Analytical and Bioanalytical Chemistry最新文献

{"title":"Rapid screening of xanthine oxidase inhibitors from Ligusticum wallichii by using xanthine oxidase functionalized magnetic metal-organic framework.","authors":"Yue Li, Hongmei Liu, Sikai Wang, Sisi Zhang, Wen Li, Guoqi Zhang, Yan Zhao","doi":"10.1007/s00216-024-05570-9","DOIUrl":"10.1007/s00216-024-05570-9","url":null,"abstract":"<p><p>In this study, xanthine oxidase was immobilized for the first time using a novel magnetic metal-organic framework material (Fe₃O₄-SiO₂-NH₂@MnO₂@ZIF-8-NH₂). A ligand fishing method was established to rapidly screen XOD inhibitors from Ligusticum wallichii based on the immobilized XOD. Characterization and properties of the immobilized enzyme revealed its excellent stability and reusability. A ligand was screened from Ligusticum wallichii and identified as ligustilide by ultra-high performance liquid chromatography tandem mass spectrometry. The IC₅₀ value of ligustilide was determined to be 27.70 ± 0.13 μM through in vitro inhibition testing. Furthermore, molecular docking verified that ligustilide could bind to amino acid residues at the active site of XOD. This study provides a rapid and effective method for the preliminary screening of XOD inhibitors from complex natural products and has great potential for further discovery of anti-hyperuricemic compounds.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142338701","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}

{"title":"Expedient measurement of total protein in human serum and plasma via the biuret method using fiber optic probe for patient samples and certified reference materials.","authors":"Sharon Yong, Cheng Yang Ng, Hong Liu, Yiting Chen, Qinde Liu, Tang Lin Teo, Tze Ping Loh, Sunil Kumar Sethi","doi":"10.1007/s00216-024-05561-w","DOIUrl":"10.1007/s00216-024-05561-w","url":null,"abstract":"<p><p>The biuret method is currently recognized as a reference measurement procedure for serum/plasma total protein by the Joint Committee for Traceability in Laboratory Medicine (JCTLM). However, as the reaction involved in this method is highly time-dependent, to ensure identical measurement conditions for calibrator and samples for high accuracy, a fast and simple measurement procedure is critical to ensure the precision and trueness of this method. We measured serum/plasma total protein using a Cary 60 spectrophotometer coupled with a fiber optic probe, which was faster and simpler than the conventional cuvette method. The biuret method utilizing alkaline solutions of copper sulfate and potassium sodium tartrate was added to the sample and calibrator (NIST SRM 927e) incubated for 1 h before measurement. A panel of samples consisting of pooled human serum, single donor serum, and certified reference materials (CRMs) from three sources were measured for method validation. Sixteen native patient samples were measured using the newly developed biuret method and compared against clinical analyzers. Additionally, the results of three cycles of a local External Quality Assessment (EQA) Programme submitted by participating clinical laboratories were compared against the biuret method. Our biuret method using fiber optic probe demonstrated good precision with within-day relative standard deviation (RSD) of 0.04 to 0.23% and between-day RSD of 0.58%. The deviations between the obtained values and the certified values for all three CRMs ranged from -0.38 to 1.60%, indicating good method trueness. The routine methods using clinical analyzers were also found to agree well with the developed biuret method using fiber optic probe for EQA samples and native patient samples. The biuret method using a fiber optic probe represented a convenient and reliable way of measuring serum total protein. It also demonstrated excellent precision and trueness using CRMs and patient samples, which made the method a simpler candidate reference method for serum protein measurement.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142363897","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}

