Analytical and Bioanalytical Chemistry最新文献

{"title":"A candidate reference measurement procedure for quantification of human insulin in serum based on immunoaffinity extraction and isotope dilution-liquid chromatography-tandem mass spectrometry.","authors":"Huixia Liu, Yanlin Han, Huimin Wang, Yuefeng Zhang, Chunlong Liu, Man Liang","doi":"10.1007/s00216-025-05900-5","DOIUrl":"10.1007/s00216-025-05900-5","url":null,"abstract":"<p><p>Accurate measurement of human insulin is critical for proper diagnosis, monitoring, and treatment of diabetes. But the insulin results of clinical immunoassay are inconsistent mainly due to antibody cross-reactivity. To standardize and ensure the accuracy of clinical assays, reference measurement procedures (RMPs) with higher metrological order are required. An isotope dilution-liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) for quantification of human insulin in serum as a candidate reference measurement procedure (cRMP) was developed and validated. Insulin was enriched from human serum by insulin antibodies immobilized on magnetic beads. The eluent was analyzed by ID-LC-MS/MS. The cRMP separated human insulin from potentially interfering compounds and enabled measurement over a range of 0.05-40 ng/g, with no matrix effects and carryover. The limit of detection (LOD) and the limit of quantitation (LOQ) in serum were 24.6 pg/g and 48.8 pg/g, respectively. Imprecision (intra-assay and inter-assay) was <2.77% at 0.436, 2.003, and 11.449 ng/g. Recoveries ranged from 99.5% to 101.7% at three spiked levels. Extraction recovery was measured at 85% or higher. Insulin analogues caused no interference for the determination of endogenous insulin. Expanded measurement uncertainty of target value-assigned samples was ≤3.5%. The cRMP was applied to measure human insulin in serum and was compared with two immunoassays using 46 serum samples. Also, a discrepancy of three candidate reference materials for the calibration of cRMP was discussed.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3731-3740"},"PeriodicalIF":3.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143955863","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":"Plastic and rubber polymers in urban PM₁₀ by pyrolysis-gas chromatography-mass spectrometry.","authors":"Tatu Martinmäki, Sanna Saarikoski, Hilkka Timonen, Jarkko V Niemi, Markus Sillanpää","doi":"10.1007/s00216-025-05906-z","DOIUrl":"10.1007/s00216-025-05906-z","url":null,"abstract":"<p><p>Microplastics, including tyre and road wear particles, have been detected in every environmental compartment in both urban and remote areas. However, their contribution to atmospheric particulate matter is still sparsely explored. These airborne micro- and nanosized particles are continuously inhaled and pose risks to the environment and public health. The objectives of this study were to develop and validate a thermoanalytical method for the quantification of microplastics in urban particulate matter. Aerosol particles smaller than 10 µm in aerodynamic diameter (PM₁₀) were sampled at the kerbside in Helsinki, Finland, during spring 2024. The samples were pretreated by homogenization and thermal desorption prior to chemical analysis by micro-furnace pyrolysis-gas chromatography-mass spectrometry. The developed method was validated in terms of selectivity, limits of quantification, linear range, trueness, precision, and measurement uncertainty. Instrument quantification levels were 8-270 ng. Expanded measurement uncertainties were 25-30% and 50-70% for the studied tyre wear rubbers and thermoplastics, respectively. Polyethylene, polyethylene terephthalate, polypropylene, polystyrene, and tyre and road wear particles were detected in urban PM₁₀ samples, and their sum accounts for 1-3% of total PM₁₀. These results represent the level of airborne microplastic particles to which people can be exposed in urban environments.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3835-3844"},"PeriodicalIF":3.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12227455/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143957075","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":"Amino acid regulation of peroxidase-like activity of Cu₂O nanozyme for detection of tetracycline antibiotics.","authors":"Yueqiang Wang, Shengwei Sun","doi":"10.1007/s00216-025-05904-1","DOIUrl":"10.1007/s00216-025-05904-1","url":null,"abstract":"<p><p>Tetracycline antibiotics (TCs) are widely used in medicine, agriculture, and animal husbandry. However, their overuse has led to environmental pollution, posing a significant threat to water sources, soil, and food safety. Therefore, there is an urgent need for efficient, sensitive, simple, and low-cost detection methods for