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Synthesis of Multi-Metal Oxoanion-Modified silver on renewable Potato-Starch based carbon microspheres via a ‘Ternary synergistic Strategy’ for sensitive adrenaline detection
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-03-01 DOI: 10.1016/j.microc.2025.113196
Zhuoxian Tang , Lin Hao , Tingyu Zhang , Hongyuan Yan , Yufan Zhang
This study introduces an innovative strategy for synthesizing low-cost, renewable carbon microspheres derived from potato starch. Uniformly dispersed potato-starch-based carbon microspheres (PCMs) were fabricated via a catalyst-free hydrothermal method, followed by calcination. Polyoxometalates (POMs) acted as both reducing and bridging agents, enabling the uniform deposition of silver nanoparticles (Ag NPs) on the PCM surface. The Ag NPs exhibited remarkable catalytic activity and a high specific surface area, effectively lowering the oxidation potential of adrenaline molecules and accelerating electron transfer, thereby enhancing detection sensitivity. As a biocarbon material, PCMs possess a high specific surface area and a porous structure, facilitating the adsorption and distribution of adrenaline molecules and thereby improving sensor performance. The synthesized ternary nanocomposite, Ag@POM/PCMs, exhibited synergistic catalytic behavior arising from the combined effects of catalytically active Ag NPs, electron-transfer-promoting POMs, and porous PCMs with a large surface area. This unique synergy significantly enhanced electrocatalytic performance, as demonstrated by high sensitivity, a broad linear detection range (0.46–1626.64 μM), and a low detection limit (0.238 μM, S/N = 3). Moreover, the material exhibited excellent stability, reproducibility, and anti-interference properties, achieving recovery rates of 99.2 % to 101.9 % in human serum samples.
{"title":"Synthesis of Multi-Metal Oxoanion-Modified silver on renewable Potato-Starch based carbon microspheres via a ‘Ternary synergistic Strategy’ for sensitive adrenaline detection","authors":"Zhuoxian Tang ,&nbsp;Lin Hao ,&nbsp;Tingyu Zhang ,&nbsp;Hongyuan Yan ,&nbsp;Yufan Zhang","doi":"10.1016/j.microc.2025.113196","DOIUrl":"10.1016/j.microc.2025.113196","url":null,"abstract":"<div><div>This study introduces an innovative strategy for synthesizing low-cost, renewable carbon microspheres derived from potato starch. Uniformly dispersed potato-starch-based carbon microspheres (PCMs) were fabricated via a catalyst-free hydrothermal method, followed by calcination. Polyoxometalates (POMs) acted as both reducing and bridging agents, enabling the uniform deposition of silver nanoparticles (Ag NPs) on the PCM surface. The Ag NPs exhibited remarkable catalytic activity and a high specific surface area, effectively lowering the oxidation potential of adrenaline molecules and accelerating electron transfer, thereby enhancing detection sensitivity. As a biocarbon material, PCMs possess a high specific surface area and a porous structure, facilitating the adsorption and distribution of adrenaline molecules and thereby improving sensor performance. The synthesized ternary nanocomposite, Ag@POM/PCMs, exhibited synergistic catalytic behavior arising from the combined effects of catalytically active Ag NPs, electron-transfer-promoting POMs, and porous PCMs with a large surface area. This unique synergy significantly enhanced electrocatalytic performance, as demonstrated by high sensitivity, a broad linear detection range (0.46–1626.64 μM), and a low detection limit (0.238 μM, S/N = 3). Moreover, the material exhibited excellent stability, reproducibility, and anti-interference properties, achieving recovery rates of 99.2 % to 101.9 % in human serum samples.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113196"},"PeriodicalIF":4.9,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143534156","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Robust SPE-UHPLC-MS/MS method for determination of multiple categories of antibiotics with broad polarity range in surface water
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-03-01 DOI: 10.1016/j.microc.2025.113198
Xinyuan Pei , Nan Zhang , Yuting Chen , Shiyu Miao , Huiyang Fu , Qingqing Zhu , Zhengbo Dai , Yi Chi , Ligang Hu , Rong Jin , Chunyang Liao
Antibiotics, as a typical class of emerging contaminants in the environment, are frequently detected at trace concentrations in various water samples. The chemical properties of antibiotics exhibit significant diversity, encompassing variations in molecular structure, amphoteric behaviour, and polarity. These differences present substantial challenges in developing universal detection methods for comprehensive monitoring of antibiotic contaminants. Therefore, it is imperative to develop more targeted, efficient, and sensitive analytical techniques. In this study, we develop a solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry (SPE-UHPLC-MS/MS) method. This method enables the simultaneous determination of 69 antibiotics divided into seven categories (tetracyclines, quinolones, sulfonamides, β-lactams, macrolides, lincosamides, and chloramphenicols) in surface water. The method achieved limits of detection (LOQs) ranging from 0.002 to 1.71 ng/L. The standard curves of the target compounds exhibited excellent linearity, with correlation coefficients (r2) > 0.995, and most spiked recoveries fell within the range of 40.4–149 %, with relative standard deviations (RSDs) below 15 %. Using this method, 19 surface water samples from Qiantang River Basin, Zhejiang Province, China were analyzed, with 29 out of 69 analytes being detected (the total concentrations ranging from 5.69 to 131 ng/L). This method provides a reliable and robust analytical approach for the comprehensive monitoring of antibiotic contaminants in environmental water, offering critical insights for pollution control and water quality management efforts.
