Paula Domínguez-Lacueva, Ewa Sikorska and María J. Cantalejo-Díez
{"title":"Excitation–emission matrix spectroscopy coupled with chemometrics for monitoring ozonation of olive oil and olive pomace oil†","authors":"Paula Domínguez-Lacueva, Ewa Sikorska and María J. Cantalejo-Díez","doi":"10.1039/D4AY02267J","DOIUrl":"10.1039/D4AY02267J","url":null,"abstract":"<p >The effects of ozonation on the Total Polyphenol Content (TPC) of olive oils remain largely unexplored, despite the significant role that polyphenols play in enhancing the health benefits and quality of these oils. Understanding how ozone treatment impacts phenolic compounds is vital, especially considering the documented negative effects of thermal and photochemical oxidation on TPC. The aim of this study was to explore the use of fluorescence spectroscopy combined with chemometrics to develop multivariate models for monitoring the effects of ozonation on TPC and key physicochemical parameters such as the peroxide index (PI), acidity index (AI), iodine value (IV) and viscosity (<em>V</em>) in both, virgin and pomace olive oils. Parallel factor analysis and principal component analysis of fluorescence excitation–emission matrices (EEMs) of ozonated olive oils revealed that as the ozonation process progressed, TPC and fluorescence emission decreased. And, at the same time, ozonation increased the values of oxidation indicators such as PI, AI, viscosity and intensity of the Rayleigh scattering signal. PLS models based on analysis of unfolded EEMs exhibited good predictive performance for PI (<em>R</em><small><sup>2</sup></small> = 0.822; RPD > 2.5), and moderate for TPC and V (<em>R</em><small><sup>2</sup></small> = 0.792 and 0.753; RPD > 2). In summary, we demonstrated the feasibility of EEM spectroscopy for monitoring the ozonation process. The use of this method can ease the characterization of ozonated olive oils and, additionally, make the analysis more sustainable.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 8","pages":" 1860-1869"},"PeriodicalIF":2.7,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ay/d4ay02267j?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143363284","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Mingfeng Lai, Shitao Lu, Bao Huang, Yanfeng Nie, Xu Wang, Jiaying Xiong and Zhenning Yu
{"title":"A photo-elutable 8–17 DNAzyme labeling and PCR-free colorimetric quantification strategy for 5-hydroxymethylcytosine in mammalian genomic DNA†","authors":"Mingfeng Lai, Shitao Lu, Bao Huang, Yanfeng Nie, Xu Wang, Jiaying Xiong and Zhenning Yu","doi":"10.1039/D5AY00111K","DOIUrl":"10.1039/D5AY00111K","url":null,"abstract":"<p >We developed a PCR-free, cost-effective colorimetric assay using gold nanoparticles (AuNPs) to quantify 5-hydroxymethylcytosine (5hmC) without expensive MS instruments or antibodies. This method employs a photo-elutable 8–17 DNAzyme label specific to 5hmC sites, achieving accuracy comparable to ELISA when measuring 5hmC levels in various ICR mouse tissues.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 8","pages":" 1749-1753"},"PeriodicalIF":2.7,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143381148","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Analysis of phosphorylation site occupancy of peptides based on a chemical derivatization method†","authors":"Xingdan Wang, Zhenghu Min, Xiaoqiu Yang, Qiwei Zhang and Qi Zheng","doi":"10.1039/D4AY02208D","DOIUrl":"10.1039/D4AY02208D","url":null,"abstract":"<p >Phosphorylation represents one of the most pervasive and meaningful post-translational modifications of proteins. The analysis of phosphorylation site occupancy is of great importance for elucidating protein function and disease mechanisms. Nevertheless, the direct mass spectrometric analysis of modification occupancy remains a significant challenge. In this study, a two-step derivatization method was employed in conjunction with liquid chromatography-tandem mass spectrometry for the examination of the phosphorylation site occupancy of peptides. The derivatization resulted in the specific labeling of phosphorylation sites and served to reduce the discrepancy in charge properties between phosphorylated and non-phosphorylated peptides, which is advantageous for their simultaneous detection. The occupancies of multiple sites from bovine casein and goldfish tissues were successfully estimated, confirming the usefulness and reproducibility of the method in the analysis of complex biological samples. Furthermore, the application of this method allowed for the observation of peptides with low occupancy, as well as peptides with markedly different occupancy levels between fish tissues. These results suggest that this methodology may be employed as a specialized analytical technique for site occupancy studies, thereby facilitating the investigation of the regulatory mechanisms that govern protein phosphorylation in biological processes.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 8","pages":" 1923-1929"},"PeriodicalIF":2.7,"publicationDate":"2025-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143381151","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yanfeng Li, Shenjie Ji, Luyao Ma, Yuchi Shen, Guanghua Yuan, Jingyi Bian, Bin Liu, Fan Meng, Nongyue He and Chao Wang
