Analytical Methods最新文献

{"title":"Application of 2D-liquid chromatography for the separation of a mixture of isomeric and structurally related azatryptophan derivatives†","authors":"Parinita Shaw, Pandidurai Sekar, Balasaheb Chavan, Sharad Duche, Arvind Mathur and Amrita Roy","doi":"10.1039/D5AY00473J","DOIUrl":"10.1039/D5AY00473J","url":null,"abstract":"<p >The present study describes the critical achiral and chiral separation of a mixture of azatryptophan derivatives having positional isomers or isobars and their enantiomers, which is successfully achieved using 2D HPLC by employing two different stationary phases and mobile phase combinations in one instrument. The first-dimension experiments were carried out under reversed-phase conditions, where the best separation of racemates was obtained with a Kinetex F5 core–shell column with 10 mM ammonium acetate in water and ACN as a mobile phase in gradient elution mode. The racemate peaks of first dimension experiments were selectively heart-cut based on the time program set in its instrument method and parked in loops for the second-dimension analysis. The parked racemate peaks were sequentially sent into the second dimension to obtain the best separation of the respective isomers, which was achieved using a Chiralcel OD-H column with 0.1% DEA in MeOH : ACN (90 : 10, v/v) as a mobile phase in isocratic elution mode. The study provides valuable insights into the separation methods, where isobars and their respective isomers can be easily and quickly separated using various stationary and mobile phase combinations within a single instrument.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 27","pages":" 5650-5661"},"PeriodicalIF":2.7,"publicationDate":"2025-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144537417","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":"Freeze-drying enhances ToF-SIMS imaging of biological tissues via structural and metabolic preservation","authors":"Hongzhe Ma, Mingru Liu, Yuxuan Zhang, Mengjiao Sun, Yanhua Chen, Zhaoying Wang and Zeper Abliz","doi":"10.1039/D5AY00550G","DOIUrl":"10.1039/D5AY00550G","url":null,"abstract":"<p >In the ToF-SIMS <em>in situ</em> analysis of mouse liver tissue, freeze-drying is superior to room-temperature drying and chemical fixation, minimizing lipid spillage while maintaining structural integrity. Freeze-drying preserves tissue structure with minimal lipid loss, whereas room-temperature drying leads to lipid spreading and chemical fixation results in background noise. Freeze-drying balances structural integrity, molecular preservation, and spectral clarity, making it the optimal ToF-SIMS prep method. Although the method was tested on lipid-rich liver tissue, it provides a framework for tissue specific preparation of ToF-SIMS.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 26","pages":" 5480-5488"},"PeriodicalIF":2.7,"publicationDate":"2025-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144482559","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 IagPLS baseline correction method for glioma identification using Raman spectroscopy","authors":"Yiran Shao, Lipu Zhou, Yan Zhou, Yibo Li and Qingbo Li","doi":"10.1039/D5AY00792E","DOIUrl":"10.1039/D5AY00792E","url":null,"abstract":"<p >As the most aggressive malignant tumours of the central nervous system, gliomas urgently require real-time intraoperative molecular diagnostic techniques to overcome the invasive limitations of conventional pathology and the uncertainties of imaging. Although Raman spectroscopy can provide non-invasive biomolecular fingerprinting information, its signal is susceptible to interference from baseline drift caused by tissue autofluorescence, resulting in masking of the effective information of the spectrum. Existing baseline correction methods (<em>e.g.</em>, polynomial fitting and asymmetric least squares) struggle to balance the challenges of noise suppression, feature preservation, and adaptation to heterogeneous tissue spectra. In this study, we propose an improved adaptive gradient-derived penalized least squares (IagPLS) method that integrates three innovative mechanisms: curvature-driven dynamic regularization, which dynamically adjusts the smoothing intensity through a gradient-sensitive penalty term and protects biomarker-rich regions while suppressing high-frequency noise; SHAP algorithm-guided feature protection, which identifies and diagnoses key Raman peaks and constructs region-specific weight constraints to avoid oversmoothing; and quantum-inspired global optimization, which models the weight update as a tunnelling potential well model and uses a Monte Carlo simulated annealing strategy to jump out of the local optimum. Based on the validation of 423 clinical Raman spectra (157 normal tissues/266 glioma tissues), IagPLS showed a significant advantage: the glioma identification accuracy of its corrected spectra reached 96.1% (tumour F1 score: 0.97) after random forest classification, which was significantly better than that of airPLS (89.4%) and agdPLS (87.0%). The key indicators show that the feature peak prominence of the spectra during IagPLS processing is improved by 82.05% compared to agdPLS, the negative residual area is reduced by 89.79% compared to airPLS, and the processing speed is improved by 43.64% compared to airPLS. SHAP interpretability analysis confirmed that the protected biomarker regions contributed 1.07-fold to classification and were highly compatible with glioma-specific spectral features. The algorithm takes less than 0.1 seconds for a single correction, combining biological interpretability with superior spectral correction to provide a reliable pre-processing tool for intraoperative optical biopsy systems. Its algorithmic framework can be extended to multimodal biomedical spectral analysis, such as near-infrared and mid-infrared spectroscopy, to promote the innovation of complex spectral pre-processing technology in precision medicine.