mol to over 100 kJ/mol, with significant increases for each individual n-alkane. The release energy of individual n-alkanes in crude oil and in tarball collected in the field were further compared in the second case study. The results not only showed an increase from 110 kJ/mol for n-alkanes in crude oil to 118 kJ/mol in tarball, but also revealed a homogenizing trend of the matrix strength of different n-alkanes in the latter. Overall, the proposed TSRP-GC-MS approach offers a powerful tool for advancing our understanding of petroleum and oil and has the potential to be expanded to the study of other complex natural mixtures.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145273426","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
How does NMR support SARS-CoV-2 protein-ligand interaction studies? 核磁共振如何支持SARS-CoV-2蛋白-配体相互作用研究?
IF 3.8 2区 化学
Analytical and Bioanalytical Chemistry Pub Date : 2025-10-09 DOI: 10.1007/s00216-025-06081-x
Norazlan Mohmad Misnan, Azira Muhamad, Mohd Ridzuan Mohd Abd Razak, Kok Wai Lam
{"title":"How does NMR support SARS-CoV-2 protein-ligand interaction studies?","authors":"Norazlan Mohmad Misnan, Azira Muhamad, Mohd Ridzuan Mohd Abd Razak, Kok Wai Lam","doi":"10.1007/s00216-025-06081-x","DOIUrl":"https://doi.org/10.1007/s00216-025-06081-x","url":null,"abstract":"<p><p>The COVID-19 pandemic has highlighted the urgent need for effective antiviral strategies against SARS-CoV-2. Nuclear magnetic resonance (NMR) spectroscopy has played a critical role by providing detailed insights into protein-ligand interactions at atomic resolution. This review compiles and critically evaluates recent NMR-based findings, highlighting how these studies have supported the identification and optimization of antiviral compounds targeting viral proteins involved in replication and immune evasion. By revealing structural and dynamic details, NMR has significantly advanced structure-based drug design and enhanced the selection of promising antiviral candidates. Integration of NMR with complementary experimental methods has further improved our understanding of small molecule interactions and mechanisms of action. Looking forward, the review emphasizes the need for greater translational application of NMR findings through interdisciplinary collaboration and recommends increased integration with clinical and preclinical research. These recommendations aim to fully harness NMR's potential, thereby strengthening preparedness for future viral threats and guiding current therapeutic development efforts.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145249121","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 validation and analysis of halogenated natural products (HNPs) in seafood samples. 海鲜样品中卤化天然产物(HNPs)的方法验证与分析。
IF 3.8 2区 化学
Analytical and Bioanalytical Chemistry Pub Date : 2025-10-08 DOI: 10.1007/s00216-025-06141-2
Marco Krämer, Walter Vetter, Oliver Kappenstein, Astrid Spielmeyer
{"title":"Method validation and analysis of halogenated natural products (HNPs) in seafood samples.","authors":"Marco Krämer, Walter Vetter, Oliver Kappenstein, Astrid Spielmeyer","doi":"10.1007/s00216-025-06141-2","DOIUrl":"https://doi.org/10.1007/s00216-025-06141-2","url":null,"abstract":"<p><p>Halogenated natural products (HNPs) are a diverse group of organohalogen compounds, predominantly found in the marine environment. Selected HNPs show structural similarity to persistent organic pollutants (POPs), but data on their occurrence is limited. An analytical method for the detection of 17 commonly reported HNPs, as well as selected POPs, using gas chromatography with electron-capture negative ionisation mass spectrometry (GC/ECNI-MS) was established and validated for salmon and blue mussel. The validation confirmed the applicability of the method with recovery rates and inter-day coefficients of variations of 52-101% and 3.7-16%, respectively. The subsequent application of the method to 17 samples of frequently consumed seafood products from the German retail market demonstrated its suitability for a wide variety of matrices. HNPs were detected in all analysed samples, with contents ranging from <0.05 to up to 7000 ng/g lipid weight (lw). Highest median values were found for mixed-halogenated compound 1 (MHC-1), 2,4,6-tribromoanisole (2,4,6-TBA), and the heptachlorinated bipyrrole Q1 (19, 6.0, and 3.4 ng/g lw, respectively). In 14 out of 17 analysed samples, the sum of HNPs was in the same concentration range or exceeded the sum of the investigated POPs, indicating the relevant exposure of consumers of seafood products in Germany to HNPs and emphasising the relevance of HNPs as organohalogen compounds in seafood samples.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145249127","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 review of the recent advances in extraction techniques for volatilome of aromatic and fragrant plants. 综述了芳香植物挥发油提取技术的最新进展。
IF 3.8 2区 化学
Analytical and Bioanalytical Chemistry Pub Date : 2025-10-08 DOI: 10.1007/s00216-025-06109-2
Valentina Chiaia, Micaela Galletta, Giuseppe Micalizzi, Luigi Mondello, Tania Maria Grazia Salerno