{"title":"Determination of per- and polyfluoroalkyl substances (PFAS) in six different fish species from Swiss lakes.","authors":"Mylène Soudani, Lucie Hegg, Camille Rime, Camille Coquoz, Denise Bussien Grosjean, Francesco Danza, Nicola Solcà, Fiorella Lucarini, Davide Staedler","doi":"10.1007/s00216-024-05524-1","DOIUrl":"10.1007/s00216-024-05524-1","url":null,"abstract":"<p><p>Per- and polyfluoroalkyl substances (PFAS) are persistent environmental contaminants with bioaccumulation potential, particularly affecting aquatic ecosystems and human health also via fish consumption. There is therefore a need for reliable extraction methods and studies to accurately assess PFAS levels in fish, crucial for understanding bioaccumulation and potential toxicological effects on both fish and humans through consumption. This study investigated PFAS levels in freshwater fish from Swiss lakes, focusing on six common species: Coregonus wartmanni, Cyprinus carpio, Oncorhynchus mykiss, Perca fluviatilis, Salmo trutta, and Squalius cephalus. Utilizing an optimized QuEChERS extraction method, 15 PFAS were analyzed in 218 fish fillet samples using liquid chromatography-mass spectrometry (LC-MS/MS). The results were compared to EU regulations and EFSA guidelines for tolerable weekly intake (TWI), with a specific focus on correlations between fish size and PFAS concentration. Our findings reveal significant PFAS contamination, particularly in Perca fluviatilis with perfluorooctane sulfonic acid (PFOS) and perfluorohexane sulfonic acid (PFHxS) levels often exceeding EU safety limits. TWI, calculated for a person of 70 kg body weight and an intake of 200 g of fish fillet, is exceeded in 95% of Coregonus wartmanni, 100% of Squalius cephalus, and in 55%, 50%, and 36% of the specimens Oncorhynchus mykiss, Salmo trutta, and Perca fluviatilis respectively. Correlation analysis between PFAS concentration and fish size in 121 Salmo trutta specimens revealed significant positive correlations for perfluorobutane sulfonic acid (PFBS), perfluorodecanoic acid (PFDA), and perfluorohexane sulfonic acid (PFHxS), and a negative correlation for perfluoropentanoic acid (PFPeA). These results underscore the critical need for continuous monitoring and regulatory efforts to mitigate PFAS exposure risks to both ecosystems and human health.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11541325/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142338692","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Incorporating dialogue in laboratory teaching.","authors":"Michael K Seery, Hendra Y Agustian, Frederik V Christiansen, Bente Gammelgaard, Rie H Malm","doi":"10.1007/s00216-024-05569-2","DOIUrl":"10.1007/s00216-024-05569-2","url":null,"abstract":"","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11541328/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142338696","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"The sensitive detection of low molecular mass peptide drugs in dried blood spots by solid-phase extraction and LC-HRMS.","authors":"Wei Chang, Siyu Yan, Xiya Yan, Zhanliang Wang, Boya Gu, Yunxi Liu, Yufeng Zhang, Sheng Yang","doi":"10.1007/s00216-024-05480-w","DOIUrl":"10.1007/s00216-024-05480-w","url":null,"abstract":"<p><p>Dried blood spot (DBS) technique has become a new popular topic in anti-doping field in recent years due to its advantages of sample stability and easy operation. It can be employed as a supplementary method to routine urine analysis. However, the small volume of DBS samples (usually 10-20 μL) significantly reduces the application value of this technique. Therefore, the development of sensitive detection methods for the analysis of prohibited substances in DBS is particularly important. In this study, based on the characteristics of low molecular mass peptide (LMMP) drugs, systematic optimization strategies were utilized for the first time to establish a sensitive detection method for LMMPs in DBS. Without using DMSO to enhance mass spectrometry ionization efficiency of peptides, the limits of detection (LOD) ranged between 0.05 and 3.74 ng/mL, significantly better than the previously reported method (0.5-20 ng/mL). This method was validated according to the guidelines of the World Anti-Doping Agency (WADA), and corresponding post-administration study was conducted, demonstrating that the method could be applied to routine analysis of LMMP drugs in DBS. Moreover, since DMSO is not involved, this method also has the potential to simultaneously detect both LMMP and small molecular drugs.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142046136","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}

