{"title":"Development and validation of a high-throughput and green ultra-performance convergence chromatography-tandem mass spectrometry assay for quantification of methoxy-polyethylene glycol propionic acid polymers.","authors":"Chunpeng Feng, Jiye Tian, Qisheng Fang, Yajie Cheng, Yue Deng, JiaRui Zhang, Shuang Feng, Qingbin Wang, Hecheng Wang, Xuan Zhao, Lei Yin","doi":"10.1007/s00216-025-05849-5","DOIUrl":"10.1007/s00216-025-05849-5","url":null,"abstract":"<p><p>As a synthetic polymer, methoxy-polyethylene glycol propionic acid (M-PEG-PA) is widely used in the biomedicine field. Unraveling the pharmacokinetic behavior of M-PEG<sub>6</sub>-PA in vivo is crucial for evaluating the safety and efficiency of M-PEG-PA-related polymers or drug delivery systems. A high-throughput and green ultra-performance convergence chromatography-tandem mass spectrometry (UPC<sup>2</sup>-MS/MS) assay was firstly developed and validated for the determination of M-PEG<sub>6</sub>-PA polymers in a biological matrix. The MRM transition (mass to charge ratio, precursor ions→fragment ions) of m/z 367.2→118.9 was used to quantify M-PEG<sub>6</sub>-PA in this study. The throughput of the assay is high and the total running time for each sample was only 2 min. The linear range of the developed UPC<sup>2</sup>-MS/MS assay for quantification of M-PEG<sub>6</sub>-PA in a biological matrix is 0.05 to 30 μg/mL (R≥0.995). Intra-day and inter-day precisions for the determination of M-PEG<sub>6</sub>-PA by this analytical assay were <6.99%. The absolute recoveries and matrix effects of M-PEG<sub>6</sub>-PA ranged from 79.50 to 92.47% and 68.72 to 81.73%, respectively. The UPC<sup>2</sup>-MS/MS assay was successfully applied to quantify the concentrations of M-PEG<sub>6</sub>-PA polymers in rat plasma samples.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3091-3102"},"PeriodicalIF":3.8,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143717700","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}
Ruoning Guo, Anna M Röhnelt, Philipp R Martin, Stefan B Haderlein
{"title":"Limitations of the molybdenum blue method for phosphate quantification in the presence of organophosphonates.","authors":"Ruoning Guo, Anna M Röhnelt, Philipp R Martin, Stefan B Haderlein","doi":"10.1007/s00216-025-05850-y","DOIUrl":"10.1007/s00216-025-05850-y","url":null,"abstract":"<p><p>Organophosphonates (OPs) are widely used as chelating agents in domestic and industrial applications. While regarded as hardly biodegradable, OPs can undergo abiotic transformation with phosphate (PO<sub>4</sub><sup>3-</sup>) as a main transformation product. As some OPs are suspected precursors of glyphosate in surface waters, their environmental fate is of current interest. Due to analytical challenges posed by quantification of individual OPs, monitoring PO<sub>4</sub><sup>3-</sup> formation is a widely used proxy to monitor OP transformations. The molybdenum blue (MB) method, employing UV/Vis spectroscopy, is frequently used for PO<sub>4</sub><sup>3-</sup> quantification due to its sensitivity and operational simplicity. However, while interference of certain inorganic ions is well-documented, the effects of OPs on the accuracy of the MB method remain unexplored. This study investigated the effects of six OPs, namely N-(phosphonomethyl)glycine (glyphosate), 1-hydroxyethylidene(1,1-diphosphonic acid) (HEDP), iminodi(methylene phosphonate) (IDMP), aminotris(methylene phosphonate) (ATMP), ethylenediaminetetra(methylene phosphonate) (EDTMP), and diethylenetriaminepenta(methylene phosphonate) (DTPMP). Spectral analysis of pure PO<sub>4</sub><sup>3-</sup> standards using the MB method exhibits two characteristic absorption maxima (λ<sub>max</sub>) at 710 and 880 nm. In the presence of OPs, a new λ<sub>max</sub> appears around 760 nm. This is accompanied by an increase in absorbance values at both 710 and 880 nm, leading to significant over-quantification of PO<sub>4</sub><sup>3-</sup> concentrations. Among the evaluated OPs, DTPMP exhibits the most substantial interference (PO<sub>4</sub><sup>3-</sup> over-quantification by up to 240%), while glyphosate causes minimal interference (≤ 20%). The effects are most pronounced at OPs:PO<sub>4</sub><sup>3-</sup> ratios ≥1. A case study simulating DTPMP transformation confirms PO<sub>4</sub><sup>3-</sup> over-quantification of up to 350%, revealing limitations of the MB method. Therefore, careful data evaluation and complementary analytical techniques for accurate PO<sub>4</sub><sup>3-</sup> measurements are indispensable in OP transformation research.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3103-3111"},"PeriodicalIF":3.8,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12103472/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143750446","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}
