Analytical and Bioanalytical Chemistry最新文献_第4页

Microscale solid-phase extraction: advances in sorbent formats, system design, integration, and detection methods. 微尺度固相萃取：吸附剂形式、系统设计、集成和检测方法的进展。

IF 4.1 2区化学

Analytical and Bioanalytical Chemistry Pub Date : 2026-09-30 DOI: 10.1007/s00216-026-06825-3

Timothy B Skaggs, Laurel C Smith, Phillip Odiambo, Adam T Woolley

{"title":"Microscale solid-phase extraction: advances in sorbent formats, system design, integration, and detection methods.","authors":"Timothy B Skaggs, Laurel C Smith, Phillip Odiambo, Adam T Woolley","doi":"10.1007/s00216-026-06825-3","DOIUrl":"https://doi.org/10.1007/s00216-026-06825-3","url":null,"abstract":"Sample preparation is essential in chemical analysis as a critical determinant of analytical sensitivity, selectivity, and throughput, and is often the most resource-intensive stage of an analytical workflow. Microscale solid-phase extraction (µSPE) helps to address the sample preparation limitations associated with conventional SPE by enabling analyte enrichment and matrix cleanup at reduced volumes, with integration potential that traditional formats cannot match. This Critical Review assesses recent advances across six µSPE modalities: reverse-phase, ion exchange, immunoaffinity, aptamer-based, nucleic acid affinity, and magnetic particle, with attention to device preparation, detection integration, and performance metrics of each platform. Key enabling technologies for advancing µSPE, such as 3D printing, are described, and notable trends in the field are identified. Additionally, significant opportunities for future development in µSPE are discussed. Ongoing work positions µSPE as a foundational technology for advancing sample preparation and enhancing chemical analysis reliability.","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149079200","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}

引用次数: 0

Fluorescence biosensing for simultaneous detection of HPV16 and HPV18. 同时检测HPV16和HPV18的荧光生物传感技术。

IF 4.1 2区化学

Analytical and Bioanalytical Chemistry Pub Date : 2026-09-29 DOI: 10.1007/s00216-026-06850-2

Ze-Lin Wang, Zhao-Li Mou, Can Yang, Sheng-Liang Jin, Han-Ying Zhan, Zhi-Qi Zhang

{"title":"Fluorescence biosensing for simultaneous detection of HPV16 and HPV18.","authors":"Ze-Lin Wang, Zhao-Li Mou, Can Yang, Sheng-Liang Jin, Han-Ying Zhan, Zhi-Qi Zhang","doi":"10.1007/s00216-026-06850-2","DOIUrl":"https://doi.org/10.1007/s00216-026-06850-2","url":null,"abstract":"Cervical, most anal, and most oropharyngeal cancers are caused by human papillomavirus (HPV), with HPV16 and HPV18 accounting for the majority of cases, necessitating simultaneous detection of multiple HPV types for identifying HPV infection, risk stratification, and screening for HPV-associated disease. Entropy-driven catalytic strand displacement reactions are DNA self-assembly amplification methods that do not require enzymes for signal amplification. Furthermore, their driving forces originate within the system, endowing them with high specificity, which provides a crucial advantage for simultaneous detection of several targets. Therefore, an analytical method was developed to amplify fluorescence signals via dual-toehold-mediated strand displacement, enabling simultaneous detection of HPV18 and HPV16. For both targets, the established method shows excellent linearity of the regression curve in the concentration range from 0.05 to 5 nM. The detection limits for HPV18 and HPV16 were 0.020 and 0.033 nM, respectively, which are highly favorable even for the detection of only a single HPV type. These results show that the developed enzyme-free assay has high sensitivity and specificity, making it a promising technique for rapid and cost-effective HPV16 and HPV18 screening.","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149079168","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}

引用次数: 0

Dual-tetrahedral DNA-enabled strand displacement amplification biosensor for cell imaging and clinical detection of miR-34a-5p in NAFLD. 双四面体dna链位移扩增生物传感器用于NAFLD中miR-34a-5p的细胞成像和临床检测。