{"title":"Capillary zone electrophoresis-tandem mass spectrometry for in-depth proteomics analysis via data-independent acquisition.","authors":"Rong Liu, Gang Lu, Xiaozhong Hu, Junhui Li, Zhenbin Zhang, Keqi Tang","doi":"10.1007/s00216-024-05502-7","DOIUrl":"10.1007/s00216-024-05502-7","url":null,"abstract":"<p><p>A capillary zone electrophoresis (CZE) system was coupled to an Orbitrap mass spectrometer operating in a data-independent acquisition (DIA) mode for in-depth proteomics analysis. The performance of this CZE-DIA-MS system was systemically evaluated and optimized under different operating conditions. The performance of the fully optimized CZE-DIA-MS system was subsequently compared to the one by using the same CZE-MS system operating in a data-dependent acquisition (DDA) mode. The experimental results show that the numbers of identified peptides and proteins acquired in the DIA mode are much higher than the ones acquired in the DDA mode, especially with the small sample loading amount. Specifically, the numbers of identified peptides and proteins acquired in the DIA mode are 1.8-fold and 2-fold higher than the ones acquired in the DDA mode by using 12.5 ng Hela digests. The proteins identified in the DIA mode also cover almost all the proteins identified in the DDA mode. In addition, a potential cancer biomarker protein, carbohydrate antigen 125, undetected in the DDA mode, can be easily identified in the DIA mode even with 12.5 ng Hela digests. The performance of the CZE-DIA-MS system for in-depth proteomics analysis with a limited sample amount has been fully demonstrated for the first time through this study.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142078719","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}

{"title":"Analysis of tissue-substrate adhesion by hyperspectral surface plasmon resonance microscopy.","authors":"Bo Yang, Hongyi Tang, Ziwei Liu, Xinxia Cai, Zhi-Mei Qi","doi":"10.1007/s00216-024-05509-0","DOIUrl":"10.1007/s00216-024-05509-0","url":null,"abstract":"<p><p>The preparation of histology slides is a critical step in histopathology, and poor-quality histology slides with weak adhesion of tissue sections to the substrate often affect diagnostic accuracy and sometimes lead to diagnostic failure due to tissue section detachment. This issue has been of concern and some methods have been proposed to enhance tissue-substrate adhesion. Unfortunately, quantitative analysis of the adhesion between tissue sections and glass slides is still challenging. In this work, the adhesion of mouse brain tissue sections on gold-coated glass slides was analyzed using a laboratory-fabricated hyperspectral surface plasmon resonance microscopy (HSPRM) system that enabled single-pixel spectral SPR sensing and provided two-dimensional (2D) distribution of resonance wavelengths (RWs). The existence of the nanoscale water gap between the tissue section and the substrate was verified by fitting the RW measured in each pixel using the five-layer Fresnel reflection model. In addition, a 2D image of the tissue-substrate adhesion distance (AD) was obtained from the measured 2D distribution of RWs. The results showed that tissue-substrate AD was 20-35 nm in deionized water and 4-24 nm in saline solution. The HSPRM system used in this work has a wide wavelength range of 400-1000 nm and can perform highly sensitive and label-free detection over a large dynamic detection range with high spectral and spatial resolutions, showing significant potential applications in stain-free tissue imaging, quantitative analysis of tissue-substrate adhesion, accurate identification of tumor cells, and rapid histopathological diagnosis.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142103039","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}

{"title":"Development of an optimized SEC method for characterization of genome DNA leakage from adeno-associated virus products.","authors":"Shuai Li, Xiaoyan Wang, Kuan-Yu Nick Lai, Jonathan Wert, Li Zhi, Mohammed Shameem, Dingjiang Liu","doi":"10.1007/s00216-024-05623-z","DOIUrl":"https://doi.org/10.1007/s00216-024-05623-z","url":null,"abstract":"<p><p>Adeno-associated virus (AAV) vectors are widely used to deliver therapeutic transgenes due to their superior safety, relatively low immunogenicity, and ability to target diverse tissues. AAV gene therapy products are typically formulated as frozen liquid and stored below - 60 °C, and therefore are subjected to multiple freeze/thaw cycles during manufacturing and administration. Recent studies have shown that genome DNA leakage could be induced by freeze/thaw stress. DNA leakage from AAV capsids has been reported to potentially impact product stability, induce immune responses, and compromise product efficacy. Thus, further characterization to improve the understanding of genome DNA leakage is necessary for mitigating the risks associated with genome DNA leakage during AAV product development. In this work, we developed an optimized size-exclusion chromatography (SEC) method for quantifying the leakage of genome DNA across multiple different AAV serotypes and demonstrated satisfactory assay performance in sensitivity, precision, and linearity. Furthermore, we showed that this method could also be applied to quantifying additional quality attributes of AAV, including the percentage of full capsids and quantification of AAV dimers. By using this optimized SEC method, we demonstrated that significantly increased free DNA was observed with increasing freeze/thaw cycles or at a temperature approaching the onset temperature for genome DNA ejection, which was effectively mitigated by the addition of 1.5% w/v sucrose in the AAV formulation. Thus, this optimized SEC method can serve as an invaluable tool for AAV formulation, product, and process development in ensuring the quality and stability of AAV gene therapy products.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142562629","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}