{"title":"Robust SPE-UHPLC-MS/MS method for determination of multiple categories of antibiotics with broad polarity range in surface water","authors":"Xinyuan Pei ,&nbsp;Nan Zhang ,&nbsp;Yuting Chen ,&nbsp;Shiyu Miao ,&nbsp;Huiyang Fu ,&nbsp;Qingqing Zhu ,&nbsp;Zhengbo Dai ,&nbsp;Yi Chi ,&nbsp;Ligang Hu ,&nbsp;Rong Jin ,&nbsp;Chunyang Liao","doi":"10.1016/j.microc.2025.113198","DOIUrl":"10.1016/j.microc.2025.113198","url":null,"abstract":"<div><div>Antibiotics, as a typical class of emerging contaminants in the environment, are frequently detected at trace concentrations in various water samples. The chemical properties of antibiotics exhibit significant diversity, encompassing variations in molecular structure, amphoteric behaviour, and polarity. These differences present substantial challenges in developing universal detection methods for comprehensive monitoring of antibiotic contaminants. Therefore, it is imperative to develop more targeted, efficient, and sensitive analytical techniques. In this study, we develop a solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry (SPE-UHPLC-MS/MS) method. This method enables the simultaneous determination of 69 antibiotics divided into seven categories (tetracyclines, quinolones, sulfonamides, β-lactams, macrolides, lincosamides, and chloramphenicols) in surface water. The method achieved limits of detection (LOQs) ranging from 0.002 to 1.71 ng/L. The standard curves of the target compounds exhibited excellent linearity, with correlation coefficients (r<sup>2</sup>) &gt; 0.995, and most spiked recoveries fell within the range of 40.4–149 %, with relative standard deviations (RSDs) below 15 %. Using this method, 19 surface water samples from Qiantang River Basin, Zhejiang Province, China were analyzed, with 29 out of 69 analytes being detected (the total concentrations ranging from 5.69 to 131 ng/L). This method provides a reliable and robust analytical approach for the comprehensive monitoring of antibiotic contaminants in environmental water, offering critical insights for pollution control and water quality management efforts.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113198"},"PeriodicalIF":4.9,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143547890","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
PVDF membrane immobilized acetylcholinesterase-based fluorescence biosensor for chlorpyrifos detection
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-03-01 DOI: 10.1016/j.microc.2025.113197
Jia Liu , Lin Li , Xin-Yue Chen , Juan Chen
Trace residues of chlorpyrifos (organophosphorus pesticides) pose significant environmental hazards due to their acute insecticidal toxicity. Chlorpyrifos inhibits acetylcholinesterase (AChE), which heightens the risks of neurological disorders. The implications of these interactions underscore the urgent need for detection strategies to mitigate the risks associated with chlorpyrifos exposure. Considering the inherently fragile nature of AChE, a novel composite membrane (PVDF/PDA/PEI) was introduced to immobilize AChE for its excellent simplicity, portability and ease of separation. And a ratiometric fluorescence biosensor based on photoluminescent carbon dots emitting at 468 nm and cobalt oxyhydroxide nanosheets emitting at 568 nm were constructed. The resulting fluorescence ratio at F468/F568 was served as a ratiometric fluorescence signal for AChE assay and chlorpyrifos detection, with a detection limit of 0.103 ng/mL. This study facilitates the precise monitoring of chlorpyrifos levels in real samples, providing a reliable method to detect even trace amounts of this widely used chlorpyrifos. By offering a balance between the activity and stability of fragile AChE, facilitating the utilization of PVDF/PDA/PEI immobilized AChE in the fabrication of a ratiometric fluorescence sensor for the purpose of chlorpyrifos detection. This advancement not only improves detection sensitivity but also contributes significantly to environmental safety and public health monitoring.
