Analytical and Bioanalytical Chemistry最新文献

{"title":"Process intensification of the chemical recovery in the pulp and paper industry using Raman spectroscopy.","authors":"M Eisenköck, A K Schwaiger, G Ramer, B Lendl, K Wieland","doi":"10.1007/s00216-025-06015-7","DOIUrl":"https://doi.org/10.1007/s00216-025-06015-7","url":null,"abstract":"<p><p>The pulp and paper industry is an active player in the European bio-economy producing wood-based, biodegradable material. The recovery of chemicals spent in the cooking step separating cellulose from the lignocellulosic biomass is a key step towards circular processing. However, seasonally varying input streams, complex chemical composition, and intricate interaction between gas and liquid phase result in precipitation of insoluble salts. As a result, clogged pipes lead to unscheduled downtimes as well as loss in valuable chemicals, challenging the economic feasibility and ecological footprint of the process. Here, Raman spectroscopy is used as a non-destructive, in situ process monitoring tool, to help deepen the understanding of the chemical interplay occurring in the chemical recovery process. In combination with multivariate regression models based on several hundred reference spectra, the spectral fingerprint is translated into critical process-relevant parameters. A workflow to set up such a multivariate model in industrial environment is shown and successful test-wise online implementation at the plant in Gratkorn, Austria, is demonstrated. Continuous monitoring allows tight process control of the interaction between gas and liquid phase. Hence, effects due to e.g. seasonally varying input streams resulting in varying chemical composition may be corrected or avoided by timely countermeasures, overall reducing unscheduled downtimes and loss of valuable chemicals.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144666762","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":"Particulate vs monolithic aerogel linings in capillaries for Raman signal gain of aqueous solutions.","authors":"Felix Spiske, Andreas Siegfried Braeuer","doi":"10.1007/s00216-025-06008-6","DOIUrl":"https://doi.org/10.1007/s00216-025-06008-6","url":null,"abstract":"<p><p>We compare particulate versus monolithic silica aerogel-lined capillaries as liquid core waveguides for Raman signal gain of liquid aqueous samples. The manufacturing process of monolithic linings, which aims to address the limited robustness of particulate aerogel linings, is discussed in detail and compared with that of particulate linings. The linings of both capillary types are characterized using scanning electron microscopy. Raman signal gain of pure water and aqueous solutions is evaluated for each type. The aqueous solutions are samples drawn at different times from the oxidative conversion of glycerol to formic acid (OxFA process). It is analyzed whether the Raman signal gain provided by aerogel-lined capillaries is affected by the property changes in this exemplary industrial process caused by the ongoing chemical reaction. Finally, the mechanical robustness of the linings and the stability of the Raman signal gain are tested under rapid and repeated capillary purge in both types.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144666761","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":"Non-invasive assessment of free steroid hormones: development of a high-throughput LC-MS/MS method for salivary steroid hormone quantification.","authors":"Tove Slettvoll, Jeanette Wahlberg, Yvonne Lood, Martin Josefsson, Elisabeth Aardal, Samira Salihovic","doi":"10.1007/s00216-025-06005-9","DOIUrl":"https://doi.org/10.1007/s00216-025-06005-9","url":null,"abstract":"<p><p>Steroid hormone concentrations reflect diverse physiological and pathological processes and have been recognized as valuable biomarkers for disease, with growing interest in their potential for patient stratification in precision medicine. Salivary steroid concentrations should reflect the free (biologically active) steroids in circulation, as steroids in the bloodstream passively diffuse to saliva. This allows for the direct measurement of free steroids without transporter protein-bound hormones (inactive form). However, implementation of salivary steroid quantification in larger studies remains limited by challenges associated with sample preparation. We began by reviewing the literature on relevant sample preparation approaches and identified commonly used 96-well solid phase extraction (SPE) methods for further evaluation. Three sample preparation methods were selected and assessed in terms of internal standard recovery and matrix effects, and their response was also compared using electrospray (ESI) versus UniSpray ionization (USI) liquid chromatography-tandem mass spectrometry (LC-MS/MS). We demonstrate a sensitive and rapid high-throughput method with Oasis HLB µElution SPE of 200 μL saliva in 96-well format and USI-LC-MS/MS for major steroids (testosterone, androstenedione, cortisone, cortisol, and progesterone) in saliva. The method achieved optimal recovery (77%), matrix effects (33%), and sensitivity with detection limits (MDL) ranging between 1.1 and 3.0 pg/mL and linearity (r² = 0.99). Intra-plate and inter-plate coefficient of variation (CV) was below 7% and 20% using USI. USI provided a higher (2.0-2.8-fold) response than ESI and higher signal-to-noise ratio (S/N). The method was then applied to 97 authentic saliva samples (41 male and 56 female) and significant correlations between age and BMI, and androgen levels were observed in both sexes. The proposed 96-well SPE USI-LC-MS/MS method is well-suited for determining steroid hormones in saliva with potential usefulness in large-scale studies and clinical settings.