Shanshan Lai, Jiahong Guo, Xin Li, Xiaoxiao Yu, Guosong Lai
{"title":"Dual DNA recycling amplification-assisted CRISPR/Cas12a cleavage for dual-channel ratiometric fluorescence biosensing of kanamycin antibiotic.","authors":"Shanshan Lai, Jiahong Guo, Xin Li, Xiaoxiao Yu, Guosong Lai","doi":"10.1007/s00216-025-05858-4","DOIUrl":"10.1007/s00216-025-05858-4","url":null,"abstract":"<p><p>Fluorescence biosensors hold significant importance for testing antibiotic residues which seriously endanger public health. However, how to adopt appropriate strategies to address the false result disadvantage involved in traditional single-channel biosensors is still a great challenge. Meanwhile, too much attention focused on designing signal amplification strategies of biosensors unavoidably decreases their detection efficiency. Herein, we combined the designed dual DNA recycling amplification strategy with CRISPR/Cas12a-mediated dual-channel signal output mode to successfully develop a novel ratiometric fluorescence biosensor for testing kanamycin (Kana) residues in complex sample matrices. The first recycling was formed from an exonuclease-assisted aptamer recognition reaction, which also triggered another cascade DNA recycling to amplify the release of the Cas12a activator. With the non-discrimination cleavage of Cas12a to cause reverse fluorescence changes of copper nanoclusters and an AMAC-labeled signal DNA, the ratiometric signal transduction strategy was constructed. Under optimal conditions, this biosensor could be applied for ultrasensitive testing of Kana antibiotics in a five-order of magnitude wide linear range with a low detection limit of 17.2 fg mL<sup>-1</sup>. Benefiting from the self-correction function of the ratiometric signal transduction mode, it showed promising practicality in lake water and milk samples with the relative error less than 4.9% to the standard ELISA results. Besides CRISPR/Cas12a-based fluorescence output efficiency improvement, this biosensor also excluded the complicated manipulations and expensive instruments required in traditional methods. Therefore, it provides a good choice for expanding the application of fluorescence biosensing technology for practical analysis application.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3191-3200"},"PeriodicalIF":3.8,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143778598","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}
Yifei Li, Yanfei Su, Zhengyu Chen, Jianxun Wu, Weilai Zhang, Chunming Xu, Quan Shi, Linzhou Zhang
{"title":"Comprehensive characterization of sulfur compounds in the diesel fraction using methylation/demethylation derived separation and GC × GC-MS/FID analysis.","authors":"Yifei Li, Yanfei Su, Zhengyu Chen, Jianxun Wu, Weilai Zhang, Chunming Xu, Quan Shi, Linzhou Zhang","doi":"10.1007/s00216-025-05860-w","DOIUrl":"10.1007/s00216-025-05860-w","url":null,"abstract":"<p><p>Comprehensive characterization of petroleum-derived sulfur compounds is crucial for researching and developing desulfurization catalysts, equipment, and processes. However, the complex composition and low concentration of sulfur compounds in oils make it challenging for molecular-level separation and characterization. In this work, sulfur compounds in the straight-run diesel fraction were selectively separated from the oil by the methylation/demethylation method, effectively yielding high-purity thiophenes and sulfides. Molecular-level compositional and structural characterization of sulfur compounds was accomplished through comprehensive two-dimensional gas chromatography (GC × GC) coupled with time-of-flight mass spectrometry. The separation significantly enhances the detection sensitivity for low-content sulfur compounds, thereby enabling a more comprehensive characterization of their molecular compositions and structures. Sulfur compounds with diverse skeletons and carbon numbers were tentatively characterized, including 1~3 cyclic sulfides, thiophenes, benzothiophenes, dihydrobenzothiophenes, dibenzothiophenes, tetrahydrodibenzothiophenes, phenanthrothiophenes, and benzonaphthothiophenes. Additionally, hundreds of individual sulfur compounds were characterized by mass spectrometry. Quantitative analysis for individual compounds and compound types was conducted using a flame ionization detector.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3201-3213"},"PeriodicalIF":3.8,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143794295","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}
