Analytical Methods最新文献

{"title":"C-ZIF-8 modified NiO photocathode and enhanced photosensitizer signal amplification for ultra-sensitive photoelectrochemical detection of lead ions†","authors":"Zhaona Zhang, Juan Wang, Siru Guo and Xinxing Wang","doi":"10.1039/D5AY00136F","DOIUrl":"10.1039/D5AY00136F","url":null,"abstract":"<p >NiO photocathodes have been developed for photoelectrochemical (PEC) sensing. However, the development of NiO-based photoactive materials with higher performance is still being pursued to further improve the sensitivity of detection. In this article, we prepared a C-ZIF-8/NiO composite material photocathode composed of porous carbon derived from ZIF-8 (C-ZIF-8) and NiO, and utilized its enhanced PEC activity and amplification effect on chlorohemin (hemin) sensitization to achieve ultra-sensitive detection of lead ions (Pb<small>²⁺</small>). The introduction of C-ZIF-8 improved the charge transfer and light absorption ability of the composite material, and significantly increased the load of hemin on the photocathode, thereby enhancing the photocurrent response by 8 times. Based on the C-ZIF-8/NiO photocathode and <em>in situ</em> generated photosensitizer signal amplification strategy, ultra-sensitive detection of Pb<small>²⁺</small> had been attained with a detection linear range of 10 pM to 5 nM and a detection limit of 2.6 pM. This study provides a new platform for high sensitivity detection of Pb<small>²⁺</small>, and extensive potential applications could be further expected.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2650-2656"},"PeriodicalIF":2.7,"publicationDate":"2025-03-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143622897","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 UPLC-MS/MS assay for determination of PA-PEG8-PA polymers in rat plasma coupled with [M − H]− to enhance sensitivity†","authors":"Jiye Tian, Chunpeng Feng, Hongyu Xue, Jiansong You, Meiyun Shi and Lei Yin","doi":"10.1039/D4AY02050B","DOIUrl":"10.1039/D4AY02050B","url":null,"abstract":"<p >Propionic acid-polyethylene glycol-propionic acid (PA-PEG-PA) is a commonly used biocompatible polymer in drug delivery systems. Unraveling the <em>in vivo</em> pharmacokinetic behavior of PA-PEG-PA polymer is important for the safety evaluation of PA-PEG-PA related drug delivery systems. In this research, a highly sensitive ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) assay was developed for detection of PA-PEG<small>₈</small>-PA polymers in complex biological matrices. Methoxy-polyethylene glycol propionic acid polymers with 6 subunits (mPEG<small>₆</small>-PA) were used as the internal standard (IS). The multiple reaction monitoring (MRM) transitions at <em>m</em>/<em>z</em> 513.4 ([M − H]<small>⁻</small> precursor ions) → 441.2 (fragment ions) and <em>m</em>/<em>z</em> 367.3 ([M − H]<small>⁻</small> precursor ions) → 118.8 (fragment ions) were chosen to determine PA-PEG<small>₈</small>-PA and mPEG<small>₆</small>-PA, respectively. The analysis time was only 5 min for each sample. Numerous parameters like specificity, sensitivity, accuracy, precision, recoveries, matrix effects and dilution effect were validated for the developed assay. The UPLC-MS/MS assay showed excellent linearity over the range of 30–1500 ng mL<small>⁻¹</small>(<em>r</em> &gt; 0.995). The assay was successfully applied to quantify the concentration of PA-PEG<small>₈</small>-PA polymers in rat plasma.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2676-2685"},"PeriodicalIF":2.7,"publicationDate":"2025-03-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143655605","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":"Nanosilver-mediated enzyme-free electrochemical immunosensor with enhanced stability for aflatoxin B1 detection in food safety†","authors":"Yu Wang and Xiaoming Ma","doi":"10.1039/D5AY00248F","DOIUrl":"10.1039/D5AY00248F","url":null,"abstract":"<p >The development and research of electrochemical immunoassays have attracted considerable attention. However, traditional electrochemical immunoassays inevitably require the participation of biological enzymes, which suffer from high cost, poor stability, inconvenient storage and easy inactivation. Herein, we constructed a bio-enzyme-free electrochemical immunoassay system specifically for the detection of aflatoxin B1 (AFB<small>₁</small>). This method was based on the traditional antigen–antibody immune recognition system utilizing the nanosilver particles (NSPs) as signal markers to replace conventional natural enzymes. Subsequently, the labeled NSPs were transferred to silver ions in the presence of nitric acid. The concentration of silver ions was determined using anodic stripping voltammetry (ASV), which correlates closely to the concentration of the target. The current intensity measured by the bio-enzyme-free electrochemical sensor exhibited a negative correlation with the concentration of AFB<small>₁</small>. Under optimized conditions, the electrochemical sensor was used to detect AFB<small>₁</small> in the dynamic concentration range of 0.01–100 ng mL<small>⁻¹</small>, and the limit of detection was 0.4882 pg mL<small>⁻¹</small>. The spiked recovery range of AFB<small>₁</small> in corn starch was determined to be between 100.98% and 109.42%, while the relative standard deviation (RSD) range was found to be from 0.34% to 3.82%. These results indicate that the electrochemical immunosensor without biological enzyme labeling has reliable accuracy, and the sensor has a broad application prospect in AFB<small>₁</small> detection.