{"title":"PVDF membrane immobilized acetylcholinesterase-based fluorescence biosensor for chlorpyrifos detection","authors":"Jia Liu ,&nbsp;Lin Li ,&nbsp;Xin-Yue Chen ,&nbsp;Juan Chen","doi":"10.1016/j.microc.2025.113197","DOIUrl":"10.1016/j.microc.2025.113197","url":null,"abstract":"<div><div>Trace residues of chlorpyrifos (organophosphorus pesticides) pose significant environmental hazards due to their acute insecticidal toxicity. Chlorpyrifos inhibits acetylcholinesterase (AChE), which heightens the risks of neurological disorders. The implications of these interactions underscore the urgent need for detection strategies to mitigate the risks associated with chlorpyrifos exposure. Considering the inherently fragile nature of AChE, a novel composite membrane (PVDF/PDA/PEI) was introduced to immobilize AChE for its excellent simplicity, portability and ease of separation. And a ratiometric fluorescence biosensor based on photoluminescent carbon dots emitting at 468 nm and cobalt oxyhydroxide nanosheets emitting at 568 nm were constructed. The resulting fluorescence ratio at F<sub>468</sub>/F<sub>568</sub> was served as a ratiometric fluorescence signal for AChE assay and chlorpyrifos detection, with a detection limit of 0.103 ng/mL. This study facilitates the precise monitoring of chlorpyrifos levels in real samples, providing a reliable method to detect even trace amounts of this widely used chlorpyrifos. By offering a balance between the activity and stability of fragile AChE, facilitating the utilization of PVDF/PDA/PEI immobilized AChE in the fabrication of a ratiometric fluorescence sensor for the purpose of chlorpyrifos detection. This advancement not only improves detection sensitivity but also contributes significantly to environmental safety and public health monitoring.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113197"},"PeriodicalIF":4.9,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143547820","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Efficient detection and validation of 4-Methoxyphenol chemical based on binary oxides intercalated ZnO-CdO nanocomposite by electrochemical approach 基于二元氧化物插层 ZnO-CdO 纳米复合材料的电化学方法对 4-甲氧基苯酚化学物质的高效检测和验证
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-03-01 DOI: 10.1016/j.microc.2025.113171
Umer Shahzad , Hadi M. Marwani , Muhammad Fazle Rabbee , Maha G. Batterjee , Jehan Y. Al-Humaidi , Zahoor Ahmad , Mohammad Mizanur Rahman Khan , Mohammed M. Rahman
In this approach, nanoscale binary doped materials was prepared by solid state method as Zinc oxide intercalated Cadmium oxide nanocomposites (ZnO-CdO NCs) and then practically implemented for the validation and electrochemical analyses using linear sweep voltammetry (LSV) and cyclic voltametric (CV) methods. Out of all the substances that were causing interferences, the constructed sensor probe showed selectivity towards 4-methoxyphenol (4-MP) due to the molecular interaction onto the intercalated surfaces of ZnO-CdO NCs. The chemical sensor exhibited enhanced electrochemical characteristics, such as higher sensitivity, a wide linear dynamic range (LDR), lower limit of detection (LOD), and good stability in detecting the specific compound 4-MP. For their optical, elemental, functional, morphological, and structural properties, the calcined ZnO-CdO NCs were analyzed using FTIR, UV, FESEM, EDS, XPS, TEM, and XRD techniques, respectively. In sensor fabrication, a flat GCE was constructed by applying a thin layer of NCs using a 5 % Nafion binder as a chemical coating agent. The calibration graph exhibited a linear relationship with a high coefficient of determination (r2 = 0.9680) throughout a broad range of 4-MP concentrations (0.22–7.5 µM). The sensitivity and limit of detection (LOD) were determined to be 1.5189 μAmM−1 cm−2 and 0.01091 µM respectively. The synthesis of ZnO-CdO NCs by solid-state method is a promising approach for developing a phenolic sensor in a broad scale by electrochemical approach. The 4-MP sensor has demonstrated a promising performance using ZnO-CdO NCs by LSV and CV methods. This significantly impacts the identification of hazardous phenolic chemicals by electrochemical methods in the environmental and healthcare sectors, hence ensuring safety.
