Qianyi Wang, Seyed Amirhossein Sadeghi, Fei Fang, Dejin Zheng, Chenxiang Luo, Guangyao Gao, Qianjie Wang, Bin Gu, Liangliang Sun
{"title":"High-throughput plasma/serum proteomics by coupling nanoparticle protein corona-based sample preparation and capillary zone electrophoresis-tandem mass spectrometry.","authors":"Qianyi Wang, Seyed Amirhossein Sadeghi, Fei Fang, Dejin Zheng, Chenxiang Luo, Guangyao Gao, Qianjie Wang, Bin Gu, Liangliang Sun","doi":"10.1039/d5ay00721f","DOIUrl":"10.1039/d5ay00721f","url":null,"abstract":"<p><p>A high-throughput workflow for bottom-up proteomics (BUP) of human plasma using capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) and nanoparticle protein corona-assisted sample preparation is presented. The streamlined approach enabled the identification and quantification of hundreds of proteins from plasma/serum samples in 3.5 hours from sample to data. Nanoparticles with varied physiochemical properties studied in this work captured different pools of the plasma/serum proteome in the protein coronas, and the protein corona-based sample preparation approach enabled the measurement of low-abundance proteins compared to the approach without nanoparticles. Applying this high-throughput workflow to serum samples of a mouse NUT carcinoma (NC) cancer model allowed the determination of differentially expressed serum proteins between NC bearing mice and healthy controls. By comparing our quantitative proteomics data with published transcriptomics data, we revealed a handful of potential serum protein biomarkers of NC cancer (<i>e.g.</i>, secreted phosphoprotein 1, SPP1). We expect this high-throughput workflow, with additional improvement in the speed of the mass spectrometer, will be useful for advancing the discovery of new protein biomarkers of diseases (<i>e.g.</i>, cancer) using plasma/serum samples.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12305297/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144726091","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}
Fahad M Alminderej, Alaa M Younis, Alaa S Amin, Hesham H El-Feky
{"title":"Ultrasound-assisted ionic liquid microextraction and colorimetric analysis for trace-level gold detection in environmental and geological samples.","authors":"Fahad M Alminderej, Alaa M Younis, Alaa S Amin, Hesham H El-Feky","doi":"10.1039/d5ay01045d","DOIUrl":"https://doi.org/10.1039/d5ay01045d","url":null,"abstract":"<p><p>A novel, precise, and targeted method has been developed for isolating, preconcentrating, and analyzing gold ions in water, ore, and food samples. This approach utilizes ultrasound-assisted dispersive liquid-liquid microextraction based on ionic liquids, combined with colorimetric detection of a distinct deep red hue. The compound 2-amino-4-(<i>m</i>-tolylazo)pyridine-3-ol (ATAP), introduced for the first time as a gold-specific chelating agent, was employed alongside the ionic liquid 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide in an ultrasonic bath maintained at 25 ± 2 °C for extraction. Following centrifugation, the gold complex was enriched within the ionic liquid droplets, and 200 μL of ethanol was added to the ionic liquid-rich layer prior to colorimetric analysis. Key variables influencing the recovery of Au<sup>3+</sup> ions were systematically examined and fine-tuned to achieve optimal results. After fine-tuning both the instrumental and experimental conditions, the proposed method demonstrated a linear dynamic range for Au<sup>3+</sup> ions between 4.0 and 240 ng mL<sup>-1</sup>, with high molar absorptivity and a Sandell sensitivity of 1.22 × 10<sup>6</sup> L mol<sup>-1</sup> cm<sup>-1</sup> and 0.016 ng cm<sup>-2</sup>, respectively. The method achieved quantification and detection limits of 3.92 and 1.30 ng mL<sup>-1</sup>, respectively. A preconcentration factor of 500 was obtained. The relative standard deviation (RSD) was calculated to be 1.89% for gold ions at a concentration of 100 ng mL<sup>-1</sup> (<i>n</i> = 10). No significant interference from various anions and cations was detected during the assessment of Au<sup>3+</sup>. These findings confirm that the proposed technique is a fast, straight-forward, highly sensitive, selective, and effective analytical approach for isolating and quantifying Au<sup>3+</sup> ions in environmental and geological samples, all while using minimal solvent volumes.