Analytical and Bioanalytical Chemistry最新文献

{"title":"Database of diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and hyperspectral imaging (HSI) spectra of pigments and dyes for historical document analysis.","authors":"Anna Sofia Reichert, Ana Belén López-Baldomero, Francisco Moronta-Montero, Ana López-Montes, Eva María Valero, Carolina Cardell","doi":"10.1007/s00216-025-05948-3","DOIUrl":"https://doi.org/10.1007/s00216-025-05948-3","url":null,"abstract":"<p><p>Characterizing pigments and dyes in historical manuscripts is challenging due to the fragility of materials, the complex composition of low-concentration elements, and sampling limitations. Consequently, complementary non-invasive analytical techniques and non-contact measurement methods are often required. This study presents the most comprehensive spectral database to date, combining diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and hyperspectral imaging (HSI) to aid in identifying pigments, dyes, and binders historically used in illuminated and decorated manuscripts. A total of 156 painting mock-ups were created using traditional techniques, incorporating variations in binders, pigment particle sizes, support types, surface roughness, and application methods. Spectral imaging was performed in the visible and near infrared (VNIR) and short-wave infrared (SWIR) regions, while DRIFTS analysis covered the middle wave infrared (MWIR) region. For DRIFTS, both contact and non-contact measurements were tested. Using the samples in the database, the influence of binder, support, and grain size on the sample spectra and color were analyzed and discussed. This database facilitates pigment and dye identification using DRIFTS or HSI data independently or in combination through data fusion, applying techniques ranging from direct spectral comparison to advanced methods such as machine learning and spectral unmixing. By making this database publicly available, the study underscores the value of DRIFTS and HSI in identifying painting materials and contributes to the preservation of historical manuscripts.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144315684","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":"Correction to: Development of a candidate reference method for the simultaneous quantification of betaine, choline and trimethylamine N‑oxide in serum samples by two‑dimensional liquid chromatography and isotope dilution tandem mass spectrometry.","authors":"Daniela Pineda-Cevallos, María Castañón Apilánez, Elena López-Cancio, Belén Prieto García, J Ignacio García Alonso, Pablo Rodriguez-Gonzalez","doi":"10.1007/s00216-025-05960-7","DOIUrl":"https://doi.org/10.1007/s00216-025-05960-7","url":null,"abstract":"","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144315683","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":"Flipping the lab with AI support: a scalable model to address the theory-practice gap in analytical chemistry education.","authors":"Paulo R M Correia, Ian M Kinchin, Thiago R L C Paixão, David T Harvey","doi":"10.1007/s00216-025-05961-6","DOIUrl":"https://doi.org/10.1007/s00216-025-05961-6","url":null,"abstract":"","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144300865","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":"Understanding the chemical stability of peptidomimetic therapeutics using high-resolution mass spectrometry: a study of terlipressin and its degradation products.","authors":"Ashwini Chawathe, Nitish Sharma","doi":"10.1007/s00216-025-05944-7","DOIUrl":"https://doi.org/10.1007/s00216-025-05944-7","url":null,"abstract":"<p><p>Terlipressin, a synthetic 12-amino acid peptidomimetic of vasopressin, is a critical therapeutic agent for hepatorenal syndrome and oesophageal variceal hemorrhage. The inherent susceptibility of therapeutic peptides to hydrolytic and oxidative degradation necessitates thorough stability profiling. Conformational changes in the peptide, arising from hydrolysis and oxidative degradation, can hinder effective target binding and thereby diminish its capacity to elicit intended downstream effects, leading to reduced efficacy. For synthetic peptides, the most relevant stability testing principles are derived from the parent International Council for Harmonisation (ICH) stability testing guidelines Q1A(R2) and Q5C [1,2]. This study investigated the intrinsic degradation pathways of terlipressin under systematically varied stress conditions, including acidic, basic, neutral, and oxidative (H₂O₂) exposure at room temperature. Terlipressin exhibited sensitivity across all tested conditions, yielding a total of eleven distinct degradation products (DPs). To facilitate the separation of these DPs, a gradient reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed utilizing an XSelect® CSH™ C18 (130 Å, 2.5 µm, 4.6 × 150 mm) column. The analytical assay method was validated according to ICH Q2(R1) guidelines. The intramolecular disulfide linkage between two cysteine residues presented a challenge for DP characterization. To address this, a chemical reduction strategy employing dithiothreitol (DTT) was integrated with ultra-high performance liquid chromatography-high resolution tandem mass spectrometry (UHPLC-HRMS/MS). This approach enabled the successful elucidation of the eleven DPs, revealing modifications such as truncation, deamidation, acetylation, and oxidation. The characterized fragmentation patterns and identified degradation products provide fundamental insights into the stability behavior of disulfide-containing therapeutic peptides, directly contributing to rational formulation design and development.