Analytical Methods最新文献

{"title":"BiFusionPathoNet: fusion network for drug-resistant bacteria identification <i>via</i> optical scattering patterns.","authors":"Yichuan Wang, Xu He, Mubashir Hussain, Luyao Ma, Jingjing Wang, Mingyue Chen, Na Yang, Xiuping Zhou, Chao Wang, Haiquan Kang, Bin Liu","doi":"10.1039/d4ay02074j","DOIUrl":"https://doi.org/10.1039/d4ay02074j","url":null,"abstract":"<p><p>The presented research introduces a new method to identify drug-resistant bacteria rapidly with high accuracy using artificial intelligence combined with Multi-angle Dynamic Light Scattering (MDLS) signals and Raman scattering signals. The main research focus is to distinguish methicillin-resistant <i>Staphylococcus aureus</i> (MRSA) and methicillin-sensitive <i>Staphylococcus aureus</i> (MSSA). First, a microfluidic platform was developed embedded with optical fibers to acquire the MDLS signals of bacteria and Raman scattering signals obtained by using a Raman spectrometer. After that, for the detection of both scattering signals of MRSA and MSSA, three models were developed: (1) ResistNet, a hybrid model combining a Transformer Encoder with ResNet, with an accuracy of 83.8% on the MDLS dataset.; (2) SERB-CNN, which attained 91.84% accuracy on a Raman scattering public dataset and 93.5% on a custom-built dataset; and (3) BiFusionPathoNet, a multimodal fusion model that reached 96.8% accuracy, significantly outperforming single-modal approaches. The acquired results demonstrated the effectiveness of this multimodal strategy for the rapid detection of drug-resistant bacteria.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142968783","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":"A new stability indicating HPLC method with QDa and PDA detectors for the determination of process and degradation impurities of ivabradine including separation of diastereomeric <i>N</i>-oxides.","authors":"Büşra Gülşen, Sıdıka Ertürk Toker","doi":"10.1039/d4ay01986e","DOIUrl":"https://doi.org/10.1039/d4ay01986e","url":null,"abstract":"<p><p>In this study, a new reversed phase high performance liquid chromatography method using two detectors was developed for the analysis of degradation and process impurities of ivabradine in pharmaceutical preparations. A PDA detector set to 285 nm wavelength and a QDa detector set to positive scan mode were used in the method. In the developed method, the separation process was carried out in a Zorbax phenyl column with a gradient application of a 0.075% trifluoroacetic acid, acetonitrile, and methanol mixture at a flow rate of 1.5 ml min^-1. During the degradation studies, the samples were exposed to acidic, alkaline, oxidative, thermal, and photolytic conditions. Process-related impurities were separated not only without interfering with each other but also with the degradation product and ivabradine peaks, and thanks to QDa, all impurities could be identified with their molecular weights. This method, in addition to providing stability data, was also able to separate two diastereomeric <i>N</i>-oxide impurities which are major oxidative degradation impurities of ivabradine having a chiral center. Some additional measurements such as solubility, specific rotation, melting point and differential scanning calorimetry analysis proved the formation of the two diastereomeric <i>N</i>-oxide impurities under oxidative conditions. Method validation was performed according to the International Council for Harmonization guidelines and the analysis of ivabradine, its process related impurities (dehydro ivabradine, acetyl ivabradine, and hydroxy ivabradine) and a major oxidative degradation product (ivabradine <i>N</i>-oxide) was successfully performed by this method.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142968770","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":"A CNN-based self-supervised learning framework for small-sample near-infrared spectroscopy classification.","authors":"Rongyue Zhao, Wangsen Li, Jinchai Xu, Linjie Chen, Xuan Wei, Xiangzeng Kong","doi":"10.1039/d4ay01970a","DOIUrl":"https://doi.org/10.1039/d4ay01970a","url":null,"abstract":"<p><p>Near-infrared (NIR) spectroscopy, with its advantages of non-destructive analysis, simple operation, and fast detection speed, has been widely applied in various fields. However, the effectiveness of current spectral analysis techniques still relies on complex preprocessing and feature selection of spectral data. While data-driven deep learning can automatically extract features from raw spectral data, it typically requires large amounts of labeled data for training, limiting its application in spectral analysis. To address this issue, we propose a self-supervised learning (SSL) framework based on convolutional neural networks (CNN) to enhance spectral analysis performance with small sample sizes. The method comprises two learning stages: pre-training and fine-tuning. In the pre-training stage, a large amount of pseudo-labeled data is used to learn intrinsic spectral features, followed by fine-tuning with a smaller set of labeled data to complete the final model training. Applied to our own collected dataset of three tea varieties, the proposed model achieved a classification accuracy of 99.12%. Additionally, experiments on three public datasets demonstrated that the SSL model significantly outperforms traditional machine learning methods, achieving accuracies of 97.83%, 98.14%, and 99.89%, respectively. Comparative experiments further confirmed the effectiveness of the pre-training stage, with the highest accuracy improvement, reaching 10.41%. These results highlight the potential of the proposed method for handling small sample spectral data, providing a viable solution for improved spectral analysis.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142968767","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":"A rapid and highly sensitive fluorescence immunochromatographic test strip for pepsin detection in human hypopharyngeal saliva.","authors":"Yaqi Liu, Lihong Chen, Jingtian Huang, Jialing Zhang, Shuting Chen, Zhenyu Lin, Ting Chen","doi":"10.1039/d4ay01833h","DOIUrl":"https://doi.org/10.1039/d4ay01833h","url":null,"abstract":"<p><p>Pepsin serves as a potential biomarker for laryngopharyngeal reflux disease (LPRD). The reported methods for detecting pepsin still have limitations, such as long reaction times and low sensitivity. Therefore, it is crucial to develop a rapid, simple and sensitive detection method. In this study, a fluorescence immunochromatographic test strip was designed for point-of-care diagnostics of LPRD. To obtain optimal fluorescence immunochromatographic conditions, key experimental factors, including microsphere particle size, binding pH, and resuspension dilution ratio, were systematically evaluated. The optimal fluorescent microsphere size was determined to be 300 nm, the most suitable reaction pH was 8.0, and the ideal resuspension solution to storage solution ratio was 1 : 4. Under these optimal conditions, the sensor had a linear range of 2.5-100.0 ng mL^-1 and a detection limit of 1.9 ng mL^-1. The relative standard deviation was below 15% for both intra- and inter-batch reproducibility. Under accelerated damage conditions at 37 °C, the test value of the test strip could be kept basically unchanged for 14 days. There was no cross-reactivity of the test strip with pepsinogen I, pepsinogen II and other interferents. In the actual sample detection, the recovery rate was between 85% and 115%. Furthermore, the proposed method was demonstrated to be green and to exhibit strong applicability based on the evaluation using the AGREEprep and the BAGI. In addition, the method has the advantages of high sensitivity, accuracy, greenness and applicability, which can meet the needs of rapid quantitative on-site detection.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142968779","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":"Determination of paclobutrazol using square wave voltammetry based on a molecularly imprinted polymer and boron-doped copper oxide/graphene nanocomposite.","authors":"Çağdaş Salih Meriç, Haci Ahmet Deveci, Müge Mavioğlu Kaya, Ayla Deveci, Neslihan Özdemir, Havva Boyacıoğlu, Mehmet Lütfi Yola","doi":"10.1039/d4ay01947d","DOIUrl":"https://doi.org/10.1039/d4ay01947d","url":null,"abstract":"<p><p>In the present study, a novel voltammetric sensor based on a boron-doped copper oxide/graphene (B-CuO-Gr) nanocomposite and molecularly imprinted polymer (MIP) was developed for the detection of paclobutrazol (PAC) in apple and orange juice samples. The B-CuO-Gr nanocomposite was prepared using sol-gel and calcination methods. After modifying glassy carbon electrodes with the B-CuO-Gr nanocomposite, PAC-imprinted electrodes were prepared in the presence of 100.0 mM pyrrole (Py) monomer and 25.0 mM PAC using cyclic voltammetry (CV). After elucidating the surface properties of the prepared B-CuO-Gr nanocomposite and PAC-imprinted electrodes using various characterization techniques, the PAC-imprinted sensor was successfully applied to apple and orange juice samples, demonstrating high recovery. A linear range of 1.0 × 10^-9 to 1.0 × 10^-8 M PAC (<i>R</i>² = 0.9983) and a detection limit (LOD) of 3.30 × 10^-10 M were observed, along with high selectivity, stability, and reproducibility for the MIP/B-CuO-Gr/GCE sensor.