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144726092","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":"Dual-response fluorescent carbon dots for Ag<sup>+</sup> and Hg<sup>2+</sup> detection study in actual samples and biological systems.","authors":"Xinyan Liu, Chao Liu, Qingyue Hu, Huihui Ge, Jie Tan, Jianhua Wang, Wei Bian","doi":"10.1039/d5ay00688k","DOIUrl":"https://doi.org/10.1039/d5ay00688k","url":null,"abstract":"<p><p>It is important to be capable of achieving highly selective detection of Ag<sup>+</sup> and Hg<sup>2+</sup> because their excessive concentrations may pose a serious threat to human health and lead to a variety of diseases. Herein, a new type of orange fluorescent carbon dot with an emission wavelength of 590 nm was synthesized by a hydrothermal method using 1,2,4-triaminobenzene dihydrochloride and ethylenediamine as raw materials. The synthesized orange carbon dots have high affinity for Hg<sup>2+</sup> and Ag<sup>+</sup> ions, which can be selectively detected by fluorescence quenching with the detection limits of 0.37 nM and 0.65 nM, respectively. Moreover, the carbon dots have good fluorescence stability for the rapid detection of Ag<sup>+</sup> and Hg<sup>2+</sup> over a wide pH range. Importantly, the addition of EDTA reversibly restored the fluorescence intensity of the mixed solution of carbon dots and Hg<sup>2+</sup>, but not the fluorescence intensity of the Ag<sup>+</sup>-containing probe solution, which allowed for a clear distinction between Hg<sup>2+</sup> and Ag<sup>+</sup>. In addition, the carbon dots have good biocompatibility and low toxicity to MCF-7 cells, which can be used for cell imaging and intracellular ion detection.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144726090","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 improved system and analytical method for determining oxygen isotopes in <sup>18</sup>O-enriched water samples.","authors":"Hongwei Li, Lianjun Feng","doi":"10.1039/d5ay00505a","DOIUrl":"https://doi.org/10.1039/d5ay00505a","url":null,"abstract":"<p><p>The spatiotemporal differences in the hydrogen and oxygen isotopic composition of water offer a powerful technical approach for research on the water cycle, paleoclimate reconstruction, and water source identification. Hydrogen and oxygen isotopes in certain specialized samples, such as <sup>18</sup>O-enriched water, have been utilized in food science, environmental ecology, and medical research. To address the low efficiency of traditional offline H<sub>2</sub>O-CO<sub>2</sub> equilibrium methods and the pronounced memory effect associated with continuous-flow techniques for <sup>18</sup>O-enriched water samples, we propose a novel analytical system and methodology for oxygen isotope determination in water. The system was independently designed and established in-house. A water equilibrium unit and an extraction preparation unit were organically combined in this system. A water bath shaker was designed for the equilibrium system to accelerate the complete equilibrium exchange and reduce reaction time. A 3.0 mL water sample was injected into a glass bottle and equilibrated with carbon dioxide gas in a water bath at 25 °C for 4 h. While maintaining a high analytical accuracy (within 0.10% and 0.50% for reference materials USGS45 and IAEA-608, respectively), this method significantly improves the efficiency, reducing the processing time by over 10 h. It offers a preferred solution for oxygen isotope analysis in water samples, particularly those enriched in <sup>18</sup>O.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144726088","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":"Comonomer distribution analysis of poly(3-hydroxybutyrate-<i>co</i>-3-hydroxyhexanoate)s using high-resolution MALDI-TOF mass spectrometry.","authors":"Naoki Kanayama, Sayaka Nakamura, Shin Sano, Mami Tanaka, Noriko Takahara, Hiroaki Sato, Hideaki Hagihara","doi":"10.1039/d5ay00910c","DOIUrl":"https://doi.org/10.1039/d5ay00910c","url":null,"abstract":"<p><p>In practical applications of poly(3-hydroxybutyrate) (PHB) copolyesters, the distribution of comonomer units within the polymer chains (<i>i.e.</i>, comonomer distribution) is an important factor influencing various material properties, alongside the comonomer structure and content. However, analytical methodologies for the characterisation and representation of comonomer distribution in PHB copolyesters remain limited. In the present study, we examined the comonomer distribution in poly(3-hydroxybutyrate-<i>co</i>-3-hydroxyhexanoate) (PHBH) using matrix-assisted laser desorption/ionisation spiral time-of-flight mass spectrometry (MALDI-spiral-TOF-MS). High-molecular-weight PHBH samples were partially methanolysed and subsequently fractionated by size-exclusion chromatography to yield oligomers of suitable molecular sizes for analysis. The high-resolution capabilities of MALDI-spiral-TOF-MS enabled the separation of ion peaks with similar <i>m</i>/<i>z</i> values in the PHBH oligomers and the determination of their accurate masses. The resulting mass spectral data were subsequently subjected to Kendrick mass defect (KMD) analysis to classify ion peaks according to their end-group structures, thereby facilitating the identification of distinct molecular species. Accurate mass measurements enabled the unambiguous determination of the corresponding molecular formulae, end groups, and monomer compositions of the PHBH oligomers. By organising the ion peak data corresponding to PHBH chains of a specific length (<i>e.g.