Analytical and Bioanalytical Chemistry最新文献

{"title":"Assessment of in-house reference materials for multi-pesticide residue analysis in three food matrices by LC–MS/MS: development, homogeneity, and stability","authors":"Andrés S. Salinas,&nbsp;Yeraldin Aguilar,&nbsp;Laura V. Morales,&nbsp;Diego A. Ahumada","doi":"10.1007/s00216-025-05826-y","DOIUrl":"10.1007/s00216-025-05826-y","url":null,"abstract":"<div><p>In-house reference materials (ihRM) are an alternative to the limited supply of reference materials for method validation and assurance of the validity of pesticide residue results. Currently, limited information exists on producing ihRM of pesticide residues in food for laboratory testing purposes for the desired matrix/analyte/concentration combination. This study aimed to develop in-house reference materials for three food matrices: banana, rice, and green coffee spiked with a total of 22 pesticides, which were selected for their relevance in food matrices, with pK_OW values ranging from −0.13 to 5.8 following the guidelines of ISO Guide 80:2014. In this study, we assessed the impact of spiking (solvent) and drying conditions (freeze-dried and oven) on homogeneity uncertainty. The final step of this work involved evaluating the homogeneity and kinetics for long-term stability (4 °C) according to the ISO 33405 guidelines, using a fully validated method based on QuEChERS and measurement by LC–MS/MS through a completely randomized block design with two-way ANOVA, and simple linear regression analysis for homogeneity and stability, respectively. In general, for the three matrices, it was found that using a predominantly aqueous solvent (&gt;70%) and freeze-drying resulted in sufficient homogeneity and no significant processing trends (slope <i>p</i>-value &gt; 0.05), compared to using an organic medium (&gt;70%), which resulted in uncertainties up to 50 times higher for several analytes. On the other hand, uncertainties for long-term stability below 3% were obtained for most of the analytes at 4 °C. The results demonstrate that homogeneous and stable ihRMs can be obtained under the provided preparation conditions, although special attention is required for processing conditions, particularly for the banana at a larger scale.</p><h3>Graphical abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":"417 12","pages":"2727 - 2739"},"PeriodicalIF":3.8,"publicationDate":"2025-03-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143612955","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":"Certified reference material for inorganic contaminants in insect protein","authors":"Fransiska Dewi,&nbsp;Lay Peng Sim,&nbsp;Sin Yee Ng,&nbsp;Ho Wah Leung,&nbsp;Wan Ting Ng,&nbsp;Richard Y. C. Shin,&nbsp;Zoltan Mester,&nbsp;Tang Lin Teo","doi":"10.1007/s00216-025-05815-1","DOIUrl":"10.1007/s00216-025-05815-1","url":null,"abstract":"<div><p>The growing interest in insect protein as an alternative to conventional protein sources is driven by the need for sustainable options with low environmental impact. While insect-based proteins provide significant nutritional benefits, ensuring their safety requires robust analytical methods and access to reliable matrix-matched certified reference materials. Currently, the availability of such materials for assessing inorganic and organic contaminants in insect proteins is limited. This paper outlines the innovative methodologies used to produce an incurred cricket powder reference material for inorganic contaminants (arsenic, cadmium, chromium, mercury, lead, arsenic species) and selenium. It details the careful selection of appropriate contaminant levels introduced through insect feed, feeding regimens, and the production of a certified reference material in compliance with ISO 17034 standard. In the development of the material, a pioneering approach was adopted, integrating tailored feed formulations for insects within controlled farming environments. Through meticulous trials, these techniques achieved satisfactory bioaccumulation of contaminants, enabling the consistent production of high-quality incurred insect protein suitable for use as quality control samples and for method development and validation of methods. The assignment of reference values for these materials was carried out using high-accuracy methods, ensuring metrological traceability with associated measurement uncertainties. The scarcity of insect-based reference materials has posed a challenge to guaranteeing the safety and quality of insect-based proteins. Hence, the development of these reference materials plays a crucial role in instilling confidence among consumers and regulatory bodies in the evolving landscape of the insect protein industry.