{"title":"Efficient detection and validation of 4-Methoxyphenol chemical based on binary oxides intercalated ZnO-CdO nanocomposite by electrochemical approach","authors":"Umer Shahzad ,&nbsp;Hadi M. Marwani ,&nbsp;Muhammad Fazle Rabbee ,&nbsp;Maha G. Batterjee ,&nbsp;Jehan Y. Al-Humaidi ,&nbsp;Zahoor Ahmad ,&nbsp;Mohammad Mizanur Rahman Khan ,&nbsp;Mohammed M. Rahman","doi":"10.1016/j.microc.2025.113171","DOIUrl":"10.1016/j.microc.2025.113171","url":null,"abstract":"<div><div>In this approach, nanoscale binary doped materials was prepared by solid state method as Zinc oxide intercalated Cadmium oxide nanocomposites (ZnO-CdO NCs) and then practically implemented for the validation and electrochemical analyses using linear sweep voltammetry (LSV) and cyclic voltametric (CV) methods. Out of all the substances that were causing interferences, the constructed sensor probe showed selectivity towards 4-methoxyphenol (4-MP) due to the molecular interaction onto the intercalated surfaces of ZnO-CdO NCs. The chemical sensor exhibited enhanced electrochemical characteristics, such as higher sensitivity, a wide linear dynamic range (LDR), lower limit of detection (LOD), and good stability in detecting the specific compound 4-MP. For their optical, elemental, functional, morphological, and structural properties, the calcined ZnO-CdO NCs were analyzed using FTIR, UV, FESEM, EDS, XPS, TEM, and XRD techniques, respectively. In sensor fabrication, a flat GCE was constructed by applying a thin layer of NCs using a 5 % Nafion binder as a chemical coating agent. The calibration graph exhibited a linear relationship with a high coefficient of determination (r<sup>2</sup> = 0.9680) throughout a broad range of 4-MP concentrations (0.22–7.5 µM). The sensitivity and limit of detection (LOD) were determined to be 1.5189 μAmM<sup>−1</sup> cm<sup>−2</sup> and 0.01091 µM respectively. The synthesis of ZnO-CdO NCs by solid-state method is a promising approach for developing a phenolic sensor in a broad scale by electrochemical approach. The 4-MP sensor has demonstrated a promising performance using ZnO-CdO NCs by LSV and CV methods. This significantly impacts the identification of hazardous phenolic chemicals by electrochemical methods in the environmental and healthcare sectors, hence ensuring safety.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113171"},"PeriodicalIF":4.9,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561912","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Sr-doped MnO2 with enhanced dual-enzyme mimetic activity for colorimetric detection of glutathione and 2,4-dichlorophenol 掺锶二氧化锰具有增强的双酶模拟活性,可用于谷胱甘肽和 2,4-二氯苯酚的比色检测
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-03-01 DOI: 10.1016/j.microc.2025.113166
Wei Shi , Xueyi Wang , Zhouping Yang , Jun Yang , Xiaoying Fu , Xianxiang Wang
The development of simple and rapid colorimetric methods for monitoring food nutrition and safety is essential for sustaining life and promoting health. Nanozymes, which exhibit high stability and multi-enzyme activity, hold significant promise for widespread applications in colorimetric analysis. In this work, we successfully synthesized strontium-doped MnO2 nanoflowers (Sr-MnO2 NFs) that exhibit both oxidase-like and laccase-like activities. The oxidase activity and laccase activity of the Sr-MnO2 NFs were 2.12 and 3 times greater than those of MnO2 nanorods (MnO2 NRs), respectively. Oxygen vacancies (Ov) and O2 play a key role in oxidase-like and laccase-like enzymes. Leveraging the excellent catalytic properties of these activities, we developed a simple, fast and highly sensitive colorimetric detection method for glutathione (GSH) and 2,4-dichlorophenol (2,4-DP), achieving low detection limits of 0.46 μM and 0.992 μM, respectively. Furthermore, the proposed method has been successfully applied to the determination of GSH and 2,4-DP in food samples.
{"title":"Sr-doped MnO2 with enhanced dual-enzyme mimetic activity for colorimetric detection of glutathione and 2,4-dichlorophenol","authors":"Wei Shi ,&nbsp;Xueyi Wang ,&nbsp;Zhouping Yang ,&nbsp;Jun Yang ,&nbsp;Xiaoying Fu ,&nbsp;Xianxiang Wang","doi":"10.1016/j.microc.2025.113166","DOIUrl":"10.1016/j.microc.2025.113166","url":null,"abstract":"<div><div>The development of simple and rapid colorimetric methods for monitoring food nutrition and safety is essential for sustaining life and promoting health. Nanozymes, which exhibit high stability and multi-enzyme activity, hold significant promise for widespread applications in colorimetric analysis. In this work, we successfully synthesized strontium-doped MnO<sub>2</sub> nanoflowers (Sr-MnO<sub>2</sub> NFs) that exhibit both oxidase-like and laccase-like activities. The oxidase activity and laccase activity of the Sr-MnO<sub>2</sub> NFs were 2.12 and 3 times greater than those of MnO<sub>2</sub> nanorods (MnO<sub>2</sub> NRs), respectively. Oxygen vacancies (Ov) and O<sub>2</sub><sup><img>−</sup> play a key role in oxidase-like and laccase-like enzymes. Leveraging the excellent catalytic properties of these activities, we developed a simple, fast and highly sensitive colorimetric detection method for glutathione (GSH) and 2,4-dichlorophenol (2,4-DP), achieving low detection limits of 0.46 μM and 0.992 μM, respectively. Furthermore, the proposed method has been successfully applied to the determination of GSH and 2,4-DP in food samples.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113166"},"PeriodicalIF":4.9,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561914","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