</i>, 21-mer), the distribution of 3-hydroxyhexanoate (3HH) units within the molecular chain was represented as a number distribution plot for that chain length. This analytical approach was also succesfully applied to PHBH film residues subjected to biodegradation in seawater.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144726089","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}
Chaozhan Chen, Ruhuan Ye, Zidong Chen, Jiayi Ye, Bin Ran, Bo Liu, Jialin Liang, Jiale Huang, Teng Shen
{"title":"A microfluidic paper-based analytical device based on a surface-modified screen-printed electrode Pt-Pd/RGO nanocomposite for glucose detection in urine.","authors":"Chaozhan Chen, Ruhuan Ye, Zidong Chen, Jiayi Ye, Bin Ran, Bo Liu, Jialin Liang, Jiale Huang, Teng Shen","doi":"10.1039/d5ay00852b","DOIUrl":"https://doi.org/10.1039/d5ay00852b","url":null,"abstract":"<p><p>Urine biomarker detection with high accuracy and sensitivity is crucial for advancing point-of-care diagnostics. This paper developed a microfluidic paper-based analytical device (μPAD) for electrochemical glucose detection in urine. The proposed μPAD employs a filter paper substrate to enable pump-free sample transport to a detection zone integrated with the screen-printed electrode (SPE), allowing rapid quantification within 60 seconds. A composite of reduced graphene oxide (RGO)/platinum-palladium nanoparticles (Pt-Pd NPs) with good analytical performance has been electrodeposited on the surface of SPEs and subsequently combined with glucose oxidase (GO<sub><i>x</i></sub>) to create a glucose biosensor (GO<sub><i>x</i></sub>/Pt-Pd NPs/RGO/SPE). Under optimized conditions, the Pt-Pd NPs/RGO/SPE shows good performance, showing a 17.4-fold sensitivity enhancement over bare SPEs in H<sub>2</sub>O<sub>2</sub> detection. The developed μPAD achieves wide linear ranges of 5 μM-20 mM (H<sub>2</sub>O<sub>2</sub>) and 20 μM-5 mM (glucose), with low detection limits of 0.97 μM and 8.1 μM, respectively. Furthermore, the μPAD shows wide linear ranges covering required detection ranges of glucose in urine, demonstrating its great potential in personal health monitoring and clinical applications requiring reliable glucose measurement in urine.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144705811","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":"Application of an FR4 printed circuit board for the fabrication of a simple and low cost patterned Cu disk for the determination of paraquat.","authors":"Narjes Negahdari, Behzad Haghighi","doi":"10.1039/d5ay00824g","DOIUrl":"https://doi.org/10.1039/d5ay00824g","url":null,"abstract":"<p><p>An FR4 printed circuit board was used to fabricate a patterned Cu disk electrode (p-Cu). It was modified with a Nafion layer (p-Cu/Nafion) and used as a disposable (single-use) sensor for the determination of paraquat. Cyclic voltammetry and linear sweep voltammetry (LSV) were used to obtain the optimal route for paraquat determination using p-Cu/Nafion. The effects of the concentration of Nafion, the type, concentration and pH of supporting electrolyte, and the applied accumulation time and potential on LSV responses of PQ were investigated. Two linear relationships were observed between square wave voltammetry (SWV) responses and the concentration of PQ in the range of 0.5-15 and 25-100 μM, under optimal experimental conditions. The obtained limit of detection (S/N = 3) and limit of quantification (S/N = 10) were 0.29 and 1.0 μM, respectively. The effects of the presence of possible interfering compounds on the SWV responses of PQ were examined and the sensor was applied for the determination of PQ in tomato juice with satisfactory results.