IF 4.1 2区化学

Analytical and Bioanalytical Chemistry Pub Date : 2026-09-29 DOI: 10.1007/s00216-026-06838-y

Xiaoyan Dai, Muling Ye, Xiaoling Li, Ying Chen, Hongmei Fu, Liang Xu, Liangxing Wang, Zhifa Shen, Yuqin Zhu

{"title":"Dual-tetrahedral DNA-enabled strand displacement amplification biosensor for cell imaging and clinical detection of miR-34a-5p in NAFLD.","authors":"Xiaoyan Dai, Muling Ye, Xiaoling Li, Ying Chen, Hongmei Fu, Liang Xu, Liangxing Wang, Zhifa Shen, Yuqin Zhu","doi":"10.1007/s00216-026-06838-y","DOIUrl":"https://doi.org/10.1007/s00216-026-06838-y","url":null,"abstract":"The clinical diagnosis of nonalcoholic fatty liver disease (NAFLD) remains challenging due to the invasiveness of liver biopsy and the lack of reliable serum biomarkers, particularly for detecting low-abundance, highly homologous microRNAs such as miR-34a-5p. Here, we constructed a dual-tetrahedral DNA nanostructure biosensor (named DTDN) that couples a target-triggered strand displacement reaction with a catalytic feedback amplification circuit within a rigid tetrahedral scaffold. Unlike conventional molecular beacon or linear probe designs, this spatial architecture accelerates recognition kinetics and suppresses false-positive signals from complex biological matrices, allowing the DTDN probe to discriminate miR-34a-5p from single-base mismatched family members and to achieve a detection limit of 500 fM directly in untreated serum. Importantly, the DTDN accurately quantifies circulating miR-34a-5p levels in NAFLD individuals, which correlate significantly with lipid profiles and transaminase levels. Beyond clinical detection, the same design enables high-contrast live-cell imaging for real-time tracking of miR-34a-5p dynamics in hepatocytes under metabolic stress. By overcoming key barriers-low abundance, sequence homology, matrix interference, and lack of non-invasive spatial readouts-this dual-tetrahedral platform offers a translational route for early NAFLD diagnosis and broader miRNA-based liquid biopsy applications.","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149079199","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}

引用次数: 0

CHA-mediated split G-quadruplex assembly: a ratiometric AIE strategy for label-free detection of APE1. cha介导的分裂g -四重体组装：用于无标记检测APE1的比例AIE策略。

IF 4.1 2区化学

Analytical and Bioanalytical Chemistry Pub Date : 2026-09-28 DOI: 10.1007/s00216-026-06845-z

Chan Yang, Zihan Yan, Yanru Qin, Ying Wei, Ziyi He, Liuting Mo, Weiying Lin

{"title":"CHA-mediated split G-quadruplex assembly: a ratiometric AIE strategy for label-free detection of APE1.","authors":"Chan Yang, Zihan Yan, Yanru Qin, Ying Wei, Ziyi He, Liuting Mo, Weiying Lin","doi":"10.1007/s00216-026-06845-z","DOIUrl":"https://doi.org/10.1007/s00216-026-06845-z","url":null,"abstract":"Apurinic/apyrimidinic endonuclease 1 (APE1), a critical enzyme in the base excision repair pathway, is a potential biomarker for numerous cancer types. Traditional APE1 activity detection methods are hindered by complex protocols, expensive labeling requirements, and vulnerability to environmental factors. Herein, we develop a label-free ratiometric fluorescent biosensor (TCHG) that integrates APE1-mediated catalytic hairpin assembly (CHA) amplification with split G-quadruplex/malachite green (MG)-mediated aggregation-induced emission (AIE) signaling for sensitive activity analysis of APE1. Our system operates through APE1's specific cleavage of apurinic/apyrimidinic (AP) site-containing double-stranded substrates, which releases trigger strands that initiate a CHA cascade. This cascade drives the assembly of split G-quadruplex structures. Upon reconstruction, the complete G-quadruplex binds MG, generating amplified near-infrared fluorescence with AIE characteristics. Simultaneously, Hoechst 33258 (HOE) embedded within double-stranded DNA provides a stable reference signal, enabling self-calibrated ratiometric output that effectively minimizes signal fluctuations from instrumental and environmental variations. The TCHG biosensor demonstrates high selectivity for APE1 with a detection limit of 2.4 × 10-3 U/mL. Importantly, it maintains reliable analytical performance in complex biological matrices, including fetal bovine serum and various cell lysates, successfully differentiating endogenous APE1 activity between normal and cancer cells. The TCHG system offers a tool for APE1 activity analysis in biological samples, with potential applications in biomedical research.","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-09-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149073091","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}