NiWO4 with oxygen vacancy induced Au nanoparticle signal amplification for electrochemical detection of swine fever virus
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-03-01 DOI: 10.1016/j.microc.2025.113207
Shiyu Jiang , Xiaohong Fu , Min Yang , Jiageng Li , Guowei Deng , Shuyong Shang , Ruibo Qin , Qiang Zhang
Classical swine fever virus (CSFV) represents a significant threat to the pig industry, capable of causing devastating infectious diseases.. It is an urgent need to identify and quantify viruses with a rapid, sensitive and accurate technology. Integration of nanotechnology will allow the development of microdevices combined with electrochemical technology for efficient virus detection. Here, the electrochemical characteristics of MWCNTs-decorated Au-NiWO4 are studied, and an ideal nanomaterial is constructed for immunosensor of CSFV antigen identifying based on steric effects about oxygen vacancy coupling CSFV enhanced reactant adsorption. The developed immunosensor detects CSFV over a range of 2 × 10-13μg·mL−1-8 × 10-9μg·mL−1, and with a detection limit of 1.58 × 10-13 μg·mL−1. In addition, AuNPs/NiWO4/Ć shows an excellent linear relationship at the scanning speed of 10 ∼ 100 mv/s, and the relative standard deviation (RSD) was found to be only 0.60 %. The synergistic integration of MWCNTs/GO, AuNPs and electroactive Au-NiWO4 provides superior signal response when used for the quantification of CSFV from CSFV antigen samples, suggesting the application prospects of this nanomaterial in detection.
{"title":"NiWO4 with oxygen vacancy induced Au nanoparticle signal amplification for electrochemical detection of swine fever virus","authors":"Shiyu Jiang ,&nbsp;Xiaohong Fu ,&nbsp;Min Yang ,&nbsp;Jiageng Li ,&nbsp;Guowei Deng ,&nbsp;Shuyong Shang ,&nbsp;Ruibo Qin ,&nbsp;Qiang Zhang","doi":"10.1016/j.microc.2025.113207","DOIUrl":"10.1016/j.microc.2025.113207","url":null,"abstract":"<div><div>Classical swine fever virus (CSFV) represents a significant threat to the pig industry, capable of causing devastating infectious diseases.. It is an urgent need to identify and quantify viruses with a rapid, sensitive and accurate technology. Integration of nanotechnology will allow the development of microdevices combined with electrochemical technology for efficient virus detection. Here, the electrochemical characteristics of MWCNTs-decorated Au-NiWO<sub>4</sub> are studied, and an ideal nanomaterial is constructed for immunosensor of CSFV antigen identifying based on steric effects about oxygen vacancy coupling CSFV enhanced reactant adsorption. The developed immunosensor detects CSFV over a range of 2 × 10<sup>-13</sup>μg·mL<sup>−1</sup>-8 × 10<sup>-9</sup>μg·mL<sup>−1</sup>, and with a detection limit of 1.58 × 10<sup>-13</sup> μg·mL<sup>−1</sup>. In addition, AuNPs/NiWO<sub>4</sub>/Ć shows an excellent linear relationship at the scanning speed of 10 ∼ 100 mv/s, and the relative standard deviation (RSD) was found to be only 0.60 %. The synergistic integration of MWCNTs/GO, AuNPs and electroactive Au-NiWO<sub>4</sub> provides superior signal response when used for the quantification of CSFV from CSFV antigen samples, suggesting the application prospects of this nanomaterial in detection.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113207"},"PeriodicalIF":4.9,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143548560","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Bio-inspired nanozymes with smartphone-assisted sensor platform for colorimetric detection of ascorbic acid in fruits and supplements
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-03-01 DOI: 10.1016/j.microc.2025.113192
Jun Li , Zue Hu , Yi Peng , Hui Yang , Qian Zhou , Nan Wang , Xianggui Chen , Xiaoqi Yu
Nanozymes have become one of the key applications in the analysis and sensing of food. However, nanozymes presented have shortcomings that limit their further application, such as complex raw material sources, and high condition requirements for synthesis. Cu-GSSG nanozymes under green preparation conditions were synthesized inspired by the detoxification process of glutathione in living organisms. Cu-GSSG nanozymes were further loaded onto filter paper to construct a smartphone-assisted colorimetric sensor test strip for ascorbic acid (AA) detection. As the excellent peroxidase-like enzymes, Cu-GSSG nanozymes showed low AA detection limit of 2.9 μM with a wide linear range of 10–300 μM. Cu-GSSG nanozymes exhibited excellent anti-interference, accuracy, and biocompatibility performances for reliable detection AA in prickly pear juice and 10 supplements. The intelligent colorimetric sensor platform based on the bio-inspired Cu-GSSG nanozymes showed the great potential in rapid detection and large-scale screening of AA in fruits and supplements.