{"title":"Novel mimetic tissue standards for precise quantitative mass spectrometry imaging of drug and neurotransmitter concentrations in rat brain tissues.","authors":"Kenichi Watanabe, Sayo Takayama, Toichiro Yamada, Masayo Hashimoto, Jun Tadano, Tetsuya Nakagawa, Takao Watanabe, Eiichiro Fukusaki, Izuru Miyawaki, Shuichi Shimma","doi":"10.1007/s00216-024-05477-5","DOIUrl":"10.1007/s00216-024-05477-5","url":null,"abstract":"<p><p>Understanding the relationship between the concentration of a drug and its therapeutic efficacy or side effects is crucial in drug development, especially to understand therapeutic efficacy in central nervous system drug, quantifying drug-induced site-specific changes in the levels of endogenous metabolites, such as neurotransmitters. In recent times, evaluation of quantitative distribution of drugs and endogenous metabolites using matrix-assisted laser desorption/ionization (MALDI)-mass spectrometry imaging (MSI) has attracted much attention in drug discovery research. However, MALDI-MSI quantification (quantitative mass spectrometry imaging, QMSI) is an emerging technique, and needs to be further developed for practicable and convenient use in drug discovery research. In this study, we developed a reliable QMSI method for quantification of clozapine (antipsychotic drug) and dopamine and its metabolites in the rat brain using MALDI-MSI. An improved mimetic tissue model using powdered frozen tissue for QMSI was established as an alternative method, enabling the accurate quantification of clozapine levels in the rat brain. Furthermore, we used the improved method to evaluate drug-induced fluctuations in the concentrations of dopamine and its metabolites. This method can quantitatively evaluate drug localization in the brain and drug-induced changes in the concentration of endogenous metabolites, demonstrating the usefulness of QMSI.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11493812/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141911247","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development, validation and application of an LC-MS/MS method quantifying free forms of the micronutrients queuine and queuosine in human plasma using a surrogate matrix approach.","authors":"Xiaobei Pan, Swathine Chandrasekaran, Jayne V Woodside, Steffi G Riedel-Heller, Martin Scherer, Michael Wagner, Alfredo Ramirez, Brian D Green","doi":"10.1007/s00216-024-05489-1","DOIUrl":"10.1007/s00216-024-05489-1","url":null,"abstract":"<p><p>Queuosine (Q) is a hypermodified 7-deaza-guanosine nucleoside exclusively synthesized by bacteria. This micronutrient and its respective nucleobase form queuine (q) are salvaged by humans either from gut microflora or digested food. Depletion of Q-tRNA in human or mouse cells causes protein misfolding that triggers endoplasmic reticular stress and the activation of the unfolded protein responses. In vivo, this reduces the neuronal architecture of the mouse brain affecting learning and memory. Herein, a sensitive method for quantifying free q and Q in human blood was developed, optimised and validated. After evaluating q/Q extraction efficiency in several different solid-phase sorbents, Bond Elut PBA (phenylboronic acid) cartridges were found to have the highest extraction recovery for q (82%) and Q (71%) from pooled human plasma. PBS with 4% BSA was used as surrogate matrix for method development and validation. An LC-MS/MS method was validated across the concentration range of 0.0003-1 µM for both q and Q, showing excellent linearity (r² = 0.997 (q) and r² = 0.998 (Q)), limit of quantification (0.0003 µM), accuracy (100.39-125.71%) and precision (CV% < 15.68%). In a sampling of healthy volunteers (n = 44), there was no significant difference in q levels between male (n = 14; mean = 0.0068 µM) and female (n = 30; mean = 0.0080 µM) participants (p = 0.50). Q was not detected in human plasma. This validated method can now be used to further substantiate the role of q/Q in nutrition, physiology and pathology.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11493786/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142003294","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}