{"title":"Elastic scattering spectrum fused with Raman spectrum for rapid classification of colorectal cancer tissues†","authors":"Yanfeng Li, Shenjie Ji, Luyao Ma, Yuchi Shen, Guanghua Yuan, Jingyi Bian, Bin Liu, Fan Meng, Nongyue He and Chao Wang","doi":"10.1039/D4AY02221A","DOIUrl":"10.1039/D4AY02221A","url":null,"abstract":"<p >Currently, HE staining and microscopic imaging are the main approaches for the diagnosis of cancerous tissues, which are inefficient, and the results are heavily dependent on doctors' experience. Therefore, establishing a rapid and accurate method for identifying cancerous tissues is of great value for the preoperative and intraoperative assessments. Raman spectroscopy is a non-destructive, label-free and highly specific method, and it has been widely reported in cancer tissue research. However, the low accuracy of Raman spectral results due to the complex compositions of the tissues limits the clinical applications of Raman spectroscopy. In this study, two-dimensional features of the biochemical composition and morphological structure were combined to classify colorectal cancer tissue by innovatively fusing the elastic scattering spectrum and Raman spectrum. In this study, the elastic scattering spectrum and Raman spectrum of 20 clinical colorectal tissues were acquired using a Raman spectrometer and a homemade elastic scattering light device. After multi-modal spectrum data processing and fusion, a composite AI model called spec-transformer was trained and tested. The results showed that the new model classified colorectal tissues with an accuracy of ≥97%. Moreover, Grad-CAM technology was applied to analyse the compositional variation between normal and colorectal cancer tissues, and it demonstrated a high expression of tryptophan and unsaturated fatty acids in cancer tissues with a reduction in tyrosine and beta-carotene expression. Our approach has potential for colorectal cancer diagnosis and could be extended for diagnosis and research on other cancers.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 9","pages":" 2029-2037"},"PeriodicalIF":2.7,"publicationDate":"2025-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143439408","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Jinran Chen, Xiurui Ke, Zhou Zhou, Wenqi Ye, Hong Liu, Wei Zhang and Xiaohong Liu
{"title":"An Ag-nanoplate decorated cavity-nanorod array SERS substrate for trace detection of PCB-77†","authors":"Jinran Chen, Xiurui Ke, Zhou Zhou, Wenqi Ye, Hong Liu, Wei Zhang and Xiaohong Liu","doi":"10.1039/D5AY00025D","DOIUrl":"10.1039/D5AY00025D","url":null,"abstract":"<p >We report the fabrication of a substrate with cavity-nanorods and decorated with Ag-nanoplates (C-NR@Ag). The cavities on the substrate are formed by metal assistant chemical etching, and the Ag-nanoplates in the cavities by galvanic cell deposition enhance the SERS performance effectively. Analytes in solution are adsorbed on Ag-nanoplates and located in hot spots, which enhance the SERS performance effectively. The enhancement factor of the Ag-nanoplates decorated on nanorod cavities is calculated to be 3.6 × 10<small><sup>6</sup></small>, which is about 3 fold higher than that on the nanorods. The C-NR@Ag substrate is able to detect polychlorinated biphenyls (PCBs) with the lower limit of detection at 1.0 × 10<small><sup>−12</sup></small> M. Additionally, due to the semi-volatile nature of PCB-77, the lower limit of detection of the C-NR@Ag substrate for PCB-77 was 1.0 × 10<small><sup>−11</sup></small> M by the non-contact collection method. These results present a novel approach towards enhancing SERS performance and facilitating the rapid detection of PCB-77.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 9","pages":" 2161-2170"},"PeriodicalIF":2.7,"publicationDate":"2025-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143432049","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Isabella C. O. F. Silva, Raquel G. Rocha, Thiago C. Oliveira, Mariana C. Marra, Luciano C. Arantes, Wallans T. P. dos Santos, Rodrigo A. A. Muñoz and Eduardo M. Richter