</p><h3>Graphical Abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":"417 12","pages":"2703 - 2715"},"PeriodicalIF":3.8,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143595975","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":"Accuracy, linearity, and statistical differences in comparative quantification in untargeted plant metabolomics using LC-ESI-Orbitrap-MS.","authors":"Christina Maisl, Rainer Schuhmacher, Christoph Bueschl","doi":"10.1007/s00216-025-05818-y","DOIUrl":"https://doi.org/10.1007/s00216-025-05818-y","url":null,"abstract":"<p><p>High-resolution mass spectrometers, particularly when paired with liquid chromatography, are the instrument of choice for untargeted metabolomics approaches. Instruments, such as the Orbitrap, offer high sensitivity, selectivity, and exceptional mass accuracy, though they pose certain technical challenges, complicating absolute and comparative quantification. Consequently, method validation is crucial to ensure reliable results, as untargeted metabolomics approaches require the detection and quantification of a large number of metabolites in a broad dynamic range. Methods can be assessed using performance characteristics like accuracy and linearity to ensure analytical reliability. This study evaluates the suitability of untargeted metabolomics methods for discovery-based investigations. A stable isotope-assisted strategy was used with wheat extracts analyzed by a Q Exactive HF Orbitrap. Results showed that 70% of all detected 1327 metabolites displayed non-linear effects in at least one of the nine dilution levels employed. However, when considering fewer levels, 47% of all metabolites demonstrated linear behavior in at least four levels (i.e., a difference factor of 8). Moreover, the analysis further suggests that the observed abundances in less concentrated samples and those outside the linear range were mostly overestimated compared to expected abundances, but hardly ever underestimated. Consequently, during statistical analysis, which is an important step in prioritizing detected metabolites and correlating them with the biological hypothesis, the number of false-positives was not inflated, but the number of false-negatives might be increased. Generally, (non-)linear behavior did not correlate with specific compound classes or polarity, suggesting non-linearity is not easily predictable based on chemical structures.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143595961","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":"Towards quality-assured measurements of microplastics in soil using fluorescence microscopy.","authors":"Quynh Nhu Phan Le, Crispin Halsall, Stoyana Peneva, Olivia Wrigley, Melanie Braun, Wulf Amelung, Lorna Ashton, Ben W J Surridge, John Quinton","doi":"10.1007/s00216-025-05810-6","DOIUrl":"https://doi.org/10.1007/s00216-025-05810-6","url":null,"abstract":"<p><p>Fluorescence microscopy is increasingly seen as a fast, user-friendly, and high-throughput method for detecting microplastics (MPs) in soil; however, its effectiveness across diverse MP types and soil properties remains underexplored. This study tested a fluorescence microscopy-Nile red (NR) staining approach on eight MP types, covering both biodegradable and non-biodegradable plastics, in three size ranges (≤ 150 µm, 100-250 µm, 500-1000 µm) across loamy, clayey, and sandy soils. Each sample, processed in triplicate, underwent a relatively quick and straightforward extraction procedure involving density separation, organic digestion, and NR staining, followed by fluorescence and bright-field microscopy. A new digital image analysis pipeline using Image J was developed to expedite and (semi)automate MP quantification. Recoveries ranged from 80% to 90% for MPs with a Feret diameter of 500-1000 µm, regardless of soil type. In contrast, the recovery of smaller MPs (Feret dia. ≤ 250 µm) varied depending on the soils and plastic types: recoveries for low-density polyethylene (LDPE) reached 85% in sandy soil and 90% in loamy soil, whereas those for biodegradable polybutylene adipate terephthalate/polylactic acid (PBAT/PLA) were only 60% and 10%, respectively. The lowest recovery rate was observed in clayey soil and for biodegradable plastics. The method was tested on non-agricultural soil samples, yielding a MP mean number concentration of 20.7 ± 9.0 MPs/g for MPs sized from dia. ≥ 25 µm, comparable to Fourier transform infrared (FPA-µ-FTIR) results of 13.1 ± 7.3 MPs/g (p > 0.05). We conclude that fluorescence microscopy with NR staining and automated particle quantification offers a time-efficient, reproducible, and accurate method for MP detection in light-textured soils, whereas limitations remain for reliable MP analysis in clay-dominated soils.