Yingjiao Shi, Ji Yang, Qianxu Yang, Yipeng Zhang, Zhongda Zeng
{"title":"Quality evaluation of metabolite annotation based on comprehensive simulation of MS/MS data from high-resolution mass spectrometry (HRMS) and similarity scoring.","authors":"Yingjiao Shi, Ji Yang, Qianxu Yang, Yipeng Zhang, Zhongda Zeng","doi":"10.1007/s00216-025-05847-7","DOIUrl":"10.1007/s00216-025-05847-7","url":null,"abstract":"<p><p>Metabolite annotation is a critical step in discovery metabolomics, but remains a significant challenge. In this study, the accuracy of metabolite annotation was systematically evaluated by leveraging the proposed strategies for simulation of tandem mass spectrometry (MS/MS) data from high-resolution mass spectrometry (HRMS) and then construction of a large-scale virtual database. Furthermore, various similarity scoring methods were comprehensively compared to assess the performance for annotation. First, three key characteristics that are essential for simulating MS/MS spectra to closely resemble experimental data were identified: (i) the number of mass-to-charge ratio (m/z) features, (ii) the differences between neighboring m/z values, and (iii) the intensity distribution of MS/MS features. These factors were employed to generate representative MS/MS spectra for subsequent study. A meticulously designed virtual MS/MS database was constructed to facilitate accurate annotation assessment, which covered over 100,000 metabolites with diverse structural similarities and differences. To evaluate annotation quality, two simulation strategies on the basis of strong and weak data inference were respectively proposed to replicate MS/MS spectra for unknown metabolites. These simulated spectra were then compared with the virtual database, which provided insights into the expected variations in experimental MS/MS data. Furthermore, eight similarity evaluation methods, including entropy similarity (ES) and weighted dot product (W/DP) algorithms, were rigorously evaluated for their effectiveness in metabolite annotation. The results revealed that some methods, such as ES, exhibited strong resistance to interference and broad adaptability across different MS/MS patterns, whereas others selectively yielded reliable outcomes under specific conditions. This study provided a systematic framework for quality evaluation in metabolite annotation and offered strategies to mitigate false-positive identifications. The findings held great significance for advancing metabolomics research and further improving annotation reliability in complex biological samples.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3061-3077"},"PeriodicalIF":3.8,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143960819","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}
Yao Liu, Yang Li, Yuting Shan, Jiufa Zhang, Xiaohe Huang, Yueyue Yu, Cuiping Ma, Yan Xu, Chao Shi
{"title":"A rolling circle mediated exponential amplification reaction with suppressed nonspecific amplification to detect pathogen RNA with high sensitivity.","authors":"Yao Liu, Yang Li, Yuting Shan, Jiufa Zhang, Xiaohe Huang, Yueyue Yu, Cuiping Ma, Yan Xu, Chao Shi","doi":"10.1007/s00216-025-05835-x","DOIUrl":"10.1007/s00216-025-05835-x","url":null,"abstract":"<p><p>Respiratory infections caused by pathogens such as influenza virus and SARS-CoV-2 seriously threaten human life and health. RNA has been widely recognized as an important biomarker for diagnosing these pathogens, creating a growing need for rapid and accurate RNA detection methods. Isothermal nucleic acid amplification has emerged as a promising molecular diagnostics approach. Exponential amplification reactions (EXPAR) is a commonly used RNA detection method, known for its simplicity and rapid signal amplification in a short time. However, traditional EXPAR is only suitable for detecting short-sequence RNA, and 3'-end template interactions in the amplification reaction can lead to nonspecific amplification, which greatly limits its practical application. Here, we established an isothermal amplification method comprising a three-way junction (3-WJ) structure and dumbbell probe (DP) for the rapid and sensitive detection of pathogen RNA in a single closed tube, termed