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144666760","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":"Quantification of parathyroid hormone in high-purity materials by two isotope dilution mass spectrometry methods.","authors":"Jiahui Li, Jingkang Li, Ming Li, Pinyi Ma, Daqian Song, Qiang Fei","doi":"10.1007/s00216-025-06007-7","DOIUrl":"https://doi.org/10.1007/s00216-025-06007-7","url":null,"abstract":"<p><p>In clinical practice, the measurement of parathyroid hormone (PTH) typically employs immunoassays, but these methods lack comparability of results due to variations in specificity or calibration. Consequently, there is a clear need to establish a highly accurate and comparable procedure for a PTH calibrator. Purity assessment for a high-purity material is a prerequisite for the standardization of PTH assay. The present study proposes an accurate quantitative method for PTH purity in high-purity materials, integrating amino acid (AA) and peptide analysis for quantitative purposes. In the beginning, a liquid chromatography mass spectrometry (LC-MS) analysis was performed to confirm its molecular weight and AA sequence. Subsequently, three quantitative AAs were selected for accurate quantification of PTH by amino acid isotope dilution mass spectrometry (AA-IDMS). Finally, in peptide-IDMS, peptide ADVNVLTK (AK) was selected as the quantitative peptide to quantify PTH. The results of the two IDMS quantification methods exhibited strong concordance, with both exhibiting minimal uncertainty. The final mass fraction of PTH in the study material was calculated to be 0.718 ± 0.022 g/g. The method developed in this study provides novel technical support and theoretical foundations for the quality assessment and quality standard formulation of PTH-related products. It has great application potential in the purity determination of other bioactive substances with similar properties as PTH, and would promote the development of the field of bioanalysis.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144648158","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-channel high-sensitivity oxidation colorimetric array based on HAuCl₄ for pesticide detection.","authors":"Yalong Pan, Lijun Han, Junxue Shen, Jing Li, Taolei Sun, Yao Yu","doi":"10.1007/s00216-025-06010-y","DOIUrl":"https://doi.org/10.1007/s00216-025-06010-y","url":null,"abstract":"<p><p>Pesticide contamination is a global challenge, threatening agricultural production and environmental safety. To address the urgent need for efficient and reliable pesticide detection methods, we developed a novel multi-channel colorimetric sensor array based on HAuCl₄-mediated oxidation reactions. This innovative system incorporates six distinct colorimetric channels coupled with advanced multivariate statistical analysis, enabling simultaneous detection and discrimination of multiple pesticide residues. Through systematic optimization of key reaction parameters, the developed sensor improved selectivity and classification accuracy, particularly for structurally similar pesticides. The platform successfully identifies 11 different classes of pesticides and distinguishes five specific pesticides across various concentration levels. This approach overcomes the limitations of traditional single-target detection methods by employing multi-parameter analysis for accurate pesticide identification. Notably, the proposed method offers several practical advantages, including simple operation, rapid detection (within 30 min), high sensitivity (detection limits of 6 μg/mL), and cost-effectiveness by eliminating the need for expensive instrumentation. These features make the developed sensor array particularly suitable for on-site pesticide screening and food safety monitoring applications.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144648147","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":"Publisher Correction: Direct detection of CRISPR-Cas9 ribonucleoprotein gene doping using RNA immunoprecipitation and quantitative PCR.","authors":"Kentaro Akiyama, Atsushi Momobayashi, Masato Okano","doi":"10.1007/s00216-025-06004-w","DOIUrl":"10.1007/s00216-025-06004-w","url":null,"abstract":"","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-07-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144641418","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 and validation of a non-chromatographic method for mercury and methylmercury in finfish using thermal decomposition gold amalgamation atomic absorption spectrophotometry (TDA-AAS) and salting-out assisted liquid-liquid extraction (SALLE).","authors":"Jake A Carter, Charles A Barber, Mesay M Wolle, Patrick J Gray","doi":"10.1007/s00216-025-05989-8","DOIUrl":"https://doi.org/10.1007/s00216-025-05989-8","url":null,"abstract":"<p><p>Accurate technologies and methods are needed to monitor both total and methylmercury in the marine food supply. Thermal decomposition gold amalgamation atomic absorption spectrophotometry (TDA-AAS) is an efficient and cost-effective technique for measuring low levels of total mercury requiring no sample preparation. Measuring methylmercury with TDA-AAS requires isolating methylmercury from the matrix and other mercury species prior to detection. We developed a method that uses ethyl acetate instead of a legacy non-polar solvent, toluene. Toluene is a potentially hazardous and problematic solvent whereas ethyl acetate is greener and safer. Additionally, the salting-out assisted liquid-liquid extraction (SALLE) approach with ethyl acetate avoids emulsion formation throughout extraction. We describe method development and validation of a SALLE and TDA-AAS detection for methylmercury in finfish. From 10 reference materials, our method recovered 80-118% of total or methylmercury with Z scores ranging from -1.98 to 2.75 (n = 184). The LOD and LOQ of the method for methylmercury were 3.8 and 27 ng/g, respectively. From extraction to detection, accurate results were obtained from a sample in less than 2 h for both total mercury and methylmercury.