引用次数: 0

Quantitative single cell analysis of gold nanoparticle association across a mouse triple-negative breast cancer cell line and blood immune cell populations. 金纳米颗粒在小鼠三阴性乳腺癌细胞系和血液免疫细胞群间关联的定量单细胞分析。

IF 4.1 2区化学

Analytical and Bioanalytical Chemistry Pub Date : 2026-09-28 DOI: 10.1007/s00216-026-06842-2

Quy Van-Chanh Le, Randall Grose, Sonia Sebastian, Anh Thai-Quynh Nguyen, Tyron Turnbull, Hien Le, Ivan Kempson

{"title":"Quantitative single cell analysis of gold nanoparticle association across a mouse triple-negative breast cancer cell line and blood immune cell populations.","authors":"Quy Van-Chanh Le, Randall Grose, Sonia Sebastian, Anh Thai-Quynh Nguyen, Tyron Turnbull, Hien Le, Ivan Kempson","doi":"10.1007/s00216-026-06842-2","DOIUrl":"https://doi.org/10.1007/s00216-026-06842-2","url":null,"abstract":"In biomedical research, understanding the heterogeneity in nanoparticle association among different cell populations is crucial for translating to efficacy and immune identification. Using time-of-flight mass cytometry (CyTOF), we quantitatively assessed the association and distribution of gold nanoparticles (AuNPs) in murine breast cancer 4T1 cells and various immune cell populations in whole blood. Our findings reveal significant variability in gold nanoparticle accumulation across different cell types. In vitro, 4T1 cells co-cultured with 0.1 nM AuNPs had a median gold mass of 0.214 pg per cell which increased proportionally and significantly (P < 0.0001) to 2.418 pg per cell when exposed to 1 nM AuNPs. Regarding immune cell populations in mouse blood directly exposed to 0.1 nM AuNPs, heterogeneity in nanoparticle association varied across immune cell populations. We observed diverse levels of gold association (median, range pg/cell) in NK cells (0.0132, 0.0014-0.0265), dendritic cells (0.0131, 0.0004-0.0272), monocytes (0.0121, 0.0006-0.0272), granulocytes (0.0126, 0.0004-0.0272), B cells (0.0099, 0.0003-0.0274), CD4 T cells (0.0072, 0.0004-0.0226), and CD8 T cells (0.0062, 0.0006-0.1113). However, the single cell analysis revealed a monocyte subpopulation had the greatest association with AuNPs with almost 2 orders of magnitude greater association than NK cell median. These findings highlight the heterogeneous association of AuNPs with immune cell subsets in blood. This observation suggests that monocytes and dendritic cells display a higher propensity for interacting with and internalizing the nanoparticles, potentially due to specific receptor-mediated interactions and internalization mechanisms.","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-09-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149068939","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}

引用次数: 0

Surface-enhanced Raman scattering spectroscopy of human cerebrospinal fluid: protocol selection and biomolecular interpretation. 人脑脊液的表面增强拉曼散射光谱：方案选择和生物分子解释。

IF 4.1 2区化学

Analytical and Bioanalytical Chemistry Pub Date : 2026-09-26 DOI: 10.1007/s00216-026-06834-2