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2799-2805"},"PeriodicalIF":2.7,"publicationDate":"2025-03-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143655643","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 fluorescence “off-on” sensor for the selective detection of mercury based on perylene dye and gold nanoparticles†","authors":"Lijiao Liang, Qiang Wang, Yanxiang Wu, Tongde Rao, Xuanping Tan, Kezhong Liang and Yuwen Zhao","doi":"10.1039/D5AY00036J","DOIUrl":"10.1039/D5AY00036J","url":null,"abstract":"<p >A novel fluorescence “off-on” strategy based on a perylene probe (PDI) and arginine functionalized gold nanoparticles (arg-AuNPs) for the sensing of mercury ions (Hg<small>²⁺</small>) has been developed. Due to the strong electrostatic and hydrophobic interactions as well as the strong π–π stacking effect, the PDI probe can be adsorbed onto the surface of the nanoparticles, inducing the aggregation of arg-AuNPs. Consequently, the fluorescence peaks of PDI at 550 and 591 nm were quenched by arg-AuNPs through an energy transfer (ET) process, which could be enhanced upon the addition of Hg<small>²⁺</small>. The presence of Hg<small>²⁺</small> could prevent the ET process, thus recovering the fluorescence of PDI. An “off-on” fluorescence signal was therefore detected. Our assay method shows very high sensitivity with a limit of detection of 0.6 nM, and remarkable selectivity against common interfering metal ions. This sensing method has also been successfully used for real sample analysis. The “off-on” fluorescence sensing method is fairly simple, fast, and inexpensive, and the fluorescence quenching mechanism of PDI induced by arg-AuNPs is expected to be utilized for more target sensing applications.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2783-2790"},"PeriodicalIF":2.7,"publicationDate":"2025-03-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143646562","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 magnetic dispersive solid phase extraction of Cd(ii) ions from dairy products using an Fe3O4@ZIF-8@IIP nanocomposite sorbent","authors":"Zohreh Saeedi, Saeed Mohammad Sorouraddin, Mir Ali Farajzadeh and Mohammad Reza Afshar Mogaddam","doi":"10.1039/D4AY02284J","DOIUrl":"10.1039/D4AY02284J","url":null,"abstract":"<p >Based on dispersive micro solid phase extraction, a magnetic ion imprinted polymer–metal organic framework (Fe<small>₃</small>O<small>₄</small>@ZIF-8@IIP) nanocomposite was prepared in this work as a selective and effective sorbent to extract and preconcentrate cadmium(<small>II</small>) ions in dairy samples. An effective extraction process was made possible by the magnetic properties of iron oxide nanoparticles, metal–organic framework's large specific surface area, and ion imprinted polymer's selectivity toward Cd(<small>II</small>) ions. Fourier transform infrared spectrometry and scanning electron microscopy were used to characterize the produced sorbent. Effective optimization factors were examined and optimized, including the volume and type of desorption solvent, the type and duration of stirring, the pH of solution, and the quantity of the sorbent. The limits of detection and quantification under optimal extraction conditions were 0.09 and 0.30 μg L<small>⁻¹</small>, respectively. The linear range, which was 0.30–100 μg L<small>⁻¹</small>, had a coefficient of determination of 0.9927. A satisfactory match was observed in the data collected after testing a certified reference material (NIST SRM 1549 powder milk) to verify the established procedure. When Cd(<small>II</small>) ions were determined at 10 μg L<small>⁻¹</small> (<em>n</em> = 5), the approach produced relative standard deviation values of ≤3.1%. The developed technique was effectively used to determine Cd(<small>II</small>) ions concentration in several dairy products.