{"title":"A review of the recent advances in extraction techniques for volatilome of aromatic and fragrant plants.","authors":"Valentina Chiaia, Micaela Galletta, Giuseppe Micalizzi, Luigi Mondello, Tania Maria Grazia Salerno","doi":"10.1007/s00216-025-06109-2","DOIUrl":"https://doi.org/10.1007/s00216-025-06109-2","url":null,"abstract":"<p><p>The last decade has witnessed an increase in the development of extraction techniques for volatile components from different matrices. Meanwhile, analytical methods have shifted toward the miniaturization of sample preparation procedures, the reduction of solvent consumption, and the adoption of solventless or solvent-minimized extraction techniques to lessen the use of organic solvents and toxic reagents. These innovations plan to enhance extraction efficiency, improve sensitivity, and side with sustainability goals by reducing environmental impact. In this context, the present review article aims to provide the readers with a comprehensive understanding of sample preparation and extraction techniques for the analysis of plant volatilome. The elucidation of plant aromatic and fragrant substances is of great significance due to their diverse roles in fragrance, flavor, agriculture, and medicine and for their potential application in biotechnological and pharmaceutical research innovations. Particularly, this review compares conventional extraction methods with alternative and more appealing, solventless methods, evaluating their efficiency, scalability, and applicability on both laboratory and industrial scale. The discussion revolves around the development of high-throughput sample preparation procedures, sampling protocols, and their different aspects and areas of application. Finally, the greenness of the different methodologies is critically evaluated in terms of solvent, time, and energy consumption, pointing out sustainable and cost-effective approaches for plant volatilome analysis.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145243633","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
Separation of PS diastereomers in GalNAc-conjugated siRNA-a comparative study of chromatographic and ion mobility mass spectrometry approaches. galnac -共轭sirna中PS非对映体的分离——色谱法和离子迁移质谱法的比较研究。
IF 3.8 2区 化学
Analytical and Bioanalytical Chemistry Pub Date : 2025-10-08 DOI: 10.1007/s00216-025-06123-4
Mona-Katharina Bill, Micaela Graglia, Jo-Anne Riley, Mateusz Zugaj, Nadeschda Demtschenko, Jonathan Fox, Lucas Bethge, Jeske J Smink, Christian Manz
{"title":"Separation of PS diastereomers in GalNAc-conjugated siRNA-a comparative study of chromatographic and ion mobility mass spectrometry approaches.","authors":"Mona-Katharina Bill, Micaela Graglia, Jo-Anne Riley, Mateusz Zugaj, Nadeschda Demtschenko, Jonathan Fox, Lucas Bethge, Jeske J Smink, Christian Manz","doi":"10.1007/s00216-025-06123-4","DOIUrl":"https://doi.org/10.1007/s00216-025-06123-4","url":null,"abstract":"<p><p>The separation and characterization of phosphorothioate (PS) diastereomers in GalNAc-conjugated siRNA presents a significant analytical challenge due to the high number of isomers present. To tackle this challenge, we explore and optimize various separation techniques, including chromatographic methods (ion-pair reversed-phase, anion exchange, and hydrophilic interaction liquid chromatography) and ion mobility mass spectrometry (IMS) to assess their efficacy in diastereomer separation. Our results indicate that AEX provides the highest diastereomer selectivity among the chromatographic techniques, although none achieved complete diastereomer separation for the chosen antisense and sense strand reference compounds. IMS, applied within a fragment-based tandem mass spectrometry approach, allows separation of all diastereomers of the antisense strand and partial resolution of the sense strand in the gas phase. The comparison of relative LC-UV quantification with IMS data reveals a strong correlation and suggests that IMS can effectively characterize diastereomer ratios not only qualitatively but also quantitatively, establishing IMS as a promising complementary analytical technique for diastereomer separation besides more established LC-UV methods.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145243620","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
Screening of selective serotonin reuptake inhibitors from Cyperus rotundus using immobilized neurotransmitter transporter affinity chromatography for antidepressant discovery. 固定化神经递质转运体亲和色谱法筛选圆形香参选择性血清素再摄取抑制剂的研究。
IF 3.8 2区 化学
Analytical and Bioanalytical Chemistry Pub Date : 2025-10-08 DOI: 10.1007/s00216-025-06105-6
Xue Zhao, Yi Yu, Lili Yang, Hui Liu, Ting Lei
{"title":"Screening of selective serotonin reuptake inhibitors from Cyperus rotundus using immobilized neurotransmitter transporter affinity chromatography for antidepressant discovery.","authors":"Xue Zhao, Yi Yu, Lili Yang, Hui Liu, Ting Lei","doi":"10.1007/s00216-025-06105-6","DOIUrl":"https://doi.org/10.1007/s00216-025-06105-6","url":null,"abstract":"<p><p>Despite advances in targeting neurotransmitter transporters, developing selective serotonin reuptake inhibitors (SSRIs) remains crucial for treating psychiatric disorders. Here, we developed an innovative affinity chromatography platform to discover novel SSRIs from Cyperus rotundus (CR), utilizing immobilized serotonin transporter (SERT) as the capture probe. Our approach employed genetically encoded unnatural amino acids (UAAs) and a \"thiol-ene\" click reaction to create a stable, functional SERT stationary phase. This immobilized SERT chromatography demonstrated superior specificity and longevity, enabling reliable ligand-receptor interaction analysis and inhibitor screening. Validation studies confirmed the platform's accuracy, with ligand affinity rankings matching conventional radioimmunoassay results. Through this method, we identified α-cyperone as a potent SERT inhibitor from CR, exhibiting high binding affinity (6.97 × 10<sup>4</sup> M<sup>-1</sup>) and favorable drug-like properties. In vivo studies revealed that α-cyperone alleviated depression-like behaviors in chronic unpredictable mild stress (CUMS) mice by modulating SERT function-inhibiting SERT reuptake and increasing synaptic 5-HT and NE concentrations. These findings position α-cyperone as a promising natural SSRI candidate. Importantly, this immobilization strategy is broadly applicable to various proteins, offering an efficient platform for high-throughput screening of targeted therapeutics from natural products.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145249115","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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