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144300866","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 a reference material for simultaneous quantitative determination of multiple veterinary drug residues.","authors":"Cheng Ma, Chengping Wu, Yunhua Gao, Lianhua Dong, Jiayi Yang, Hailan Chen","doi":"10.1007/s00216-025-05952-7","DOIUrl":"https://doi.org/10.1007/s00216-025-05952-7","url":null,"abstract":"<p><p>Excessive use of multiple veterinary drugs can lead to the accumulation of residues in food derived from animals, thereby posing potential risks to human health and the environment. Accurate quantification of residues from multiple veterinary drugs is essential for ensuring effective monitoring and regulatory compliance. In this study, a robust high-performance liquid chromatography coupled with diode array detection (HPLC-DAD) method was developed for the simultaneous determination of six veterinary drug residues, including florfenicol (FF), thiamphenicol (TAP), difloxacin (DIF), sulfadimidine (SDM), trimethoprim (TMP), and fenvalerate (FEN). This method was subsequently applied to quantify the multiple veterinary reference material (MVRM). Using the MVRM with assigned values, the varying performance of pre-treatment methods for multiple veterinary drugs in meat samples was evaluated, which may result in differing quantitative outcomes. The application of MVRM is helpful for ensuring food safety and safeguarding human health.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144300863","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":"Characterization of endogenous SUMOylation sites by click chemistry-based proteomics.","authors":"Ke Ma, Sixian Chen, Jun Zhang, Xinglong Jia, Rufeng Fan, Mingjun Li, Li Dong, Minjia Tan, Wensi Zhao, Dong Xie","doi":"10.1007/s00216-025-05957-2","DOIUrl":"https://doi.org/10.1007/s00216-025-05957-2","url":null,"abstract":"<p><p>SUMOylation, an essential ubiquitin-like modification in eukaryotes, plays vital roles in both physiological and pathological regulation, positioning it as a promising therapeutic target. However, the low abundance of SUMOylation and the high enzymatic activity of sentrin/SUMO-specific proteases (SENPs) complicate the identification of endogenous sites. In this study, we integrated click chemistry, acid cleavage, and SUMOylated peptide enrichment into the workflow and developed a promising methodology for system-wide identification of SUMOylation sites. In total, we identified 962 endogenous SUMOylation sites in HEK293T cells under heat shock conditions, which showed good complementarity with previous studies. Our approach uncovered 105 potentially new sites, including SSRP1-K248/K319/K612, DHX9-K806, and ILF3-K241, which showed high conservation and were located in functionally important domains. The overlap between SUMOylation sites and the known ubiquitination or acetylation sites suggested the potential PTM crosstalks. KEGG analysis further suggested SUMOylated proteins were associated with carbon metabolism and biosynthesis of amino acids pathways. Collectively, this study provides a valuable tool for systematically identifying SUMOylation sites, advancing further biological understanding of their dynamic regulatory networks and pathophysiological mechanisms.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144300862","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":"Direct detection of CRISPR-Cas9 ribonucleoprotein gene doping using RNA immunoprecipitation and quantitative PCR.","authors":"Kentaro Akiyama, Atsushi Momobayashi, Masato Okano","doi":"10.1007/s00216-025-05959-0","DOIUrl":"https://doi.org/10.1007/s00216-025-05959-0","url":null,"abstract":"<p><p>Gene doping, using technologies such as CRISPR-Cas9, poses a considerable threat to the integrity of sports. In 2018, the World Anti-Doping Agency implemented a ban on genome editing, which highlighted the need for sensitive and specific detection methods. Detection techniques that are currently available have shown effectiveness in specific contexts, but are limited by low sensitivity and short detection windows. To overcome these limitations, this study presents a new detection method for CRISPR-Cas9 ribonucleoprotein (RNP) complexes, termed RNA immunoprecipitation followed by quantitative PCR (RIP-qPCR). The primary focus of this research was the in vitro development of a detection method targeting genes critical for doping, including myostatin (MSTN), α-actinin 3 (ACTN3), erythropoietin receptor (EPOR), and erythropoietin (EPO), with in vivo proof-of-concept demonstrated using MSTN. The RIP-qPCR method demonstrated sensitive performance, with a limit of quantification of 0.1 ng/mL in plasma. This method successfully detected single guide RNA targeting MSTN, ACTN3, EPOR, and EPO, along with two types of Cas9 proteins in RNP complexes in vitro. Additionally, the detection capabilities of RIP-qPCR were maintained for up to 30 days when plasma samples were stored at 4 °C. In vivo experiments were performed where RNPs were administered via intramuscular and intravenous injections to target the murine Mstn gene. CRISPR-Cas9 RNPs remained detectable for up to 24 h following intramuscular injection and 12 h after intravenous injection. This study underscores the potential of RIP-qPCR as a powerful tool for anti-doping analysis, with future efforts on expanding the target gene panel to enhance the detection of gene editing in sports doping.