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144705812","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 size exclusion chromatography cartridge-based analytical method for determination of free drug in nano-liposomal oncology drug formulations.","authors":"Wei Zhang, Mark Paciolla, Lijun Duan, Elise Bradley, Aastha Chadha, Bhavesh Barot, Kaylee Worrell","doi":"10.1039/d4ay02124j","DOIUrl":"https://doi.org/10.1039/d4ay02124j","url":null,"abstract":"<p><p>A reliable and stability-indicating size exclusion chromatography (SEC) cartridge-based free drug testing method was developed for active loading nanoliposome formulations through a systematic development approach. The SEC spin cartridge columns (7K MWCO, 2 mL) were used for developing the liposome free drug testing procedure. The SEC cartridge column retention capacity for a Mirati drug was determined (445 μg per cartridge). SEC testing conditions were studied to achieve a good separation between liposomes and the free drug, including cartridge conditioning, buffer wash steps for liposomal drug elution, organic media wash steps for free drug elution, and sample size effect. Qualification of this newly developed SEC cartridge method has demonstrated its specificity/selectivity without interference and excellent detection linearity (correlation coefficient (<i>R</i>) > 0.999) over a study concentration range (1.0 to 46.9 μg mL<sup>-1</sup>), sufficient LOQ (0.52 μg mL<sup>-1</sup> equivalent to 1.7% of free drug in a liposome formulation at 2.5 mg mL<sup>-1</sup>), acceptable accuracy/recovery of 81 to 89% for free drug in spiked samples at 4.5%, 9%, and 18% levels (sample loading by a regular pipet) and 88 to 97% at 10% spike level (sample loading by a positive displacement pipet), good method precision (RSD (<i>n</i> = 6) of 4% NMT) for free drug determination, and 3 days solution stability for both standard and sample solutions (2-8 °C). In comparative sample testing, the SEC free drug test results were in good agreement with the solid phase extraction (SPE) test results for active loading formulations. The new method's stability-indicating ability has been proved through monitoring free drug in a liposome sample stored at -20 °C and -80 °C.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144705813","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 Golgi-targeting fluorescent probe for the detection of hydrazine in biological and environmental systems.","authors":"Hui-Juan Lai, Xu Wang, Yuan Wang, Wei-Na Wu, Zhi-Hong Xu","doi":"10.1039/d5ay00690b","DOIUrl":"https://doi.org/10.1039/d5ay00690b","url":null,"abstract":"<p><p>Hydrazine (N<sub>2</sub>H<sub>4</sub>) is regarded as an extremely toxic agent but it is used in large quantities as a chemical raw material in various industries, which poses a severe danger to both the environment and public health. Notably, the Golgi apparatus (GA) of hepatocytes is frequently affected by toxins in cases of hepatotoxicity. Therefore, developing a probe to monitor N<sub>2</sub>H<sub>4</sub> in environmental systems and within the GA of live cells is highly valuable. A Golgi-targeting fluorescent probe, BHMBS, is synthesized to detect N<sub>2</sub>H<sub>4</sub>. The probe BHMBS emits faint green fluorescence at 550 nm, which is remarkably enhanced after adding N<sub>2</sub>H<sub>4</sub>. The probe can detect N<sub>2</sub>H<sub>4</sub> with an ultra-short reaction time, high sensitivity, and excellent selectivity, making it a valuable tool to monitor N<sub>2</sub>H<sub>4</sub> in the real world and image the N<sub>2</sub>H<sub>4</sub> fluctuations in cells and zebrafish.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144705810","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":"Nondestructive presymptomatic detection of blue-fluorescing substances in tomato leaves infected with <i>Ralstonia solanacearum</i> using a polyvinyl alcohol hydrogel.","authors":"Shigeyuki Iwasa, Yuso Kobara, Katsumi Maeda, Arina Asano, Tatsuya Shimanuki, Kuniaki Nagamine","doi":"10.1039/d5ay00579e","DOIUrl":"https://doi.org/10.1039/d5ay00579e","url":null,"abstract":"<p><p>This study proposes a nondestructive technique for the presymptomatic detection of pathogenic infections of plants, aiming to effectively prevent and control plant diseases in agriculture. The present and previous studies indicated that an increase in blue-fluorescing substances, including chlorogenic acid, in tomato leaves is a promising biomarker of infection with the pathogenic soil bacterium <i>Ralstonia solanacearum.</i> A soft and adhesive polyvinyl alcohol (PVA) hydrogel conformably adhered to the hydrophobic surface of the tomato leaf with a complex topography, mediated by non-volatile glycerol, enabling effective extraction of blue-fluorescing substances in a nondestructive manner. The fluorescence intensity of the PVA hydrogel increased a few days before the appearance of visible symptoms of bacterial wilt. This technique is expected to become a fundamental technology for the early detection of plant diseases.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144705814","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}