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142968791","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":"In-cell NMR reveals metabolic adaptations in central carbon pathways driving antibiotic tolerance in <i>Salmonella</i> Typhimurium.","authors":"Alexandra L N Zahid, Ke-Chuan Wang, Line Elnif Thomsen, Sebastian Meier, Pernille Rose Jensen","doi":"10.1039/d4ay02023e","DOIUrl":"https://doi.org/10.1039/d4ay02023e","url":null,"abstract":"<p><p>Antibiotic tolerance presents a significant challenge in eradicating bacterial infections, as tolerant strains can survive antibiotic treatment, contributing to the recurrence of infections and the development of resistance. However, unlike antibiotic resistance, tolerance is not detectable by standard susceptibility assays such as minimal inhibitory concentration (MIC) tests. Consequently, antibiotic tolerance often goes unnoticed in clinical settings. Bacterial metabolism is closely linked to antibiotic efficacy, and thus presents as a potential target for novel diagnostic methods. Recent advancements in nuclear magnetic resonance (NMR) spectroscopy, including dynamic nuclear polarization (DNP-NMR), enable a non-invasive real-time approach to analyzing bacterial metabolism. In this study, we applied both ¹H and in-cell ¹³C NMR spectroscopy to investigate metabolic adaptations in a tolerance-evolved <i>Salmonella</i> Typhimurium strain, C10, developed through ten cycles of ampicillin treatment. Our results demonstrated that despite similar MICs and growth rates, the C10 strain exhibited a 25-fold increase in tolerance compared to the wild-type, while exhibiting lower metabolic activity. Under ampicillin stress, however, the C10 strain maintained higher metabolic activity and demonstrated greater resilience in glucose consumption and metabolite production relative to the wild-type. Using DNP-NMR, rapid metabolic shifts in the C10 strain were identified within 10 minutes of exposure to high concentrations of ampicillin, characterized by accumulation of key metabolites such as pyruvate and acetate. Overall, our findings underscore the potential of real-time NMR-based analyses to provide deeper insights into antibiotic tolerance and distinguish between susceptible and tolerant bacterial strains.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142941518","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":"Galactose oxidase oxidation and glycosidase digestion for glycoRNA analysis.","authors":"Jianbo Deng, Xinyu Miao, Xiaotong Wang, Sheng-Ye Wen, Zeyang Zhou, Shuwei Li, Junhong Jiang, Xiaodong Yang, Shuang Yang","doi":"10.1039/d4ay02046d","DOIUrl":"https://doi.org/10.1039/d4ay02046d","url":null,"abstract":"<p><p>Ribonucleic acid (RNA), essential for protein production and immune function, undergoes glycosylation, a process that attaches glycans to RNA, generating unique glycoRNAs. These glycan-coated RNA molecules regulate immune responses and may be related to immune disorders. However, studying them is challenging due to RNA's fragility. Therefore, a robust method for identifying glycoRNA is important. To address this, we optimized parameters for RNA stability, oxidation, and digestion, thereby enriching and identifying glycoRNAs. This breakthrough paves the way for exploring their potential interactions with immune receptors and tumor suppression. Our approach involved investigating factors such as preservation reagent, enzyme buffer, digestion temperature, oxidant, glycosidase, and incubation time. We successfully optimized digestion conditions, achieving efficient cleavage of <i>N</i>-linked glycoRNAs at room temperature using 25 mM ammonium bicarbonate, demonstrating the effectiveness of this method. Additionally, RNA preservation in RNAlater at -80 °C allows controlled release of glycoRNAs within hours. While sequential digestion of different glycoRNA types is possible, significant degradation occurs after the first glycosidase step. Therefore, we recommend separate harvesting for each glycoRNA type. We also established RNA-seq analysis for identifying various glycoRNA types, including snoRNAs and tRNAs. The optimized SPCgRNA method paves the way for further research on <i>N</i>-glycosylation in health and disease.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142941511","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":"A novel fluorescent probe for rapid and selective detection of fluoride ions in living cells.","authors":"Tingting Feng, Jiaxue Yang, Yi Wang, Taozhu Hu, Longjia Yan, Yi Le, Li Liu","doi":"10.1039/d4ay02173h","DOIUrl":"https://doi.org/10.1039/d4ay02173h","url":null,"abstract":"<p><p>A novel fluorescent probe DTP, based on fluorine-silicon complexation, extends emission to 590 nm and achieves a 5 minutes response time. It shows high selectivity and a 0.98 μM detection limit for fluoride ions, with successful bioimaging application in living cells.