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-07-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144648146","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":"Sensitive electrochemical sensor based on hybrid material F-doped carbon quantum dots (Cdots) and NiO nanoparticles: detection of ketoconazole in pharmaceutical formulations and tap water samples.","authors":"Carolina Meneses Dos Santos, Francisco Walison Lima Silva, Octávio P L de Souza, Thiago C Canevari, Ricardo Erthal Santelli, Vivian M Saez, Fernando Henrique Cincotto","doi":"10.1007/s00216-025-06002-y","DOIUrl":"https://doi.org/10.1007/s00216-025-06002-y","url":null,"abstract":"<p><p>This study presents a novel electrochemical sensor for ketoconazole determination, developed using an advanced hybrid material composed of fluorine-doped carbon quantum dots (F-Cdots) and nickel oxide nanoparticles (NiONPs) to modify a glassy carbon electrode (GCE). The redox behavior of the modified electrode was evaluated using cyclic voltammetry, revealing an irreversible oxidation peak at 0.59 V, associated with the transfer of a single electron. The modified sensor exhibited a performance approximately 50% higher than that of the unmodified GCE. Square wave voltammetry was optimized for quantification, with the best results obtained in 0.1 M phosphate buffer solution (PBS) at pH 9. The sensor exhibited a low detection limit of 7.12 nmol L⁻¹ and a quantification limit of 23.49 nmol L⁻¹. A strong linear response (r = 0.999) was observed over a ketoconazole concentration range from 0.037 to 11.13 µmol L⁻¹. Its wide linear range represents a key advantage, increasing practical applicability and versatility in various analytical scenarios compared to previous methods. The sensor was successfully applied to pharmaceutical formulations and tap water samples, achieving recovery rates between 88.8 and 103.6%. Furthermore, it demonstrated minimal interference from other compounds, highlighting its high selectivity and robustness for real applications in pharmaceutical quality control and environmental monitoring.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-07-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144635871","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":"Enzyme-induced fluorescence signal-on for specific detection of alkaline phosphatase and imaging in live cells.","authors":"Zhifeng Wang, Yu Huang, Ke Pei, Tingting Feng","doi":"10.1007/s00216-025-06003-x","DOIUrl":"https://doi.org/10.1007/s00216-025-06003-x","url":null,"abstract":"<p><p>A highly sensitive and stable fluorescent strategy for detecting alkaline phosphatase (ALP) in complex samples was developed using oxidized single-walled carbon nanohorns (oxSWCNHs) and exonuclease I (Exo I). A ssDNA probe, comprising a fluorophore-labeled aptamer and a 3' phosphate group, was designed and synthesized. In the absence of ALP, the ssDNA probe binds to oxSWCNHs, causing fluorescence quenching. When ALP is present, it removes the 3' phosphate group from the ssDNA, releasing a free 3'-OH group. The dephosphorylated ssDNA is then hydrolyzed by Exo I, generating a single base and FAM, which cannot bind to oxSWCNHs, resulting in enhanced fluorescence of the system. This strategy was successfully applied to image hepatocytes, showing the potential of our sensing system for ALP bioimaging in living cells. The method has good selectivity and high sensitivity under optimized experimental conditions, with a detection limit of 0.4 mU/mL and a range of 0.5-50 mU/mL. Additionally, it was used to study the inhibitory effects of Na₃VO₄. This method has great potential for the quantitative detection of ALP in clinical diagnostics.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144625110","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":"Characterizing cyanopeptides and transformation products in freshwater: integrating targeted, suspect, and non-targeted analysis with in silico modeling.","authors":"Audrey Roy-Lachapelle, Morgan Solliec, Christian Gagnon","doi":"10.1007/s00216-025-05999-6","DOIUrl":"https://doi.org/10.1007/s00216-025-05999-6","url":null,"abstract":"<p><p>Harmful algal blooms (HABs) pose significant risks to environmental and public health, primarily through cyanotoxin production. Influenced by anthropogenic and climatic factors, cyanobacteria require advanced methods for identifying and characterizing their secondary metabolites. This study presents a multi-step approach to investigate the most abundant cyanopeptides in freshwater samples from agricultural and urban areas, aiming to improve their characterization and understand their environmental fate. A targeted method was developed to quantify 28 cyanopeptides across seven families, being one of the most extensive quantitative analyses of cyanopeptides. Significant concentrations of 14 congeners were detected, ranging from 0.038 to 5.68 µg L^-1. A suspect screening method was developed and applied to expand detection, integrating CyanoMetDB and in silico modeling for the prediction of molecular features, increasing confidence in characterization. This approach enabled the identification of 26 uncommon cyanopeptides, including the newly characterized [DMAdda⁵, GluOMe⁶]microcystin-LHty. Additionally, a novel non-targeted analysis method was developed, combining compound class search, in silico modeling, and the enviPath UG & Co KG biotransformation prediction tool. This new strategy led to the identification of seven new transformation products and potential microcystins, including a new dopamine-modified microcystin-YR and the new linear [seco-1/7][Asp³]microcystin-LR. By integrating targeted, suspect, and non-targeted approaches, this study significantly enhanced cyanopeptide detection and characterization, providing valuable insights for environmental monitoring and public health protection.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144615700","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}