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143584211","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":"A dual-mode RNA-splitting aptamer biosensor for sensitive HIV Tat peptide detection via colorimetry and fluorescence.","authors":"Rui Huang, Li-Kang Yin, Can Yang, Ze-Lin Wang, Rui-Min Ni, Han-Ying Zhan, Zhi-Qi Zhang","doi":"10.1007/s00216-025-05823-1","DOIUrl":"https://doi.org/10.1007/s00216-025-05823-1","url":null,"abstract":"<p><p>Early diagnosis of human immunodeficiency virus (HIV) is critical for effective treatment; however, traditional antibody methods encounter challenges during the infection window, and nucleic acid tests require specialized equipment. In this study, a dual-mode ribonucleic acid (RNA)-splitting aptamer biosensor was developed to target the HIV trans-activator of transcription (Tat) protein, a key HIV biomarker for viral replication throughout the infection cycle. The biosensor integrates colorimetric and fluorescent detection techniques by utilizing gold nanoparticles (AuNPs) and two types of aptamers, one labeled with carboxyfluorescein (FAM). In the presence of Tat, RNA-splitting aptamers adsorb onto AuNPs, protecting them from recombination, while the fluorescence of FAM is quenched via fluorescence resonance energy transfer (FRET). Aptamers form a ternary complex with Tat, preventing adsorption and leading to thioflavin T-induced aggregation of AuNPs, accompanied by a visible color change and fluorescence signal restoration. The biosensor demonstrated excellent sensing performance, with a linear range of 0.5-60 nM and a detection limit of 0.28 nM, successfully detecting Tat in human serum. Therefore, this low-cost dual-mode detection platform offers a promising tool for early HIV diagnosis and potential applications in clinical and point-of-care fields.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143584236","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":"SI-traceable characterisation of the first reference material for nanoparticle number concentration in suspension to support regulatory compliance","authors":"Dorota Bartczak,&nbsp;Susana Cuello Nuñez,&nbsp;Ada Kubicka,&nbsp;David Ojeda,&nbsp;Armando Sanchez Cachero,&nbsp;Simon Cowen,&nbsp;Stephen Ellison,&nbsp;Gill Holcombe,&nbsp;Heidi Goenaga-Infante","doi":"10.1007/s00216-025-05789-0","DOIUrl":"10.1007/s00216-025-05789-0","url":null,"abstract":"<div><p>Reference materials (RMs) are increasingly needed to support number-based characterisation of nanomaterials (NM) in a regulatory context for the purpose of method development, validation and measurement quality control. To date, RMs for number concentration in suspension with a directly assigned value that is SI traceable have been rather scarce, being the LGCQC5050 the only material commercialised so far. This could be attributed to the limited availability of metrologically validated measurement methods and stability challenges associated with long-term storage of NM suspensions. This paper describes development and characterisation of the first RM consisting of 30-nm colloidal gold nanoparticles and value assigned for particle number concentration using the dynamic mass flow (DMF) method with single particle ICP-MS (spICP-MS). Special attention is paid to systematic assessment of the DMF method’s performance under operating conditions set outside recommendations described in ISO/TS 19590:2024, but that still comply with key requirements of this method (e.g. use of an ICP-MS system in equilibrium, a cooled spray chamber, etc.). The results of such investigations are reported here for the first time. The paper also discusses practical considerations for the production, storage and transport of nano RMs, and provides guidance on best practice for the production and certification of future nano RMs in accordance with ISO 17034:2016.</p><h3>Graphical abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":"417 12","pages":"2655 - 2667"},"PeriodicalIF":3.8,"publicationDate":"2025-03-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143584242","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":"Application of separation and configuration identification of the four tetrabenazine stereoisomers in determining their pharmacokinetics.","authors":"Jianxin Li, Haoran Li, Kai Liu, Alan Kueichieh Chang, Ying Pei, Wenbao Liu, Jiao Ai, Nan Wang, Yuhui Liu, Zhen Jiang, Lijiang Chen, Xiao Liang","doi":"10.1007/s00216-025-05813-3","DOIUrl":"https://doi.org/10.1007/s00216-025-05813-3","url":null,"abstract":"<p><p>Tetrabenazine (TBZ) is used in the treatment of psychiatric diseases, and it works by inhibiting vesicular monoamine transporter 2 (VMAT2) protein to exert a curative effect. TBZ is administered as the mixture of stereoisomers in clinical treatment. TBZ has two chiral centers, and therefore, it has four stereoisomers, and this greatly makes it difficult to separate the stereoisomers and to identify their configurations because of their high susceptibility to structural transformation. This study aims to develop a method to resolve TBZ into four individual peaks, corresponding to the four stereoisomers (1-4). Based on the different binding affinities between TBZ stereoisomers and VMAT2, the UF-UHPLC-QQQ/MS method is used to determine the absolute configuration of TBZ stereoisomers 1 and 2. Molecular docking simulations are used to verify the accuracy of UF-UHPLC-QQQ/MS. The configurations of stable stereoisomers 3 and 4 were confirmed by electron circular dichroism (ECD). The established analytical method was applied to determine the pharmacokinetics of each TBZ stereoisomer in vivo. It was found that the stereoisomer 1 (3R,11bR-TBZ) showed better bioavailability and more excretion than the other stereoisomers. The results of tissue distribution experiments indicated a much higher content of 3R,11bR-TBZ in the brain, suggesting that it may better penetrate the blood-brain barrier and exert its therapeutic effects there. The paper addresses the complex problem of separating and identifying stereoisomers with multiple chiral centers, which is a significant challenge in pharmaceutical chemistry. And this work could provide a basis for the preparation of TBZ stereoisomers and a reference for the method of separating drugs with multichiral centers and identifying unstable drugs based on their configurations.