Analytical Methods最新文献

{"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_<i>x</i>) to create a glucose biosensor (GO_<i>x</i>/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 H₂O₂ detection. The developed μPAD achieves wide linear ranges of 5 μM-20 mM (H₂O₂) 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^-1), sufficient LOQ (0.52 μg mL^-1 equivalent to 1.7% of free drug in a liposome formulation at 2.5 mg mL^-1), 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 (N₂H₄) 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 N₂H₄ in environmental systems and within the GA of live cells is highly valuable. A Golgi-targeting fluorescent probe, BHMBS, is synthesized to detect N₂H₄. The probe BHMBS emits faint green fluorescence at 550 nm, which is remarkably enhanced after adding N₂H₄. The probe can detect N₂H₄ with an ultra-short reaction time, high sensitivity, and excellent selectivity, making it a valuable tool to monitor N₂H₄ in the real world and image the N₂H₄ 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}

{"title":"Analysis of thermal degradation of bis(2-phenylpyridine) (acetylacetonate)iridium(III) (Ir(ppy)₂(acac)) using spectroelectrochemistry.","authors":"Tae-Ho Yang, Hye-Ri Joe, Jin-Seon Heo, Sungmin Kwon, Jonghee Lee, Jae-Hyun Lee","doi":"10.1039/d5ay00828j","DOIUrl":"https://doi.org/10.1039/d5ay00828j","url":null,"abstract":"<p><p>Enhancing the lifespan of organic light-emitting diodes (OLEDs) is crucial for developing stable, high-performance devices. The operational lifetime and performance of OLEDs are reportedly primarily enhanced by the thermal and chemical stability of their constituent single molecules. Therefore, understanding the thermal and electrical stability of these organic molecules is essential for long-lifetime OLED fabrication. However, the degradation of these materials during thermal evaporation has not yet been evaluated. In this study, we investigated the thermal degradation of bis(2-phenylpyridine) (acetylacetonate)iridium(III) (Ir(ppy)₂(acac)), a widely used green phosphorescent dopant, using spectroelectrochemistry (SEC) and matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) spectroscopy techniques. SEC measurements revealed the ability of the Ir(ppy)₂(acac) molecules to exhibit different polaron states before and after thermal aging. Gaussian fitting showed the presence of additional polaron absorption peaks in the SEC spectra, which indicated that degradation occurred gradually over the first 4 h of aging and then saturated. MALDI-TOF analysis confirms these results, showing an additional peak at 622.9 <i>m</i>/<i>z</i>, corresponding to thermally aged Ir(ppy)₂(acac), alongside the intrinsic molecule peak at 599.8 <i>m</i>/<i>z</i>. This result suggested that the Ir(ppy)₂(acac) ligand underwent thermal aging-induced degradation in the deposition chamber. Through this study, we anticipate contributing to related research and industrial advancement by enabling the rapid evaluation of the thermal degradation of OLED materials.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144697131","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":"Rapid, multiplex, one-pot CRISPR/Dx system for detecting cancer fusion genes.","authors":"Jiaqi Li, Cia-Hin Lau, Jianchao Wang, Weidong Wu, Zhihao Huang, Xiaoqing Chen, Jiahui Li, Yumei Huang, Tao Wang, Yulin Li, Zihan Zhao, Meijing Xu, Gang Chen, Sheng Tong, Haibao Zhu","doi":"10.1039/d5ay00783f","DOIUrl":"https://doi.org/10.1039/d5ay00783f","url":null,"abstract":"<p><p>Targeted therapies directed at fusion genes have proven remarkably effective against cancers. Therefore, the rapid and reliable identification of cancer fusion genes can guide subsequent therapeutic treatment and predict prognosis. By integrating the RT-RPA and CRISPR/Cas12a approaches, we developed a one-pot CRISPR/Dx system for the rapid and multiplex detection of cancer fusion genes. A tube with unique assemblies was created using 3D printing technology to realize this application. As proof of principle, we demonstrated the feasibility of the one-pot CRISPR/Dx system in detecting lung cancer by targeting <i>ROS1</i> fusions. The performance of the one-pot CRISPR/Dx detection system was comparable to a two-tube-based testing platform. When tested with synthetic RNA fusions, both approaches efficiently detected all 14 <i>ROS1</i> fusions with an LOD in the range of 5-10 copies per μL, without generating a background signal, even in the presence of a large excess of wild-type RNA. The total reaction time for both approaches was 30 minutes. Notably, the one-pot CRISPR/Dx detection system minimized the operation steps and aerosol contamination without compromising detection sensitivity and specificity. Furthermore, its diagnostic power was validated using clinical samples. Thus, we successfully developed a rapid, multiplex, one-pot CRISPR/Dx detection system for detecting 14 clinically relevant <i>ROS1</i> fusions with high sensitivity and specificity. It is also cost-effective and simple to operate, thereby realizing the ultimate goal of establishing CRISPR/Dx as the paragon of cancer diagnostics for home self-testing and point-of-care testing.