the rolling circle mediated exponential amplification reaction (RC-EXPAR). The introduction of the DP eliminated the 3'-end of the template, suppressing nonspecific amplification caused by the 3'-end extension in the reaction. Although the trigger generation by the 3-WJ structure is a linear amplification process, the RC-EXPAR amplifies the triggers exponentially to enhance signal output further and increase sensitivity. The proposed method showed a high sensitivity with a limit of detection (LOD) of 10<sup>3</sup> copies/mL. Moreover, RC-EXPAR demonstrated strong anti-interference capability in complex biological matrices. This work opens up new ideas for suppressing nonspecific amplification and provides a promising signal amplification strategy for rapid, sensitive, and specific pathogen detection in clinical.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3009-3020"},"PeriodicalIF":3.8,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143690529","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}
Han Zheng, Xiaoping Song, Haifeng Wang, Yue Kou, Jia Li
{"title":"Determination of the water content of crude oil by thermometric titration.","authors":"Han Zheng, Xiaoping Song, Haifeng Wang, Yue Kou, Jia Li","doi":"10.1007/s00216-025-05833-z","DOIUrl":"10.1007/s00216-025-05833-z","url":null,"abstract":"<p><p>The water content of crude oil needs to be accurately and conveniently determined. A thermometric titration method in which triethyl orthoformate and water react stoichiometrically and then absorb heat has been developed to determine the water content of crude oil. Triethyl orthoformate solution was used as the titrant; a mixture of cyclohexane, isopropanol, and xylene was used as the solvent; and dodecylbenzene sulfonic acid was used as the catalyst. The optimized method has a water mass range of 5 to 300 mg. The upper limit of water mass (300 mg) was greater than those of Karl Fischer coulometric titration (KFCT) and azeotropic distillation-KFCT (AD-KFCT). Real-time calibration by alternatively measuring the sample and a standard and modifying the result by the neighboring recovery was used to reduce the effect of the shift of the calibration curve. The effect of the types of catalysts and titrants was investigated. When the certified reference materials of light or heavy crude oil for water content were measured, the relative standard deviation and absolute value of the relative error of the results were ≤ 1.2% and ≤ 3.9%, respectively. The repeatability and accuracy were better than those of the distillation, KFCT, and AD-KFCT. The present method can determine the water content of commercial crude oil with good accuracy and convenience, and thus has the potential to be an international standard method.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"2997-3008"},"PeriodicalIF":3.8,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143690533","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 comparative study of data-independent acquisition and data-dependent acquisition in liquid chromatography-mass spectrometry-based untargeted metabolomics analysis of Panax genus sample.","authors":"Yi Wu, Yang Wang","doi":"10.1007/s00216-025-05861-9","DOIUrl":"10.1007/s00216-025-05861-9","url":null,"abstract":"<p><p>Data-independent acquisition (DIA) and data-dependent acquisition (DDA) are frequently employed in the execution of tandem mass spectrometry (MS2) analyses. This study explored the application of DIA (MSe) and DDA (fast-DDA) in liquid chromatography-mass spectrometry (LC-MS)-based untargeted metabolomics using Panax genus samples. MSe provided comprehensive sample information, extracting more ion peaks with better peak shape and increased scan points compared to fast-DDA. Features from MSe data are four times more than those from fast-DDA data. Fast-DDA, however, delivered high-quality MS2 data, enhancing compound annotation via the GNPS web tool. Database matches with fast-DDA data were nearly 35 times greater than those using MSe data. Therefore, combining MSe and fast-DDA can improve data analysis and metabolite annotation. An improved workflow integrating DIA and DDA was proposed, requiring additional QC sample injections for DDA analysis but eliminating the need for sample reprocessing and re-analysis, thus saving time and resources. The established workflow was applied to the Panax genus samples analysis to confirm its applicability. This study offers a deeper understanding of DIA and DDA, guiding the selection of data acquisition strategies for LC-MS-based untargeted metabolomics.