environmental pollution monitoring. In this study, the catalytic activity of copper-based nanozymes was regulated by AAs. Lysine, aspartic acid, glycine, and arginine were chosen as ligands to synthesize different copper-based nanozymes. The results showed that the type of amino acid significantly influenced the particle size, morphology, and peroxidase (POD)-like catalytic activity of Cu₂O. Based on these amino acid-regulated Cu₂O nanozymes, we further developed a highly sensitive, easy-to-use, and low-cost colorimetric sensor array that can effectively distinguish TCs. This sensor array was successfully validated in binary mixtures and wastewater environments. This study not only provides important insights into the small-molecule regulation of copper-based nanozyme catalytic performance but also offers a novel approach for the detection of TCs in environmental monitoring.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3813-3823"},"PeriodicalIF":3.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12227342/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143961057","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":"Accounting for shear scission in the size-exclusion chromatography of debranched starch.","authors":"Jihui Zhu, Ziyi Wang, Robert G Gilbert","doi":"10.1007/s00216-025-05917-w","DOIUrl":"10.1007/s00216-025-05917-w","url":null,"abstract":"<p><p>The chain-length distribution (CLD) of starch influences many functional properties of starch-containing substances, and also contains information about starch biosynthetic processes. The commonest method for measuring this CLD is to debranch the starch enzymatically, and then to measure the molecular weight distribution of the resulting linear chains using size-exclusion chromatography (SEC). However, SEC suffers from various artifacts, including shear scission of longer chains. Here, a method of correcting for such shear scission is developed: fitting the apparent CLDs (affected by shear scission) with biosynthesis-based models, over a range of flow rates, and extrapolating the resulting model-based parameters to zero flow rate. To apply this, the apparent CLDs of five rice starches were measured using SEC with a range of flow rates, and these apparent CLDs were parameterized using biosynthesis-based models. The model parameters fitted from CLDs at different flow rates were extrapolated to zero flow rate, and were then used to calculate the CLD that would be obtained with zero flow rate, thereby taking partial account of shear scission. The extrapolation suggests that shear scission significantly degrades extra-long (degree of polymerization, DP, >1500) amylose chains to shorter chains (DP ~ 500-1500), which, if uncorrected, would vitiate inferences from SEC results. The partial correction method devised here can be used to develop more reliable relationships between structural and biosynthesis-related parameters of starch and functional properties of starch-containing substances.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3945-3957"},"PeriodicalIF":3.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12227465/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144136132","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":"Green and simple microextraction method based on deep eutectic solvent-assisted smartphone digital imaging colorimetry (SDIC) for Rhodamine B analysis in food products.","authors":"Buse Tezcan, Aslıhan Dalmaz, Sezen Sivrikaya Özak","doi":"10.1007/s00216-025-05932-x","DOIUrl":"10.1007/s00216-025-05932-x","url":null,"abstract":"<p><p>This study employed a deep eutectic solvent-based liquid-liquid microextraction method and smartphone digital image colorimetry to detect and quantify Rhodamine B in foods. The deep eutectic solvent, a green solvent, was prepared by mixing tetrabutylammonium bromide and octanol in a 1:2 ratio. It was observed that Rhodamine B dyestuff readily transitioned to the DES phase, eliminating the need for additional reagents. The impact of various parameters, including DES type, molar ratio, volume, solution pH, ultrasonic time, centrifugation time, and sample volume, on extraction efficiency was examined, and the most effective conditions were determined. Additionally, the diameter of the prepared colorimetric box and the distance between the detector and the sample were investigated, leading to the identification of optimal conditions. The developed method's limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.0054 μg/mL and 0.018 μg/mL, respectively, for the measurements taken using seven parallel blank solutions at 554 nm. The relative standard deviations intraday and interday were 1.29% and 2.03%, respectively. The calibration graph demonstrated good linearity, with a coefficient of determination of 0.9996. The developed method's intraday and interday relative standard deviation values were 2.03% and 1.29%, respectively. Rhodamine B was detected in food samples using the developed method, obtaining extraction recoveries ranging from 95.16 to 103.88%.