{"title":"Low-cost and portable 3D-printed sensor for the determination of secnidazole in pharmaceutical and seized drug samples†","authors":"Isabella C. O. F. Silva, Raquel G. Rocha, Thiago C. Oliveira, Mariana C. Marra, Luciano C. Arantes, Wallans T. P. dos Santos, Rodrigo A. A. Muñoz and Eduardo M. Richter","doi":"10.1039/D4AY02096K","DOIUrl":"10.1039/D4AY02096K","url":null,"abstract":"<p >Additive manufacturing (3D printing), particularly fused deposition modeling (FDM), has rapidly advanced, offering customized designs, reduced waste, lower costs, and fast prototyping for electroanalytical applications. Herein, the electrochemical secnidazole (SCZ) behavior was studied using additive manufactured electrodes (AMEs) based on commercial carbon black and polylactic acid (PLA) conductive filament. Before use, AMEs were submitted to electrochemical/chemical activation (+1.4 V and −1.0 V, both for 200 s) in basic medium (0.5 mol L<small><sup>−1</sup></small> NaOH). Under optimized square wave voltammetry (SWV) conditions and using 0.12 mol L<small><sup>−1</sup></small> Britton Robinson buffer (pH = 2.0) as supporting electrolyte, SCZ exhibited excellent linearity within the concentration range of 2.5 to 250.0 μmol L<small><sup>−1</sup></small> (<em>R</em><small><sup>2</sup></small> = 0.998). The proposed method was successfully applied to detect and quantify SCZ in pharmaceutical and seized samples. The obtained results were statistically similar (95% confidence level) to the values obtained by HPLC. These findings demonstrate that the 3D-printed electrodes developed in this study provide a cost-effective, facile, and highly sensitive platform for on-site SCZ analysis, presenting significant potential for future forensic applications.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 9","pages":" 2038-2045"},"PeriodicalIF":2.7,"publicationDate":"2025-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143389526","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Rafael L. Zamboni, Cristiane Kalinke, Luís M. C. Ferreira, Maurício A. P. Papi, Elisa S. Orth, Craig E. Banks, Luiz H. Marcolino-Júnior and Márcio F. Bergamini
{"title":"Preconcentration-enhanced electrochemical detection of paraoxon in food and environmental samples using reduced graphene oxide-modified disposable sensors†","authors":"Rafael L. Zamboni, Cristiane Kalinke, Luís M. C. Ferreira, Maurício A. P. Papi, Elisa S. Orth, Craig E. Banks, Luiz H. Marcolino-Júnior and Márcio F. Bergamini","doi":"10.1039/D4AY02240H","DOIUrl":"10.1039/D4AY02240H","url":null,"abstract":"<p >Organophosphates, such as paraoxon, are widely used as insecticides in agriculture, making their detection in environmental and food samples crucial due to their high toxicity. This study presents the development of an electrochemical sensor for the detection of paraoxon, using a screen-printed carbon electrode (SPCE) modified with electrochemically reduced graphene oxide (rGO). The modification enhanced the sensor's electrical conductivity and electrochemical performance. A novel preconcentration approach, involving potential pulses at −1.0 and 0.0 V, was employed to improve the adsorption of paraoxon on the electrode surface. Detection was performed by square wave voltammetry, and under optimized conditions, the rGO-SPCE sensor exhibited a linear range from 1.0 to 30 μmol L<small><sup>−1</sup></small>, with detection and quantification limits of 0.26 and 0.86 μmol L<small><sup>−1</sup></small>, respectively. The sensor demonstrated excellent repeatability (RSD = 4.22%), reproducibility (RSD = 7.14%), and selectivity (RSD < 9.22%). The method was successfully applied to tap water, grape and apple juices, and canned corn water samples, achieving recoveries of approximately 98% at the lowest concentration (1.0 μmol L<small><sup>−1</sup></small>) with minimal matrix effects. This approach offers a simple, low-cost, and rapid method for paraoxon detection in water and food samples.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 9","pages":" 2214-2223"},"PeriodicalIF":2.7,"publicationDate":"2025-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143439409","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yaqian Zhang, Shenglan Chen, Xionglong Ye, Weimin Kong, Yang Chen and Yanting He
{"title":"Facile synthesis of hydrangea-like copper–tannic acid networks for separation and purification of His-rich proteins with exceptional performance†","authors":"Yaqian Zhang, Shenglan Chen, Xionglong Ye, Weimin Kong, Yang Chen and Yanting He","doi":"10.1039/D4AY02276A","DOIUrl":"10.1039/D4AY02276A","url":null,"abstract":"<p >Highly selective separation and purification of histidine-rich (His-rich) proteins from complex biological samples is crucial for disease diagnosis, but it still remains a challenge. In this work, hydrangea-like Cu–tannic acid (TA) networks were fabricated <em>via</em> one-step assembly of Cu<small><sup>2+</sup></small> and natural polyphenol for separation and purification of bovine hemoglobin (BHb) from complex biosamples. The preparation procedure was simple, fast and cost-effective. Interestingly, hydrangea-like morphology was obtained by the cross-linked assembly of Cu–TA nanosheets and resulted in a hierarchically porous structure. Benefiting from the large surface area and highly abundant Cu<small><sup>2+</sup></small>, hydrangea-like Cu–TA networks exhibited exceptional adsorption performance towards BHb including ultra-high adsorption capacity (25 116.6 mg g<small><sup>−1</sup></small>) and excellent selectivity. Moreover, hydrangea-like Cu–TA networks possessed good reusability for five adsorption–desorption cycles without the need for regeneration in fresh reaction solution. In addition, hydrangea-like Cu–TA networks were successfully adopted for highly selective separation and purification of BHb from a complex biosample (bovine whole blood). In a word, this work demonstrated that hydrangea-like Cu–TA networks could act as a cost-effective and sustainable adsorbent with exceptional performance, which showed great potential in separation and purification of His-rich proteins for the omics analysis and disease diagnosis.