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3215-3228"},"PeriodicalIF":3.8,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143762491","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":"Identification and characterization of chiral vitamin C using ion mobility and theoretical calculation.","authors":"Ying Zou, Manli Zhang, Dongdong Zhou, Chaoxian Chi, Fangling Wu, Chuan-Fan Ding","doi":"10.1007/s00216-025-05855-7","DOIUrl":"10.1007/s00216-025-05855-7","url":null,"abstract":"<p><p>Vitamin C (L-( +)-ascorbic acid, L-AA) is an essential micronutrient. Its diastereoisomer, D-(-)-isoascorbic acid (D-IAA), is only 5% as active as L-AA. Therefore, it is crucial to identify and characterize the diastereoisomers of ascorbic acid. In this work, a straightforward and direct method using ion mobility-mass spectrometry (IM-MS) was proposed to identify ascorbic acid isomers. Ternary complexes [L-AA + γ-CD + 2Cs-H]<sup>+</sup> and [D-IAA + γ-CD + 2Cs-H]<sup>+</sup>, formed by non-covalent interaction of the isomer with the selective agent γ-CD and the metal ion Cs<sup>+</sup>, were separated in ion drift tubes with a resolution of R<sub>p-p</sub> as high as 1.398. Meanwhile, comparisons with different CDs and metal ions revealed varying separation efficiencies. Theoretical calculations were conducted to determine the optimal conformations of [L-AA + γ-CD + 2Cs-H]<sup>+</sup> and [D-IAA + γ-CD + 2Cs-H]<sup>+</sup>. Conformational analysis highlighted distinct structural differences at the molecular level, providing insight into the mobility separation mechanism of AA via the formation of ternary complexes with γ-CD and metal ions. Additionally, a quantitative analysis for the determination of chiral isomers was established with effective linearity and acceptable sensitivity. The method was successfully applied to assess L-AA/D-IAA content in pharmaceuticals and fruit samples.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3157-3168"},"PeriodicalIF":3.8,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143794297","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}
Miriam Guadaño-Sánchez, Juan J López, Luis A Serrano, Laura Álvaro-Gómez, Lucas Pérez, Matilde Saura-Múzquiz, Javier L Urraca
{"title":"Determination of cyclopiazonic acid in food samples by using molecularly imprinted polymers based on magnetic halloysite nanotubes.","authors":"Miriam Guadaño-Sánchez, Juan J López, Luis A Serrano, Laura Álvaro-Gómez, Lucas Pérez, Matilde Saura-Múzquiz, Javier L Urraca","doi":"10.1007/s00216-025-05854-8","DOIUrl":"10.1007/s00216-025-05854-8","url":null,"abstract":"<p><p>A fast, accurate, and simple method of molecularly imprinted solid-phase extraction from magnetic molecularly imprinted polymers (m-MISPE) has been developed for the determination of cyclopiazonic acid (CPA) in food samples. For the synthesis of the magnetic molecularly imprinted polymers, the core-shell method through microwave irradiation was employed. Firstly, as the core halloysite nanotubes were functionalized with magnetite nanoparticles. Then, the molecular imprinted polymer (MIP) shell was created around the halloysite nanotube cores by microwave induction. In the MIP synthesis for the template molecule, an analogous compound in structure to that of CPA has been used as a surrogate molecule to reduce the costs and toxicity produced by the toxin. Besides, washing and elution m-MISPE steps were optimized to eliminate the interferences. Cross-reactivity of the m-MISPE proposed method has been tested with different mycotoxins to determine the selectivity of the polymer towards CPA (imprinting factor (IF): MIP/NIP<sub>CPA</sub> = 3,1; MIP/NIP<sub>ZON</sub> = 2,2; MIP/NIP<sub>AOH</sub> = 1,7; MIP/NIP<sub>OCRA</sub> = 0,8). Finally, the m-MISPE method has been successfully applied to rice flour samples at three different concentration levels, 75, 120, and 200 μg/L, whose recoveries were 83, 97, and 93% and their RDS were 1, 2, and 2, respectively. The detection and quantification limits were 11.1 and 36.5 µg/kg respectively. This procedure is considered an easy and economical analytical way to determine CPA in food in routine laboratories of any food quality and is easy to implement versus the current methods in the determination of this mycotoxin.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":"3141-3156"},"PeriodicalIF":3.8,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143956746","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}