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"4163-4177"},"PeriodicalIF":3.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12276117/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144223918","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":"Assessment of current use pesticides in flowers, pollen provision, and wild bees: HPLC-ESI-MS/MS method development and field implementation.","authors":"Carolina Honert, Katharina Wifling, María José Lazo Hernández, Carsten A Brühl","doi":"10.1007/s00216-025-05935-8","DOIUrl":"10.1007/s00216-025-05935-8","url":null,"abstract":"<p><p>Synthetic pesticide use is a major driver of pollinator declines in agricultural landscapes. To understand the impact of pesticides, it is essential to quantify residues in food resources and in insects themselves. We developed simple, fast, and cost-effective multiresidue methods for the simultaneous quantification of up to 83 current use pesticides (CUPs) in flowers (0.5 g sample weight) and 71 CUPs in pollen provision (0.1 g sample weight) via liquid chromatography-tandem mass spectrometry. Additionally, methods were developed for individual wild bees (Osmia bicornis), enabling the analysis of 65 CUPs in 0.02 g samples (females) and 45 CUPs in 0.01 g samples (males). The extractions used acidified acetonitrile (2.5% formic acid), with phase separation assisted by ammonium formate and clean-up via freeze-out. The validation showed limits of quantification between 0.00025 mg/kg and 0.05 mg/kg for flowers, 0.0002 mg/kg to 0.052 mg/kg for pollen provision, 0.0002 mg/kg to 0.08 mg/kg for female bees, and 0.00008 mg/kg to 0.1 mg/kg for male bees. The methods were applied to flowers, pollen provision, and post-pupal bees from agricultural sites. In total, 47 CUPs were detected in flowers, 35 in pollen provision, and 4 in post-pupal bees, with herbicides being most prevalent. This study highlights the exposure of pollinators to CUP mixtures, including emerging bees that have not yet been active in the environment. Our methods provide practical tools for monitoring CUP residues in small environmental samples, supporting the assessment of exposure in plant-insect matrices.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"4199-4213"},"PeriodicalIF":3.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12276102/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144265001","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":"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":"10.1007/s00216-025-05960-7","url":null,"abstract":"","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"4279"},"PeriodicalIF":3.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12276088/pdf/","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":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A multiplexed LC-MS/MS method to reveal changes in inflammatory and coagulation cascades induced by host infection.","authors":"Gabriella Pinto, Anna Illiano, Stefania Serpico, Fabio Maurelli, Elena Scaglione, Roberta Colicchio, Mariateresa Vitiello, Marco Varelli, Paola Salvatore, Angela Amoresano","doi":"10.1007/s00216-025-05950-9","DOIUrl":"10.1007/s00216-025-05950-9","url":null,"abstract":"<p><p>Inflammation has been considered a pivotal player in the most severe forms of respiratory infections like COVID-19, which induces a significant alteration of inflammatory cytokines called cytokine storm. Above the immune system, abnormalities in coagulation parameters have been observed in COVID-19-affected subjects displaying an increased risk of a blood clot causing thromboembolic events. Currently, clinical methods for monitoring infections rely on serological tests that detect the antibody response using enzyme-linked immunosorbent assays (ELISA). While ELISA offers high sensitivity, it is limited by complex procedures, significant matrix interference, and antibody cross-reactivity. This study aims to develop a mass spectrometry (MS)-based analytical method to support clinical investigations into the host response to infection. The use of S-Trap column digestion in a short time overcomes the limitations of traditional bottom-up proteomics protocols by significantly reducing processing time and eliminating the need for a desalting step. A targeted tandem MS approach using multiple reaction monitoring (MRM) ion mode was established to simultaneously quantify a panel of approximately 60 proteins associated with the inflammatory response and