{"title":"Bio-inspired nanozymes with smartphone-assisted sensor platform for colorimetric detection of ascorbic acid in fruits and supplements","authors":"Jun Li ,&nbsp;Zue Hu ,&nbsp;Yi Peng ,&nbsp;Hui Yang ,&nbsp;Qian Zhou ,&nbsp;Nan Wang ,&nbsp;Xianggui Chen ,&nbsp;Xiaoqi Yu","doi":"10.1016/j.microc.2025.113192","DOIUrl":"10.1016/j.microc.2025.113192","url":null,"abstract":"<div><div>Nanozymes have become one of the key applications in the analysis and sensing of food. However, nanozymes presented have shortcomings that limit their further application, such as complex raw material sources, and high condition requirements for synthesis. Cu-GSSG nanozymes under green preparation conditions were synthesized inspired by the detoxification process of glutathione in living organisms. Cu-GSSG nanozymes were further loaded onto filter paper to construct a smartphone-assisted colorimetric sensor test strip for ascorbic acid (AA) detection. As the excellent peroxidase-like enzymes, Cu-GSSG nanozymes showed low AA detection limit of 2.9 μM with a wide linear range of 10–300 μM. Cu-GSSG nanozymes exhibited excellent anti-interference, accuracy, and biocompatibility performances for reliable detection AA in prickly pear juice and 10 supplements. The intelligent colorimetric sensor platform based on the bio-inspired Cu-GSSG nanozymes showed the great potential in rapid detection and large-scale screening of AA in fruits and supplements.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113192"},"PeriodicalIF":4.9,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143534157","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Extraction of natural active ingredients from Eucommia ulmoides leaves by natural deep eutectic solvent-based surfactant-free microemulsion: Experimental and mechanism study
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-03-01 DOI: 10.1016/j.microc.2025.113199
Jian-Dong Wang , Yan-Hao Liu , Yu-Jie Fu
This study presented the development of a nanoscale, tunable surfactant-free microemulsion (SFME) formulated with natural deep eutectic solvents (NaDES) for the efficient extraction of phytochemicals. The NaDES-SFME, composed of octanol, thymol, ethanol and water, was characterized using a ternary phase diagram, conductivity measurements and UV absorption spectroscopy. The optimal NaDES-SFME composition (15 % v/v NADES, 45 % v/v ethanol and 40 % v/v water) demonstrated superior extraction performance compared to conventional solvents, achieving extraction yields of seven phytochemicals from Eucommia ulmoides leaves that were 1.15–3.55 times higher. FT-IR, dynamic light scattering (DLS) and fluorescence microscopy revealed a reverse W/O structure at 46.7 nm, mimicking cell membranes to penetrate plant matrices and dissolve compounds. Ultrasound-assisted extraction, optimized via response surface methodology, achieved a maximum total yield of 9.763 mg/g under the conditions of 50 °C, 41 min and a solid–liquid ratio of 31 mg/mL. The Pareto plot indicated that the extraction time was the main factor affecting the extraction efficiency and the secondary kinetic model could better fit the dissolution pattern of the phytochemicals. Density functional theory (DFT) analysis confirmed hydrogen bonding as the key mechanism for the high extraction yield. Finally, the combination of ethanol addition and rotary evaporation allowed for a high recovery of the phytochemicals, with a recovery rate of more than 96 %. This green, cost-effective and high-yield microemulsion holds promise for industrial-scale phytochemical extraction and utilization.