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 16","pages":" 3331-3343"},"PeriodicalIF":2.7,"publicationDate":"2025-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143810241","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 ultra-fast UPLC-MS/MS approach for the quantification of baricitinib in the HLM matrix: greenness assessment with application to in vitro and in silico metabolic stability studies","authors":"Mohamed W. Attwa, Ali S. Abdelhameed and Adnan A. Kadi","doi":"10.1039/D5AY00294J","DOIUrl":"10.1039/D5AY00294J","url":null,"abstract":"<p >Baricitinib (Olumiant) is a Janus kinase inhibitor utilized for the management of COVID-19, rheumatoid arthritis, and alopecia areata. It received U.S. Food and Drug Administration approval on May 31, 2018. This work developed a sensitive, rapid, environmentally friendly, and reliable UPLC-MS/MS method for quantifying baricitinib in human liver microsomes, utilized to evaluate the <em>in vitro</em> metabolic stability of baricitinib in HLMs. The StarDrop software, with DEREK and P450 metabolic programs, was employed to detect the structural warnings related to BCB and assess the <em>in silico</em> metabolic lability. The validation of the UPLC-MS/MS approach conformed to U.S. Food and Drug Administration standards for bioanalytical approach validation. The present UPLC-MS/MS method exhibited a wide range of linearity (1.0–3000 ng mL<small>⁻¹</small>) and optimum separation of analytes in an ultra-fast separation time (1 min) and was reproducible and accurate in the absence of human liver microsome matrix effects. Baricitinib and encorafenib (the internal standard) were examined employing an isocratic mobile phase technique on a reversed phase (SB C18) column. This study assessed the accuracy and precision of UPLC-MS/MS methodologies for intra- and inter-day evaluations, which ranged from −1.20% to 8.67% and 0.12% to 11.67%, respectively. The intrinsic clearance of baricitinib was quantified at 27.49 mL min<small>⁻¹</small> kg<small>⁻¹</small>, while the <em>in vitro</em> half-life was established at 29.50 minutes. <em>In silico</em> analysis proposes that slight structural alterations to the pyrrole ring (88%) and the pyrimidine ring (5%) in drug design may increase safety and metabolic stability related to baricitinib. The evaluation of <em>in silico</em> absorption, distribution, metabolism, excretion, and metabolic stability characteristics for baricitinib is crucial for advancing innovative drug discovery focused on enhancing metabolic stability.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2718-2732"},"PeriodicalIF":2.7,"publicationDate":"2025-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143646568","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":"Advancing analytical chemistry with carbon quantum dots: a comprehensive review","authors":"Ilyos Eliboev, Alisher Ishankulov, Elyor Berdimurodov, Komiljan Chulpanov, Maksud Nazarov, Berdiyev Jamshid, Bekzod Toshpulotov, Rano Tukhtaeva, Muslum Demir, Kamila Rashidova, Fazliddin Jalilov and Khudaybergan Polvonov","doi":"10.1039/D4AY02237H","DOIUrl":"10.1039/D4AY02237H","url":null,"abstract":"<p >Carbon Quantum Dots (CQDs) have gained significant attention as versatile nanomaterials in analytical chemistry due to their strong fluorescence, high sensitivity, and biocompatibility features. This review explores the synthesis, functionalization, and broad applications of CQDs in various analytical domains, including bioimaging, diagnostics, and environmental monitoring. CQDs' unique properties, such as tunable emission and ease of surface modification, enhance their performance in fluorescence and electrochemical sensing. CQDs present emerging applications in single-cell analysis, point-of-care diagnostics, and food safety. Technological advancements in green synthesis and hybrid nanomaterial integration are paving the way for more sustainable, efficient, and scalable analytical tools. However, challenges related to reproducibility, stability, and large-scale production persist, highlighting the need for continued research. The present review provides a comprehensive overview of CQDs' impact, emphasizing their potential to transform analytical chemistry through innovative applications and future breakthroughs.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2627-2649"},"PeriodicalIF":2.7,"publicationDate":"2025-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143655560","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 dCas9/sgRNA complex-mediated competitive assay for accurate and sensitive Pseudomonas aeruginosa analysis†","authors":"Buyi Wang, Ziyao Yu, Zhihao Zhang, Zilu Zhu and Yanhai Song","doi":"10.1039/D4AY02194K","DOIUrl":"10.1039/D4AY02194K","url":null,"abstract":"<p > <em>Pseudomonas aeruginosa</em> (<em>P. aeruginosa</em>), a Gram-negative pathogenic bacterium, is one of the most common bacteria that causes severe infectious diseases. However, accurate and efficient detection of <em>P. aeruginosa</em> in clinical samples is a huge challenge. Therefore, in this study, we developed a Cas9 derivative (dCas9)/sgRNA-mediated competitive assay for the sensitive and precise characterization of genomic materials from <em>P. aeruginosa</em>. Our approach involved the identification of target genomic