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 26","pages":" 5343-5354"},"PeriodicalIF":2.7,"publicationDate":"2025-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144332063","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":"Introduction to neutron techniques for cultural heritage","authors":"Analytical Methods Committee, AMCTB No. 118","doi":"10.1039/D5AY90075A","DOIUrl":"10.1039/D5AY90075A","url":null,"abstract":"<p >Since the early 2000s, neutron techniques have become available for the non-invasive characterisation of cultural heritage artefacts, especially those made of metal, ceramic or stone. This is thanks to the ability of neutrons to penetrate deeply into objects, to study their inner volume non-invasively. The neutron methods available can efficiently provide information on the composition and micro-structural properties of materials, along with 2D and 3D images of an artefact's internal structure, helping to answer questions related to manufacturing processes, state of degradation, authenticity and provenance. This Technical Brief presents an overview of the main neutron-based methods and the different types of neutrons suitable for the characterisation of materials of interest in cultural heritage and includes case studies highlighting the impact of these applications in archaeological and historical research.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 26","pages":" 5527-5531"},"PeriodicalIF":2.7,"publicationDate":"2025-06-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144323877","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":"Protein quantification in complex samples using gel electrophoresis with online intrinsic fluorescence imaging and Gaussian fitting arithmetic†","authors":"Xinke Zhai, Yiren Cao, Youli Tian, Ke-er Chen, Zixian Yu, Qiang Zhang, Chengxi Cao and Xu Xu","doi":"10.1039/D4AY02064B","DOIUrl":"10.1039/D4AY02064B","url":null,"abstract":"<p >Traditional polyacrylamide gel electrophoresis (PAGE) has been widely used for analysis of proteins. However, protein quantification (PQ) based on SDS-PAGE with staining remains inaccurate, time-consuming and complex. Even though PAGE with online intrinsic fluorescence imaging (IFI) has well addressed these issues, it still suffers from the narrow detection window of 8 lanes and poor quantitation owing to low resolution. Herein, we improved the gel electrophoresis tank (GET) for a wider detection window of 10 lanes with uniform UV radiation and developed a Gaussian fitting arithmetic for accurate PQ at low resolutions. To demonstrate the improvement, we used bovine serum albumin (BSA) in whey samples as a model protein and conducted the relevant experiments. As demonstrated by the experiments, the IFI system could be well used for the simultaneous real-time imaging analysis of 10 lanes. In particular, the Gaussian fitting-based analyzer could be used for the computation of peak area with low resolution, greatly improving the function of PAGE-IFI for protein analysis of complex samples. In addition, the developed method exhibited a good limit of detection (LOD) of 14 ng and limit of quantification (LOQ) of 42 ng, a fair dynamic range of 50–8000 ng, recovery of 106.37% for a urine sample, recovery of 94.96% for the whey sample, intra-day RSD value of 9.17%, and inter-day RSD value of 10.06%. All these results indicated the potential of the developed GET, Gaussian fitting-based analyzer and the proposed method for the determination of protein in complex samples.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 27","pages":" 5749-5758"},"PeriodicalIF":2.7,"publicationDate":"2025-06-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144537483","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":"An innovative multispectral sensor for rapid wine adulteration detection using wavelength selection algorithms†","authors":"Chengbo Yang, Jingjun Wu, Zhouqing Qian and Zhiliang Zhao","doi":"10.1039/D5AY00751H","DOIUrl":"10.1039/D5AY00751H","url":null,"abstract":"<p >Effective detection of wine adulteration can protect the rights and interests of consumers and producers. The combination of spectroscopic technology and chemometric methods can achieve adulteration discrimination of wine, providing feasibility for developing consumer-grade wine adulteration detection equipment. This study attempts to use a wavelength selection algorithm to guide the development of a four-channel, low-cost spectroscopic device for rapid identification of wine adulteration. Firstly, this study utilized a miniature spectrometer to obtain the Vis-NIR spectra of wine (only the Vis portion was used). Secondly, by integrating the successive projections algorithm (SPA), spectral degradation, and traversal methods, four wavelengths and their parameters related to wine adulteration discrimination are determined for the selection of filters. Then, a CCD camera and four filters were packaged into a 4-channel spectral sensor. Finally, a random forest (RF) discrimination model was established, and an improved spectral index (SI) combined method was used to enhance the model's performance. The results indicate that the snapshot-based multispectral sensor can achieve high accuracy in identifying wine adulteration (97.47%) and has the characteristics of small size and low cost. At the same time, the research findings also demonstrate that by integrating the SPA, SI, spectral degradation, and traversal methods, effective central wavelengths and resolution specifications can be provided for the construction of dedicated spectral sensors.