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142941464","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":"Development of a new method using dispersive liquid-liquid microextraction with hydrophobic natural deep eutectic solvent for the analysis of multiclass emerging contaminants in surface water by liquid chromatography-mass spectrometry.","authors":"Fernanda Volpatto, Luciano Vitali","doi":"10.1039/d4ay02012j","DOIUrl":"https://doi.org/10.1039/d4ay02012j","url":null,"abstract":"<p><p>A new analytical method was developed for the determination of 14 multiclass emerging organic contaminants in surface waters using LC-MS, and Dispersive Liquid-Liquid Microextraction (DLLME) for extraction. Different Natural Deep Eutectic Solvents (NADESs) composed of terpenes and organic acids were tested as extraction solvents and characterized by Fourier Transform Infrared Spectroscopy (FTIR), Hydrogen Nuclear Magnetic Resonance Spectroscopy (¹H-NMR), Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), density, and viscosity, eliminating the need to use traditional chlorinated solvents. NADES produced with butyric acid and thymol showed the best results and was selected for application for the first time in the extraction of emerging organic contaminants of different classes in water samples. Vortex was used as the dispersion mode, eliminating the use of the dispersion solvent. Chromatographic conditions and sample preparation were optimized using multivariate experimental designs. The optimized chromatographic conditions included the column oven temperature, mobile phase modifiers, and stationary phase type. The optimized conditions for sample preparation included the extraction temperature and pH, salting out effect, and extraction solvent volume. The analytical performance was evaluated through repeatability and intermediate precision tests, with RSD values below 20%, and recoveries between 70 and 120%. The coefficient of determination was greater than 0.98 for all analytes. LOQs varied between 1.5 and 35 μg L^-1. DLLME is a simple technique, it does not require expensive and specific equipment. Furthermore, replacing traditional chlorinated solvents with NADES makes the procedure more environmentally friendly. The method presented here can be applied to a wide range of analytes for the analysis of fresh, brackish, and salt waters. Up to the present moment, this is the first study using NADES based thymol and butyric acid for the determination of multiclass emerging contaminants in surface waters samples.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-01-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142941503","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":"Qualitative and quantitative nondestructive determination of cyanide in water and distilled spirits by Raman integrating sphere.","authors":"Xu Hai-Sheng, Cheng Jing, Yang Da-Peng, Zhao Chu-Qiu, Liu Yan, Tao Sha, Huang Bao-Kun","doi":"10.1039/d4ay02157f","DOIUrl":"https://doi.org/10.1039/d4ay02157f","url":null,"abstract":"<p><p>Cyanide often forms as a byproduct during the fermentation process of distilled spirits, and excessive amounts can cause damage to health. Cyanide poisoning is also common in alcoholic beverages and water. Therefore, the cyanide content measurement in water and distilled spirits is essential. Here, a Raman integrating sphere technique for the <i>in situ</i> detection of cyanide has been established, and a lower limit of detection of 1.56 mg L^-1 in water and ethanol was achieved, owing to the efficient collection of Raman signals and the efficient use of laser power. The Raman peak of cyanide is located at 2080 cm^-1. The detection range was from 1.56 to 25 mg L^-1 cyanide in water, ethanol, and liquor with high linearity (<i>R</i>² = 0.9986, 0.9986, and 0.9908) and precision (%RSD = 5.53%, 6.92%, and 14.12%). This instrument provides an alternative method for detecting cyanide, which can not only be used for accurate qualitative and quantitative detection of cyanide but also for food safety detection and physical evidence analysis of cyanide in beverage poisoning. Key to our method is that it offers advantages such as no need for sample pretreatment, simplicity and speed of operation, non-destructive analysis, minimal sample consumption (only 3 milliliters are required for a single measurement), and the ability to preserve the analyzed sample as evidence.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-01-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142941524","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}