Roberto Gobbato, Federica Tramer, Paola Sist, Arianna Sartori, Valter Sergo, Alois Bonifacio

{"title":"Surface-enhanced Raman scattering spectroscopy of human cerebrospinal fluid: protocol selection and biomolecular interpretation.","authors":"Roberto Gobbato, Federica Tramer, Paola Sist, Arianna Sartori, Valter Sergo, Alois Bonifacio","doi":"10.1007/s00216-026-06834-2","DOIUrl":"https://doi.org/10.1007/s00216-026-06834-2","url":null,"abstract":"Surface-enhanced Raman scattering (SERS) of human cerebrospinal fluid (CSF) is a promising tool for identifying possible small-molecule pathological biomarkers in neurodegenerative and neuroinflammatory diseases. However, the biochemical interpretation of CSF SERS spectra remains incomplete and lacks consensus. By critically reviewing the available literature, and by using various experimental approaches, the spectral band interpretation of this biofluid is evaluated. The suitability of different SERS protocols and CSF preprocessing strategies, including analysis performed with and without deproteinization, was also critically evaluated through the comparison of six procedures employing both Ag and Au substrates. Analyses of CSF spiked with selected biomolecules, spectral changes induced by sequential enzymatic depletion treatments, spectral fitting, and reconstruction of an artificial CSF sample all indicate that the primary contributors to the SERS spectrum of CSF obtained from Au substrates with a near-infrared excitation (785 nm) are creatinine, hypoxanthine, xanthine, uric acid and guanine. Additionally, results from linear combination fitting by using pure components spectra and other experimental observations strongly emphasize the importance of considering competition for binding sites, spectral overlapping, and matrix effects when interpreting SERS spectra of complex biological fluids.","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-09-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149056718","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}

引用次数: 0

An ionic liquid-functionalized styrene-maleic anhydride copolymer brush stationary phase coupled with offline two-dimensional LC-MS/MS for comprehensive exosomal phospholipid profiling in breast cancer. 离子液体功能化苯乙烯-马来酸酐共聚物刷状固定相结合离线二维LC-MS/MS用于乳腺癌外泌体磷脂的综合分析。

IF 4.1 2区化学

Analytical and Bioanalytical Chemistry Pub Date : 2026-09-25 DOI: 10.1007/s00216-026-06832-4

Xinhui Guan, Yuying Zhang, Xiaoqiao Ma, Haiyan Wang, Xiaoqiang Qiao, Xiaofei Gu

{"title":"An ionic liquid-functionalized styrene-maleic anhydride copolymer brush stationary phase coupled with offline two-dimensional LC-MS/MS for comprehensive exosomal phospholipid profiling in breast cancer.","authors":"Xinhui Guan, Yuying Zhang, Xiaoqiao Ma, Haiyan Wang, Xiaoqiang Qiao, Xiaofei Gu","doi":"10.1007/s00216-026-06832-4","DOIUrl":"https://doi.org/10.1007/s00216-026-06832-4","url":null,"abstract":"Comprehensive characterization of exosomal phospholipids is essential for understanding cancer-associated metabolic alterations and discovering potential biomarkers, but remains challenging due to their extensive structural diversity and the limited selectivity and coverage of conventional liquid chromatography-tandem mass spectrometry (LC-MS/MS) approaches. In this study, an ionic liquid-functionalized styrene-maleic anhydride copolymer brush stationary phase (Sil-BHHICl) was developed and integrated into an offline two-dimensional (2D) LC-MS/MS platform for comprehensive exosomal phospholipid profiling. The Sil-BHHICl stationary phase exhibited a hydrophilic interaction/reversed-phase mixed-mode retention mechanism and provided enhanced selectivity toward phospholipids, enabling efficient separation at both the phospholipid-class and molecular-species levels. The developed analytical platform enabled comprehensive profiling of plasma-derived exosomal phospholipids, resulting in the identification of 274 molecular species belonging to 10 phospholipid classes. Lipidomic analysis of plasma exosomes from breast cancer patients and healthy controls revealed distinct phospholipid alterations associated with breast cancer and identified five candidate biomarkers, among which LysoPC-O (16:0) exhibited the strongest discriminatory ability. Pathway enrichment analysis further indicated that the altered phospholipids were predominantly associated with glycerophospholipid metabolism, suggesting extensive lipid metabolic remodeling in breast cancer. Overall, this study establishes a mixed-mode chromatographic platform for high-coverage exosomal phospholipid profiling and demonstrates its potential for lipidomics-based biomarker discovery and investigation of disease-associated metabolic alterations.","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149056668","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}