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 27","pages":" 5774-5781"},"PeriodicalIF":2.7,"publicationDate":"2025-06-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144537416","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":"First-in-class hydrazone–pyrazoline sensors for selective detection of Zn2+, Cd2+, and Hg2+ in aqueous environments†","authors":"Alexander Ciupa","doi":"10.1039/D5AY00639B","DOIUrl":"10.1039/D5AY00639B","url":null,"abstract":"<p >Six first-in-class hydrazone–pyrazoline fluorescent sensors that selectively detect Zn<small>²⁺</small>, Cd<small>²⁺</small>, and Hg<small>²⁺</small> at three distinct wavelengths in aqueous environments are reported. These novel hybrid sensors are synthesized in just two steps from inexpensive, commercially available materials, enabling rapid generation and screening for desirable photophysical properties. Lead sensor <strong>P1</strong> was validated for <em>in situ</em> detection of group 12 metals in river and pond water using a portable, low-cost device. Crucially, this system enabled rapid, naked-eye detection of toxic metals directly in the environment without the need for expensive instrumentation or mains electricity. These findings establish a new direction in pyrazoline sensor research and set a high benchmark for future sensor development.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 27","pages":" 5782-5787"},"PeriodicalIF":2.7,"publicationDate":"2025-06-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ay/d5ay00639b?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144537482","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}

{"title":"Recent advances in upconversion nanoparticles for biomolecule detection: a review","authors":"Shuoshuo Cheng, Bin Huang, Kangqiang Lu, Jinhui Li, Herui Wen and Jialin Zhang","doi":"10.1039/D5AY00631G","DOIUrl":"10.1039/D5AY00631G","url":null,"abstract":"<p >Given the continuously increasing requirements for biological detection, upconversion nanoparticle (UCNP)-based techniques offer a novel research direction for biomolecule detection. Due to their superior and stable photophysical characteristics, UCNPs have received widespread attention and have been extensively applied for reliable and highly sensitive detection of biomolecules. Herein, we review articles based on three aspects: UCNP synthesis, surface functionalization, and application in biomolecule detection. The future development trend of UCNPs is also anticipated. Several synthesis methods are introduced, and the advantages and disadvantages of these synthesis methods are summarized and compared. Control of UCNP size and shape, as well as UCNP doping, is discussed. For surface modification, we introduce approaches such as surface silanization, ligand exchange, ligand oxidation, ligand attraction and electrostatic layer by layer assembly. In addition, we focus on UCNP-based luminescence sensors for the analysis of biomolecules, such as nucleic acids, amino acids, proteins, carbohydrates, uric acid and lipids. These upconversion nanomaterials were used as carriers for recognition, transmission or signal amplification and significantly improved the performance of biomolecule detection. Finally, the shortcomings of UCNP are analyzed and its future prospects are presented. This review provides new insights into the application of upconversion nanoparticles as an important element in biomolecule detection.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 27","pages":" 5563-5578"},"PeriodicalIF":2.7,"publicationDate":"2025-06-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144537485","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 highly sensitive flow injection chemiluminescence method for myoglobin detection in beef samples based on zinc ion-induced “dragging” of heme iron†","authors":"Yali Zhang, Yuhan Ma, Yapin Zhao and Jing Ha","doi":"10.1039/D5AY00774G","DOIUrl":"10.1039/D5AY00774G","url":null,"abstract":"<p >We report for the first time that zinc ions (Zn<small>²⁺</small>) significantly enhance the chemiluminescence (CL) signal of the luminol–hydrogen peroxide (luminol–H<small>₂</small>O<small>₂</small>) system by “dragging” heme iron out of myoglobin (Mb). Integrating this with myoglobin aptamer (Mb aptamer) specific recognition enables sensitive and specific quantification of Mb content in beef samples.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 25","pages":" 5155-5159"},"PeriodicalIF":2.7,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144309315","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":"Concentration dependence of Kubelka–Munk function and apparent absorbance button sample holder infrared spectra","authors":"Robert L. White","doi":"10.1039/D5AY00758E","DOIUrl":"10.1039/D5AY00758E","url":null,"abstract":"<p >Button sample holder infrared spectra in Kubelka–Munk function and apparent absorbance formats are evaluated. Trends in plots of vibration band area and peak intensity <em>versus</em> concentration are compared. Two test sample powders were comprised of different concentrations of caffeine dispersed in potassium chloride and copper thiosulfate mixed with kaolinite and potassium chloride in different ratios. When infrared spectra of caffeine and copper thiosulfate were measured by diffuse reflection, Kubelka–Munk calibration functions tended to be linear whereas apparent absorbance functions were curved. However, over narrow concentration ranges, both formats provided linear plots and exhibited similar sensitivities. For samples with the highest clay content, the kaolinite O–H stretching and inorganic oxide vibration band area <em>versus</em> concentration plots were linear over wider ranges than the Kubelka–Munk function plots.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 26","pages":" 5519-5526"},"PeriodicalIF":2.7,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ay/d5ay00758e?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144332064","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}