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144697132","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":"Dynamic extraction of microplastics from simulated and natural freshwaters using a rotating coiled column.","authors":"Mikhail S Ermolin, Elena Yu Savonina, Alexandr I Ivaneev, Tatiana A Maryutina, Petr S Fedotov","doi":"10.1039/d5ay00943j","DOIUrl":"https://doi.org/10.1039/d5ay00943j","url":null,"abstract":"<p><p>At present, microplastic pollution in aquatic environments is raising increasing concerns on its risks for the human health. The efficiency of existing water treatment technologies, which are based on different physical principles, is still insufficient for the removal of microplastics from aqueous media, and hence, novel methods are needed. Thus far, liquid-liquid extraction has not been used in water treatment processes; however, it has great potential for removing microplastics from water. This study was aimed at the development of a novel method based on dynamic liquid-liquid extraction in a rotating coiled column for the removal of microplastics from aqueous samples. It was demonstrated that liquid-liquid extraction in a rotating coiled column (inner capacity 25 of mL) using castor oil as the stationary phase offered more than 96% recovery rate of the five most abundant microplastics (μPE, μPP, μPS, μPVC, and μPET) of different sizes (<63, 63-100, and 100-250 μm) from simulated freshwater (sample volume of 20 mL). An average recovery rate of 100% was observed for the mixture of these five microplastics from a spiked natural river water sample. Notably, the recovery rate was not dependent on the size and type of microplastics under study. It was also found that in a column with a tubing bore of 1.6 mm, the flow rate of the aqueous suspension of microplastics (mobile phase) could be increased up to 5 mL min^-1 without decreasing the extraction efficiency. The scale-up of the extraction process was also possible.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144688352","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":"Green, innovative oral capsules of three anti-Parkinson's drugs: formulation, <i>in vitro</i> evaluation, and robust RP-HPLC validation.","authors":"Samar M Mahgoub, Abdullah S Alawam, Hassan A Rudayni, Ahmed A Allam, Khaled Hesham Ezzat, Saber A A Elsuccary, Abdelatty M Radalla, Rehab Mahmoud","doi":"10.1039/d5ay00698h","DOIUrl":"https://doi.org/10.1039/d5ay00698h","url":null,"abstract":"<p><p>Parkinson's disease (PD) remains a debilitating neurodegenerative disorder, with levodopa (LEV) as the cornerstone of its management. However, the long-term use of LEV is often complicated by motor fluctuations and dyskinesias, necessitating adjunct therapies such as carbidopa (CAR) and safinamide (SAF) to enhance efficacy and reduce side effects. Despite the promising therapeutic potential of this combination, the simultaneous analysis of the three drugs in pharmaceutical formulations poses significant analytical challenges. This study addresses this critical gap by developing and validating a sensitive and specific reversed-phase high-performance liquid chromatography (RP-HPLC) method for their simultaneous quantification in pure forms and in-house oral capsule formulations. The optimized method utilized a gradient elution using phosphate buffer (pH 3, 0.1 M) and acetonitrile as the mobile phase, a C8 stationary phase, and UV detection at 240 nm, achieving baseline separation within 11 min. Validation studies demonstrated excellent linearity, precision (RSD < 2%), accuracy (recovery 98.97-100%), and robustness, with LODs of 0.063 μg mL^-1, 0.112 μg mL^-1, and 0.058 μg mL^-1, and LOQs of 0.190 μg mL^-1, 0.341 μg mL^-1, and 0.177 μg mL^-1 for LEV, CAR, and SAF, respectively. The in-house capsule formulation exhibited uniform drug content (90-110% of label claim), rapid disintegration (<8 min), and complete dissolution of LEV and CAR within 45 min, while SAF showed sustained release over 60 min. The method is offering a reliable and sustainable approach for quality control, pharmaceutical analysis, and industrial applications. The greenness profile of the method was rigorously evaluated using the NEMI, AGP, ESA, AGREE, and MoGAPI methods. Furthermore, the blueness of the technique was studied using the BAGI method, confirming its alignment with green analytical chemistry principles.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144688353","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 electronic tongue and hyperspectral imaging with a CNN-transformer fusion model for rapid detection of botanical origins of honey.","authors":"Wanqing Zeng, Zhiqiang Wang, Zihan Wang, Yanrong Wang, Hanbing Yin, Suchao Xu","doi":"10.1039/d4ay02222j","DOIUrl":"https://doi.org/10.1039/d4ay02222j","url":null,"abstract":"<p><p>The botanical origin of honey significantly impacts its nutritional composition, quality, and price. Traditional identification methods are often complex, require expensive equipment, and are time-consuming. This article proposes a rapid detection method for the botanical origin of honey based on an electronic tongue (ET) and hyperspectral imaging (HSI) combined with a CNN-transformer fusion model. First, gustatory and spectral data of honey samples from different botanical origins are collected by ET and HSI systems, respectively. A CNN-transformer fusion model is proposed to perform feature extraction, information interaction, and pattern recognition on the collected ET and HSI data. This model employs a dual-path CNN-transformer to capture local and global features of ET and HSI signals at different scales. A multi-scale interaction module is designed to enhance cross-modal communication and facilitate information sharing between the ET and HSI information. Finally, the contrastive information bottleneck (CIB) module is adopted to optimize mutual information through contrastive learning and enable the integration of ET and HSI features for classification and recognition. The experimental results demonstrate that this method achieves superior recognition accuracy in classifying and identifying honey botanical origin compared to that using either the ET or HSI alone. Its experimental mean test set accuracy, precision, recall, and F1 score reached 99.08%, 99.09%, 99.05%, and 0.9906, respectively. This study provides a new detection method for the botanical source of different kinds of honey, which has a promising application in honey and other food industries.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144688351","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}