引用次数: 0

Modulating proteoform charge states and signal intensities in LC-MS using a nanoflow sheath liquid interface. 利用纳米流鞘状液体界面调制LC-MS中蛋白质形态电荷状态和信号强度。

IF 4.1 2区化学

Analytical and Bioanalytical Chemistry Pub Date : 2026-09-25 DOI: 10.1007/s00216-026-06835-1

Tobias Waldmann, Philipp T Kaulich, Christian Neusüß

{"title":"Modulating proteoform charge states and signal intensities in LC-MS using a nanoflow sheath liquid interface.","authors":"Tobias Waldmann, Philipp T Kaulich, Christian Neusüß","doi":"10.1007/s00216-026-06835-1","DOIUrl":"https://doi.org/10.1007/s00216-026-06835-1","url":null,"abstract":"To investigate intact proteins in biological samples, hyphenation of mass spectrometers (MS) with separation techniques like liquid chromatography (LC) or capillary zone electrophoresis (CZE) is crucial. While reversed-phase nanoLC is typically coupled directly (\"sheathless\") to a mass spectrometer, for CZE-MS coupling, sheath liquid interfaces are typically used. Here, we coupled the reversed-phase nanoLC to an Orbitrap Fusion Lumos using a nanoflow sheath liquid interface (nanoCEasy-interface) and compared the results with the conventional (\"sheathless\") coupling. We investigated the influence of emitter orifice diameter and the use of sheath liquid on proteoform ionization using constant LC flow independently of any high voltage as required for CZE separations. We found that a smaller emitter orifice is beneficial regarding proteoform intensity. Furthermore, the used sheath liquid also has a major effect on the resulting proteoform intensity, especially for emitters with a larger orifice and thus increased dilution of the column's effluent with sheath liquid. Additionally, the sheath liquid influenced the charge state distributions of proteoforms, e.g., shifting the most abundant charge state of histone H4 from 15+ to 8+ upon addition of a 2-propanol:water (1:1, v/v) with 0.5% formic acid sheath liquid to the column effluent. This approach allows for easily reducing co-isolation of proteoforms by shifting their charge states to higher m/z and thus increasing the m/z difference between proteoforms with similar mass.","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149056760","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}

引用次数: 0

Comprehensive molecular profiling of lignin-derived products from reductive catalytic fractionation by HPLC-UV/MSⁿ: from monomers to heavy oligomers. 用HPLC-UV/MSn还原催化分离木质素衍生产物的综合分子分析：从单体到重聚物。

IF 4.1 2区化学

Analytical and Bioanalytical Chemistry Pub Date : 2026-09-25 DOI: 10.1007/s00216-026-06836-0