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144300864","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":"Examining the effects of analytical replication on data quality in a non-targeted analysis experiment.","authors":"Troy M Ferland, Heather D Whitehead, Timothy J Buckley, Alex Chao, Jeffrey M Minucci, E Tyler Carr, Greg Janesch, Safia Rizwan, Nathaniel Charest, Antony J Williams, James P McCord, Jon R Sobus","doi":"10.1007/s00216-025-05940-x","DOIUrl":"https://doi.org/10.1007/s00216-025-05940-x","url":null,"abstract":"<p><p>Non-targeted analysis (NTA) methods are integral to environmental monitoring given their ability to expand measurable chemical space beyond that of traditional targeted methods. Such vast quantities of NTA data are generated that exhaustive manual review is generally unfeasible. Computational tools facilitate automated data processing, but cannot always distinguish real signals (i.e., originating from a chemical in a sample) from artifacts. Replicate analysis is recommended to aid data review, but as NTA studies become larger, the cost of analytical replication becomes untenable. A need therefore exists for examination of information penalties associated with reduced replication. To investigate this issue, using an existing NTA dataset, we performed over 70,000 simulations of variable replication designs and calculated false discovery rates (FDRs) and false negative rates (FNRs) for NTA features and occurrences. We used regression models to explore associations between replication percentage and FDR/FNR, and to test whether rates were affected by NTA feature attributes. Inverse relationships were generally observed between replication percentage and FDR/FNR, such that lower replication yielded higher information penalties. Significant increases in FDR/FNR were observed for suspected per- and polyfluoroalkyl substances (PFAS) compared to non-PFAS, highlighting the potential for differences in information penalties across feature groups. Specific quantitative information penalties are expected to be unique for each NTA study based on sample type and workflow. The methods presented here can support future pilot-scale investigations that will inform the required level of replication in full-scale studies.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-06-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144293161","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":"Multi-residue environmental method for seed treatment insecticides, neonicotinoid degradation products, and fungicides using liquid chromatography tandem mass spectrometry with a new ionization source.","authors":"Jascika A A Maclean, Shannon Bartelt-Hunt, Joyce Cristale, Sathaporn Onanong, Daniel D Snow","doi":"10.1007/s00216-025-05927-8","DOIUrl":"https://doi.org/10.1007/s00216-025-05927-8","url":null,"abstract":"<p><p>Few methods provide simultaneous determination of multiple pesticides and degradation products in environmental samples using liquid chromatography tandem mass spectrometry (LC-MS/MS). As LC-MS/MS method performance is significantly influenced by the type and design of the ion source, we compared three ion sources: electrospray ionization (ESI) source, atmospheric pressure chemical ionization (APCI) source and UniSpray™ ionization source. A gain in sensitivity was observed with UniSpray™ and ESI as compared to APCI source on the same instrument. Matrix effects in the three interfaces were evaluated in reagent water and wastewater extracts. UniSpray™ showed the lowest matrix effect among the three sources, with APCI exhibiting more pronounced signal enhancement. A solid-phase extraction method using the UniSpray™ source provides method detection limits (MDLs) ranging from 0.00189 to 0.0209 µg/L in extracts from water samples. Recoveries in water ranged up to 94.35%, with above 60% of the pesticides having an average recovery exceeding 70%.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-06-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144281931","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":"Quantitative determination and validation of 96 pesticides in cannabis by LC-MS/MS and GC-MS/MS.","authors":"D A MacKenzie, A M Anyanwu, G McRae, J E Melanson","doi":"10.1007/s00216-025-05918-9","DOIUrl":"https://doi.org/10.1007/s00216-025-05918-9","url":null,"abstract":"<p><p>Canada has established a strict set of testing requirements for pesticides that are unauthorized for use on cannabis, currently holding the most extensive list of analytes in North America to date, listing minimum method performance limits rather than maximum allowable concentration limits. These requirements establish the need for validated analytical methods capable of quantifying pesticides and growth regulators in highly variable cannabis inflorescence prior to distribution and sale. We have developed quantitative LC-MS/MS and GC-MS/MS methods capable of quantifying the 96 pesticides unauthorized in Canada for use on cannabis in dried cannabis flower and hemp. Herein, we report the validation results for linearity, precision, within- and between-sample accuracy, recovery, ion suppression, and limits of quantitation in dried cannabis inflorescence. Accuracy is evaluated in 10 cultivars varying in major cannabinoid content as well as ground whole-plant hemp to demonstrate method performance over a range of sample types. Results of the application of the current method to six cannabis samples seized from illegal storefronts by the Ontario Provincial Police are also reported.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-06-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144265003","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}