{"title":"Extraction of natural active ingredients from Eucommia ulmoides leaves by natural deep eutectic solvent-based surfactant-free microemulsion: Experimental and mechanism study","authors":"Jian-Dong Wang ,&nbsp;Yan-Hao Liu ,&nbsp;Yu-Jie Fu","doi":"10.1016/j.microc.2025.113199","DOIUrl":"10.1016/j.microc.2025.113199","url":null,"abstract":"<div><div>This study presented the development of a nanoscale, tunable surfactant-free microemulsion (SFME) formulated with natural deep eutectic solvents (NaDES) for the efficient extraction of phytochemicals. The NaDES-SFME, composed of octanol, thymol, ethanol and water, was characterized using a ternary phase diagram, conductivity measurements and UV absorption spectroscopy. The optimal NaDES-SFME composition (15 % v/v NADES, 45 % v/v ethanol and 40 % v/v water) demonstrated superior extraction performance compared to conventional solvents, achieving extraction yields of seven phytochemicals from <em>Eucommia ulmoides</em> leaves that were 1.15–3.55 times higher. FT-IR, dynamic light scattering (DLS) and fluorescence microscopy revealed a reverse W/O structure at 46.7 nm, mimicking cell membranes to penetrate plant matrices and dissolve compounds. Ultrasound-assisted extraction, optimized via response surface methodology, achieved a maximum total yield of 9.763 mg/g under the conditions of 50 °C, 41 min and a solid–liquid ratio of 31 mg/mL. The Pareto plot indicated that the extraction time was the main factor affecting the extraction efficiency and the secondary kinetic model could better fit the dissolution pattern of the phytochemicals. Density functional theory (DFT) analysis confirmed hydrogen bonding as the key mechanism for the high extraction yield. Finally, the combination of ethanol addition and rotary evaporation allowed for a high recovery of the phytochemicals, with a recovery rate of more than 96 %. This green, cost-effective and high-yield microemulsion holds promise for industrial-scale phytochemical extraction and utilization.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113199"},"PeriodicalIF":4.9,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143547887","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Eco-friendly green HPLC-ELSD and HPLC-UV methods for estimation of hydroxypropyl cellulose, aspartame, and cherry flavor in Montelukast sodium chewable tablets: A reverse engineering approach 用于估算孟鲁司特钠咀嚼片中羟丙基纤维素、阿斯巴甜和樱桃香精的环保型绿色 HPLC-ELSD 和 HPLC-UV 方法:逆向工程方法
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113183
Niroja Vadagam , Karthik Sara , S. Naveen , Chandrasekar Kuppan , Narasimha Swamy Lakka
In this study, a reverse engineering approach is utilized to evaluate and estimate critical excipients in Reference Listed Drug Products (RLDs), aiding in the formulation of cost-effective generics drug products. The key excipients, Hydroxypropyl cellulose (HPC), aspartame, and cherry flavor, used in the manufacturing of Montelukast sodium chewable tablets (for asthma and allergic rhinitis treatment), were quantitatively estimated using newly developed HPLC-UV and HPLC-ELSD methods. HPLC-ELSD separation for HPC was achieved in 35-minutes using a binary gradient consisting of water-formic acid-acetonitrile with a C18 column (150x4.6-mm,4.6-µm), flow rate of 0.4-mL/min, injection volume of 50-µL, column temperature of 35 °C, and evaporator temperature of 85 °C. Aspartame and cherry flavor were estimated using HPLC-UV method consisting of 30-minutes gradient with phosphate buffer-acetonitrile along with a C18 column, flow rate of 0.8-mL/min, injection volume of 50-µL, column temperature of 35 °C, auto-sampler of 10 °C, and UV detection at 220-nm for aspartame and 248-nm for cherry flavor. Method validation studies performed as in-line with the USP<1225> and ICH, Q2(R2) guidelines, demonstrating excellent specificity (no peak overlap and interference), precision, recovery (90.0–110.0 %), and linearity (HPC: 93.839–387.989 µg/mL with R2 > 0.9980; Aspartame: 5.05–119.23 µg/mL with R2 > 0.9998; Cherry flavor; 5.04–121.03 µg/mL with R2 > 0.9999). The validated HPLC-ELSD and HPLC-UV methods were supported real-time quantitative analysis of excipients in Montelukast sodium tablets, aiding in the reverse engineering process for the generic drug products development. These methods and approach can also be utilized for the RLDs where HPC, aspartame and cherry flavor are critical role in generics product development (ANDAs).
{"title":"Eco-friendly green HPLC-ELSD and HPLC-UV methods for estimation of hydroxypropyl cellulose, aspartame, and cherry flavor in Montelukast sodium chewable tablets: A reverse engineering approach","authors":"Niroja Vadagam ,&nbsp;Karthik Sara ,&nbsp;S. Naveen ,&nbsp;Chandrasekar Kuppan ,&nbsp;Narasimha Swamy Lakka","doi":"10.1016/j.microc.2025.113183","DOIUrl":"10.1016/j.microc.2025.113183","url":null,"abstract":"<div><div>In this study, a reverse engineering approach is utilized to evaluate and estimate critical excipients in Reference Listed Drug Products (RLDs), aiding in the formulation of cost-effective generics drug products. The key excipients, Hydroxypropyl cellulose (HPC), aspartame, and cherry flavor, used in the manufacturing of Montelukast sodium chewable tablets (for asthma and allergic rhinitis treatment), were quantitatively estimated using newly developed HPLC-UV and HPLC-ELSD methods. HPLC-ELSD separation for HPC was achieved in 35-minutes using a binary gradient consisting of water-formic acid-acetonitrile with a C<sub>18</sub> column (150x4.6-mm,4.6-µm), flow