Xun Kuang, Linyu Zhu, Cunhao Cui, Xintong Xiao, Zhongyue Zhou, Fei Qi

{"title":"Comprehensive molecular profiling of lignin-derived products from reductive catalytic fractionation by HPLC-UV/MSn: from monomers to heavy oligomers.","authors":"Xun Kuang, Linyu Zhu, Cunhao Cui, Xintong Xiao, Zhongyue Zhou, Fei Qi","doi":"10.1007/s00216-026-06836-0","DOIUrl":"https://doi.org/10.1007/s00216-026-06836-0","url":null,"abstract":"Reductive catalytic fractionation (RCF) has emerged as a leading lignin-first biorefinery strategy for producing valuable phenolic chemicals. However, molecular-level characterization of its highly complex product mixtures remains challenging due to extensive structural isomerism, severe ion suppression, and the limited capability of conventional mass spectrometry to resolve higher molecular weight species. Herein, we present a comprehensive analytical platform based on high-performance liquid chromatography coupled with ultraviolet detection and multi-stage mass spectrometry (HPLC-UV/MSn) for direct characterization of RCF-derived phenolic products without further derivatization or fractionation after centrifugation. By integrating chromatographic separation with tandem mass spectrometry, the approach transforms congested one-dimensional mass spectra into two-dimensional molecular landscapes, enabling the differentiation of structural isomers and the putative assignment of more than 50 phenolic species through retention behavior and MSn fragmentation patterns. The chromatographic dimension also improves the detectability of some weak signals, extending molecular coverage from monomers to heavy oligomers with molecular weights up to approximately 1050 Da. In addition, a preliminary concentration-response assessment was conducted using six representative model compounds spanning oxidized phenolics, a non-oxidized phenolic monomer, reduced propyl G/S monomers, and a C-C-linked dimer. By bridging the long-standing analytical gap between volatile monomers and complex oligomeric fractions, this work provides a powerful and broadly applicable platform for elucidating lignin depolymerization pathways, tracking structural evolution during RCF, and accelerating the rational optimization of biomass valorization processes.","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149035921","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}

引用次数: 0

Development of a certified reference material for polycyclic aromatic hydrocarbons (PAH) in olive oil. 橄榄油中多环芳烃（PAH）标准物质的研制。

IF 4.1 2区化学

Analytical and Bioanalytical Chemistry Pub Date : 2026-09-25 DOI: 10.1007/s00216-026-06826-2

Thomas Sommerfeld, Jan Lisec, Christian Jung, Tatjana Mauch, Juliane Riedel, Sebastian Recknagel, Sibylle Penk, Sabine Buttler, Silke Richter, Matthias Koch

{"title":"Development of a certified reference material for polycyclic aromatic hydrocarbons (PAH) in olive oil.","authors":"Thomas Sommerfeld, Jan Lisec, Christian Jung, Tatjana Mauch, Juliane Riedel, Sebastian Recknagel, Sibylle Penk, Sabine Buttler, Silke Richter, Matthias Koch","doi":"10.1007/s00216-026-06826-2","DOIUrl":"https://doi.org/10.1007/s00216-026-06826-2","url":null,"abstract":"Like all edible vegetable oils, olive oils can be contaminated with lipophilic organic pollutants such as polycyclic aromatic hydrocarbons (PAH). Olive oils are susceptible to PAH contamination, typically due to combined effects including environmental pollution, oil processing, and migration from food contact materials. Monitoring PAH levels in olive oil is therefore essential to ensure food safety and consumer protection. According to Commission Regulation 2023/915, maximum levels have been set for certain PAH: 2 µg kg-1 for benzo[a]pyrene (BaP) and 10 µg kg-1 for PAH-4, representing the sum of BaP, benz[a]anthracene (BaA), benzo[b]fluoranthene (BbF), and chrysene (Chr). However, no certified reference material (CRM) is currently available containing PAH-4 at the regulated maximum levels. To address this deficiency, the first CRM for PAH-4 in extra virgin olive oil (BAM-A001) was developed based on the requirements of ISO 33405. BAM-A001 is intended to be used for performance evaluation and validation of analytical methods for the determination of PAH in olive oil and similar vegetable oils. The entire CRM development process including preparation, homogeneity and stability studies, and value assignment is presented. The certified mass fractions of BaP (1.44 µg kg-1) and PAH-4 (7.33 µg kg-1) were determined upon in-house study at BAM using stable isotope dilution analysis gas chromatography mass spectrometry (SIDA-GC-MS). In addition, BAM-A001 underwent secondary characterization for lead (Pb) and cadmium (Cd) levels, acknowledging an EU regulation allowing a maximum of 0.1 mg kg-1 Pb in oils and fats.","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149056736","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}

引用次数: 0