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143584239","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":"Predicting bone aging using spatially offset Raman spectroscopy: a longitudinal analysis on mice.","authors":"Hongmei Dou, Wendong Sun, Shuo Chen, Keren Chen","doi":"10.1007/s00216-025-05819-x","DOIUrl":"https://doi.org/10.1007/s00216-025-05819-x","url":null,"abstract":"<p><p>Osteoporosis, a global health concern, poses an increasing challenge due to the aging population. While dual-energy X-ray absorptiometry (DXA) scans measuring bone mineral density (BMD) remain the clinical standard for osteoporosis diagnosis, this method's inability to detect changes in bone chemical composition limits its effectiveness in early diagnosis. This study applies Raman spectroscopy on examining bone aging in Senescence Accelerated Mouse Prone 6 (SAMP6) mice compared to their senescence-resistant controls (SAMR1) over an age period from 6 to 10 months. We performed Raman spectroscopic analysis on mouse tibiae both transcutaneously and on exposed bone. Leave-one-out cross-validation combined with partial least squares regression (LOOCV-PLSR) was applied to analyze Raman spectra to predict age, BMD, and maximum torque (MT) as determined by biomechanical testing. Our results revealed significant correlations between Raman spectroscopic predictions and reference values, particularly for age determination. To our knowledge, this study represents the first demonstration of transcutaneous Raman spectroscopy for accurate bone aging prediction, showing a strong correlation with established reference measurements.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-03-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143571871","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: Robust discrimination between closely related species of salmon based on DNA fragments","authors":"Debra Ellisor,&nbsp;Mary Gregg,&nbsp;Angela Folz,&nbsp;Antonio Possolo","doi":"10.1007/s00216-025-05800-8","DOIUrl":"10.1007/s00216-025-05800-8","url":null,"abstract":"","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":"417 12","pages":"2749 - 2750"},"PeriodicalIF":3.8,"publicationDate":"2025-03-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s00216-025-05800-8.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143565580","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 of amyloid β (1–42) certified reference material NMIJ CRM 6210-a","authors":"Kazumi Saikusa,&nbsp;Tomoya Kinumi,&nbsp;Megumi Kato","doi":"10.1007/s00216-025-05797-0","DOIUrl":"10.1007/s00216-025-05797-0","url":null,"abstract":"<div><p>Amyloid β is a well-known peptide biomarker for Alzheimer’s disease. Various methods for amyloid β such as immunological assays have been reported. It is important to establish metrological traceability using a certified reference material (CRM) at the highest level in the calibration hierarchy to assess equivalence of measured values obtained from each method. Herein, we developed a CRM for amyloid β, named as NMIJ CRM 6210-a, with a concentration traceable to the International System of Units (SI). This CRM comprises a lyophilized synthetic peptide with a human amyloid β (1–42) sequence (hereafter, amyloid β) and includes oxidated, deamidated, and isomerized forms of amyloid β. Two certified values were assigned for the mass concentration of total amyloid β (a mixture of amyloid β and its oxidized, deamidated, and isomerized forms) and amyloid β, determined via amino acid analyses with two different hydrolysis methods with different liquid chromatography mass spectrometry methods coupled to isotope-dilution mass spectrometry on the reconstituted solution of the candidate material with (1.00 <span>(pm)</span> 0.01) g of 0.1% ammonia aqueous solution. The quantitative results obtained from amino acid analyses were converted into mass concentration using the density and molar mass, resulting in certified values of (46 <span>(pm)</span> 11) mg/L for total amyloid β and (42.6 <span>(pm)</span> 7.0) mg/L for amyloid β, respectively. The amyloid β content in total amyloid β was determined by calculating the relative area percentage using liquid chromatography with ultraviolet detection. Furthermore, the storage stability of this CRM was evaluated along with its stability in use, both of which were shown to be stable.</p><h3>Graphical Abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":"417 12","pages":"2679 - 2689"},"PeriodicalIF":3.8,"publicationDate":"2025-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143555527","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}