coagulation cascade. Among the proteins analyzed, 90% exhibited a good instrumental response, with 63% showing significant dysregulation in COVID-19 patients compared to controls, enabling the identification of key protein changes linked to the host's infection response. The proposed method leverages the enhanced sensitivity and selectivity of the multiplexed LC-MRM/MS technique, made possible by triple quadrupole mass spectrometers. These instruments effectively filter precursor and product ions, allowing specific monitoring of fragmentation patterns unique to each peptide sequence. By combining a rapid digestion protocol with a multiplexed LC-MRM/MS approach, this method offers a valuable solution for clinical laboratories aiming for high-specificity, high-performance analyses within a shortened analysis time.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"4015-4023"},"PeriodicalIF":3.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144493311","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":"Enhanced electrochemical detection of acetaminophen using CoNi-LDH-based sensor with ultra-wide linear range and superior performance.","authors":"Jianxia Gu, Li Fan, Jian Bai, Zhanbin Jin, Tingting Wei","doi":"10.1007/s00216-025-05901-4","DOIUrl":"10.1007/s00216-025-05901-4","url":null,"abstract":"<p><p>Electrochemical sensors for acetaminophen (AP) determination often face limitations in linear range, rarely achieving millimolar levels. This work synthesized CoNi-LDH (cobalt-nickel layered double hydroxide) via a simple hydrothermal method. By optimizing the Co/Ni ratio, the sensor based on CoNi-LDH-1 demonstrates efficient AP detection with an ultra-wide linear range spanning from 5 μM to 5 mM, enabling versatile AP monitoring in diverse samples. Furthermore, the sensor also exhibits exceptional stability, reproducibility, and selectivity. Notably, it successfully quantified AP in real-world samples (tap water and urine) while maintaining a wide linear range. The superior performance of the sensor stems from CoNi-LDH-1's unique spiky sphere morphology, abundant active sites, enhanced electron transport capability, and the synergistic effect between Co and Ni components. This work provides valuable insights for expanding the linear range of electrochemical sensors, advancing their application in analytical chemistry.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3741-3752"},"PeriodicalIF":3.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143960757","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":"Label-free quantitative shotgun analysis of bis(monoacylglycero)phosphate lipids.","authors":"Lian Y Wang, Rico J E Derks, Kevin A J Brewster, Danilo Prtvar, Sabina Tahirovic, Stefan A Berghoff, Martin Giera","doi":"10.1007/s00216-025-05890-4","DOIUrl":"10.1007/s00216-025-05890-4","url":null,"abstract":"<p><p>Interest in the role of bis(monoacylglycero)phosphate (BMP) lipids in lysosomal function has significantly grown in recent years. Emerging evidence highlights BMPs as critical players not only in Niemann-Pick disease type C (NPC) but also in other pathologies such as neurodegeneration, cardiovascular diseases, and cancers. However, the selective analysis of BMPs is significantly hindered by isomeric phosphatidylglycerol (PG) lipids. While this can be addressed by chromatographic separation, it poses a significant challenge for shotgun lipidomics approaches. Here, we present a shotgun lipidomics strategy to detect and separate BMPs from PGs using differential fragmentation of sodiated ions. This approach, including isotope correction, is integrated into an existing quantitative shotgun lipidomics workflow (Lipidyzer combined with Shotgun Lipidomics Assistant software) that simultaneously quantifies >1400 lipids. Validation using K-562 cell extracts demonstrated acceptable linearity, trueness, repeatability, and a limit of quantification of 0.12 µM, confirming robust analytical performance. Finally, characteristic accumulation of BMP lipids is shown in bone marrow-derived macrophages from NPC mice, demonstrating its applicability. Our method presents a quantitative, selective, rapid, and robust solution for shotgun-based BMP analysis without the need for extensive chromatographic separation or derivatization. The integration of BMP lipid detection into the Lipidyzer platform, alongside the recently launched iSODA data visualization tool, empowers chemists and biologists to gain deeper insights into BMP lipid biology.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3665-3673"},"PeriodicalIF":3.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12206189/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143957497","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}