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 9","pages":" 2144-2152"},"PeriodicalIF":2.7,"publicationDate":"2025-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143432050","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Chen Lu, Jiayue Chen, Shengsheng Zhang, Yaru Tian, Xinyu Ying, Dan Zhang, Zhidan Luo, Xinxin Si and Ming Li
{"title":"Development of a vitrified CRISPR/Cas12b-based assay for rapid genotyping of SLCO1B1 SNPs without DNA amplification†","authors":"Chen Lu, Jiayue Chen, Shengsheng Zhang, Yaru Tian, Xinyu Ying, Dan Zhang, Zhidan Luo, Xinxin Si and Ming Li","doi":"10.1039/D4AY02015D","DOIUrl":"10.1039/D4AY02015D","url":null,"abstract":"<p >Two single nucleotide polymorphisms (SNPs) in the human <em>SLCO1B1</em> gene, c.388A>G (rs2306283) and c.521T>C (rs4149056), are independent determinants of the efficacy and side effects of statin drugs. Multinational clinical guidelines recommend testing for <em>SLCO1B1</em> genotypes before the initial use of statins. Current <em>SLCO1B1</em> SNP identification methods, primarily based on quantitative fluorescence PCR, rely on expensive equipment, are time-consuming, and require cold-chain storage for reagents, making them unsuitable for use in resource-limited healthcare settings. In this study, we developed a CRISPR/Cas12b-based amplification-free genotyping technique for <em>SLCO1B1</em> SNPs. Within 30 minutes of the isothermal reaction, genotyping of the c.388A>G and c.521T>C SNPs in the <em>SLCO1B1</em> gene can be observed by the naked eyes under blue light. Additionally, maltodextrin was identified as an effective vitrification stabilizer for the CRISPR/Cas12b premix. A low-cost vitrification process was optimized to prepare a glass like solid reagent <em>via</em> room-temperature vacuum drying. The vitrified CRISPR/Cas12b reagent retained approximately 88% of its activity after 30 days of storage at 37 °C, eliminating the need for cold-chain storage and allowing for long-term preservation at room temperature. This vitrified CRISPR/Cas12b based rapid SNP detection technique is especially suitable for genotyping drug metabolism genes in primary healthcare settings, providing effective guidance for precision medicine in clinical practice.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 9","pages":" 2083-2093"},"PeriodicalIF":2.7,"publicationDate":"2025-02-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143397546","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Susan Varghese, Merin K. Abraham, Ali Ibrahim Shkhair, Geneva Indongo, Greeshma Rajeevan, Arathy B. K., Anju S. Madanan and Sony George
{"title":"Near infrared-emitting carbon dots for the detection of glial fibrillary acidic protein (GFAP): a non-enzymatic approach for the early identification of stroke and glioblastoma†","authors":"Susan Varghese, Merin K. Abraham, Ali Ibrahim Shkhair, Geneva Indongo, Greeshma Rajeevan, Arathy B. K., Anju S. Madanan and Sony George","doi":"10.1039/D4AY02013H","DOIUrl":"10.1039/D4AY02013H","url":null,"abstract":"<p >Immunoassay techniques are widely recognized for their sensitivity and selectivity in biomarker detection; however, their high cost, time-consuming protocols and limited stability often pose significant limitations. In this study, we address these challenges by developing an antibody-free fluorescent platform for the detection of glial fibrillary acidic protein (GFAP), a biomarker released from astrocytes, which plays a critical role in neurological diseases such as ischemic stroke and glioblastoma (GBM). Glutamic acid (GA), a neurotransmitter prevalent in the brain, was selected to quench a near-infrared (NIR) emitting carbon dot-based probe, exploiting the potential interaction between GA and GFAP. The probe demonstrated a turn-on response towards GFAP in the presence of various co-existing biomolecules and ions with a detection limit of 1.8 pg mL<small><sup>−1</sup></small>. A real sample assay conducted in human serum further validated the performance of the probe, achieving a recovery rate of 85% to 97%, underscoring the potential of the probe as a reliable and cost-effective tool for GFAP detection in clinical settings.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 8","pages":" 1850-1859"},"PeriodicalIF":2.7,"publicationDate":"2025-02-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143187821","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}