sequences using the dCas9/sgRNA complex, which occupied the “sensing probe” (SP) binding site, resulting in an increased availability of free SP. SP subsequently facilitated DNA polymerase/endonuclease-mediated signal cycles and signal production, enabling highly sensitive detection of <em>P. aeruginosa</em>. The proposed competitive assay demonstrated a robust linear response to <em>P. aeruginosa</em> within a concentration range from 10 CFU mL<small>⁻¹</small> to 10<small>⁶</small> CFU mL<small>⁻¹</small>, leveraging numerous signal amplification processes and competitive target recognition while exhibiting robust anti-interference capacity. Compared with former strategies, the proposed competitive assay enabled the accurate detection of <em>P. aeruginosa</em> by directly identifying and binding genomic sequences, which could be easily extended to the detection of other bacteria by simply changing the sgRNA. In addition, the proposed approach exhibits significant clinical potential for early disease diagnosis owing to its excellent sensitivity and accuracy.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2791-2798"},"PeriodicalIF":2.7,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143655545","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 oxidase-like nanozyme-based sensor array for the specific detection and discrimination of catechins†","authors":"Lijun Yang, Zhiyi Zhang, Tiantian Zhou, Wei Qi and Mengfan Wang","doi":"10.1039/D4AY02133A","DOIUrl":"10.1039/D4AY02133A","url":null,"abstract":"<p >In this study, a nanozyme-based sensor array was developed to achieve the identification and discrimination of three catechins (catechin, epicatechin, and epigallocatechin). The Fc@ZIF-67 NC nanozyme was synthesized with oxidase-like activity through the high-temperature carbonization of ferrocene-encapsulated ZIF-67. Two Fc@ZIF-67 NC-involved oxidase-like reactions were designed to generate three detectable signals (including two colorimetric signals and one fluorescent signal), which constituted the fingerprints of the analytes. By combining with linear discriminant analysis (LDA), different kinds and concentrations of catechins can be discriminated with this sensor array. Besides, the sensor array was proved feasible in the identification of catechins in real samples. This method provides a promising methodology for the discrimination and identification of natural products in food.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2763-2770"},"PeriodicalIF":2.7,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143646566","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 stable and sensitive strip biosensors for the rapid detection of organophosphates and aflatoxin B1 in agricultural samples†","authors":"Xiaoshan Luo, Liudi Liu, Xuanbo Wang, Disi Lu, Yuexi Liang, Osmani Chacón Chacón, Gang Li, Xiaoqin Wang and Zhaozhu Zheng","doi":"10.1039/D4AY02229G","DOIUrl":"10.1039/D4AY02229G","url":null,"abstract":"<p >In this study, we present a facile and efficient method for fabricating silk fibroin hydrogel films encapsulating the acetylcholinesterase enzyme (AChE) and pH test strips (biosensor strips) for detecting organophosphorus pesticides (OPs) and aflatoxin B1 (AFB1). These biosensor strips possess several unique properties: flexibility, time efficiency, and high stability. Upon exposure to OPs or AFB1, AChE activity is inhibited, leading to a discernible color change on the pH test strip, enabling rapid and sensitive visual detection of these contaminants. The strips were effectively utilized as a practical and sensitive platform for the visual detection of OPs and AFB1. The limits of detection for paraoxon, aldicarb, and AFB1 were determined to be 6.57, 8.92, and 0.274 ng mL<small>⁻¹</small>, respectively. Furthermore, the applicability of these biosensors for detecting OPs or AFB1 in real samples of Chinese cabbage and peanuts was successfully demonstrated. Additionally, the performance of these novel strip composites was validated through comparison with commercial pesticide rapid test papers. Notably, the encapsulated AChE enzymes retained significant sensitivity for over 18 months, even when stored at 37 °C, and the biosensor strips exhibited remarkable resistance to sensitivity loss caused by inhibitors. This work presents a highly sensitive and stable enzyme-based visual detection paper for agricultural and food safety applications. In addition to its outstanding resistance to interference, the developed biosensor ensures reliable reproducibility and maintains stability over long-term use. This new approach to OP analysis in ecological samples has also been effectively used in the determination of OPs in lake water.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2665-2675"},"PeriodicalIF":2.7,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143646593","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}