rate of 0.4-mL/min, injection volume of 50-µL, column temperature of 35 °C, and evaporator temperature of 85 °C. Aspartame and cherry flavor were estimated using HPLC-UV method consisting of 30-minutes gradient with phosphate buffer-acetonitrile along with a C<sub>18</sub> column, flow rate of 0.8-mL/min, injection volume of 50-µL, column temperature of 35 °C, auto-sampler of 10 °C, and UV detection at 220-nm for aspartame and 248-nm for cherry flavor. Method validation studies performed as in-line with the USP&lt;1225&gt; and ICH, Q2(R2) guidelines, demonstrating excellent specificity (no peak overlap and interference), precision, recovery (90.0–110.0 %), and linearity (HPC: 93.839–387.989 µg/mL with R<sup>2</sup> &gt; 0.9980; Aspartame: 5.05–119.23 µg/mL with R<sup>2</sup> &gt; 0.9998; Cherry flavor; 5.04–121.03 µg/mL with R<sup>2</sup> &gt; 0.9999). The validated HPLC-ELSD and HPLC-UV methods were supported real-time quantitative analysis of excipients in Montelukast sodium tablets, aiding in the reverse engineering process for the generic drug products development. These methods and approach can also be utilized for the RLDs where HPC, aspartame and cherry flavor are critical role in generics product development (ANDAs).</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113183"},"PeriodicalIF":4.9,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143527295","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Electrochemical sensor based on nickel phthalocyanine conjugated polymer for selective detection of p-aminophenol
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-28 DOI: 10.1016/j.microc.2025.113191
Xue Cai, Rui Tao, Meitong Li, Xinyu Yun, Xinyu Yang, Jiayue Sun, Chuangyu Wei
This work reports an advanced, high-efficiency electrochemical sensor for detecting p-aminophenol (p-AP), based on a nickel phthalocyanine polymer containing an S-linker. The nickel phthalocyanine polymer was synthesized via the cyclization reaction with ortho-positioned dicyano groups. The nickel phthalocyanine polymer was drop-coated on GCE to form a modified electrode (PNiPc@GCE), which demonstrated sensitive electrochemical responses. Optimal conditions for preparing the modified electrode and detecting p-AP were selected through electrochemical experiments. Cyclic voltammetry (CV) curves at different rates (20 mV s−1 ∼ 200 mV/s) indicated that the oxidation of p-AP follows a diffusion-controlled process on the surface of the PNiPc@GCE electrode. The p-AP, in the range of 0.1 ∼ 1000 μM, was detected using DPV curves, displaying a good linear response under optimal conditions. The sensitivity was determined to be 21.70 mA µM−1 cm−2, and the LOD was 20 nM (S/N = 3). Furthermore, the recovery experiments were conducted at different concentration levels in practical water samples, showing relatively satisfactory recoveries and indicating the potential of the PNiPc@GCE sensor for quantitative detection of p-AP molecules in practical applications. Following storage at room temperature for eight weeks, the sensor remained at 95 % of its original peak current, with negligible interference. Therefore, the developed sensor made a valuable contribution to advancing electrochemical sensing technology and its application in the environment.
{"title":"Electrochemical sensor based on nickel phthalocyanine conjugated polymer for selective detection of p-aminophenol","authors":"Xue Cai,&nbsp;Rui Tao,&nbsp;Meitong Li,&nbsp;Xinyu Yun,&nbsp;Xinyu Yang,&nbsp;Jiayue Sun,&nbsp;Chuangyu Wei","doi":"10.1016/j.microc.2025.113191","DOIUrl":"10.1016/j.microc.2025.113191","url":null,"abstract":"<div><div>This work reports an advanced, high-efficiency electrochemical sensor for detecting p-aminophenol (p-AP), based on a nickel phthalocyanine polymer containing an S-linker. The nickel phthalocyanine polymer was synthesized via the cyclization reaction with <em>ortho</em>-positioned dicyano groups. The nickel phthalocyanine polymer was drop-coated on GCE to form a modified electrode (PNiPc@GCE), which demonstrated sensitive electrochemical responses. Optimal conditions for preparing the modified electrode and detecting p-AP were selected through electrochemical experiments. Cyclic voltammetry (CV) curves at different rates (20 mV s<sup>−1</sup> ∼ 200 mV/s) indicated that the oxidation of p-AP follows a diffusion-controlled process on the surface of the PNiPc@GCE electrode. The p-AP, in the range of 0.1 ∼ 1000 μM, was detected using DPV curves, displaying a good linear response under optimal conditions. The sensitivity was determined to be 21.70 mA µM<sup>−1</sup> cm<sup>−2</sup>, and the LOD was 20 nM (S/N = 3). Furthermore, the recovery experiments were conducted at different concentration levels in practical water samples, showing relatively satisfactory recoveries and indicating the potential of the PNiPc@GCE sensor for quantitative detection of p-AP molecules in practical applications. Following storage at room temperature for eight weeks, the sensor remained at 95 % of its original peak current, with negligible interference. Therefore, the developed sensor made a valuable contribution to advancing electrochemical sensing technology and its application in the environment.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113191"},"PeriodicalIF":4.9,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143534260","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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Microchemical Journal
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