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Carbon cloth-supported flower-shaped NiCo2O4 microsphere for high-performance binder-free non-enzymatic glucose sensor
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-25 DOI: 10.1016/j.microc.2025.113163
Jing Li , Jijie Shi , Hui Ren , Junjie Yang , Dan Xiao , Xiaoqin Li , Xinhui Wang , Yong Guo , Zhaoyu Jin
A novel non-enzymatic glucose sensor is developed by directly growing flower-shaped NiCo2O4 microsphere on flexible carbon cloth (NCO/CC) through a one-step electro-deposition with subsequent mild heat treatment. Benefiting from the excellent conductivity between the three-dimensional (3D) structure of NiCo2O4 and CC, as well as the synergic effect between the nickel and cobalt cations, the NCO/CC can not only offer more additional active sites, but also significantly enhance its electrocatalytic performance. Under the optimized conditions, the NCO/CC electrode reveals excellent activity with a broad linear detection range from 10 to 2000 μM, a high sensitivity of 5260 μA mM−1 cm−2, and a low detection limit (LOD) of 0.2 μM, along with good repeatability and long-term stability. Furthermore, the NCO/CC was successfully utilized to detect glucose in actual beverage samples, showing competitive performance. The straightforward and practical method offers a novel approach to measuring glucose in real-world applications.

Novelty statement

3D flower-shaped NiCo2O4 microspheres growing on flexible carbon cloth (NCO/CC) were fabricated by a facile one-step electro-deposition with subsequent mild heat treatment.
The fabricated NCO/CC electrode exhibits a wide linear detection range, high selectivity, good reproducibility, and stability towards the detection of glucose.
{"title":"Carbon cloth-supported flower-shaped NiCo2O4 microsphere for high-performance binder-free non-enzymatic glucose sensor","authors":"Jing Li ,&nbsp;Jijie Shi ,&nbsp;Hui Ren ,&nbsp;Junjie Yang ,&nbsp;Dan Xiao ,&nbsp;Xiaoqin Li ,&nbsp;Xinhui Wang ,&nbsp;Yong Guo ,&nbsp;Zhaoyu Jin","doi":"10.1016/j.microc.2025.113163","DOIUrl":"10.1016/j.microc.2025.113163","url":null,"abstract":"<div><div>A novel non-enzymatic glucose sensor is developed by directly growing flower-shaped NiCo<sub>2</sub>O<sub>4</sub> microsphere on flexible carbon cloth (NCO/CC) through a one-step electro-deposition with subsequent mild heat treatment. Benefiting from the excellent conductivity between the three-dimensional (3D) structure of NiCo<sub>2</sub>O<sub>4</sub> and CC, as well as the synergic effect between the nickel and cobalt cations, the NCO/CC can not only offer more additional active sites, but also significantly enhance its electrocatalytic performance. Under the optimized conditions, the NCO/CC electrode reveals excellent activity with a broad linear detection range from 10 to 2000 μM, a high sensitivity of 5260 μA mM<sup>−1</sup> cm<sup>−2</sup>, and a low detection limit (LOD) of 0.2 μM, along with good repeatability and long-term stability. Furthermore, the NCO/CC was successfully utilized to detect glucose in actual beverage samples, showing competitive performance. The straightforward and practical method offers a novel approach to measuring glucose in real-world applications.</div></div><div><h3>Novelty statement</h3><div>3D flower-shaped NiCo<sub>2</sub>O<sub>4</sub> microspheres growing on flexible carbon cloth (NCO/CC) were fabricated by a facile one-step electro-deposition with subsequent mild heat treatment.</div><div>The fabricated NCO/CC electrode exhibits a wide linear detection range, high selectivity, good reproducibility, and stability towards the detection of glucose.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113163"},"PeriodicalIF":4.9,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561916","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
Label-free electrochemical aptasensor based on cellulose nanocrystal-modified paper-based device for Salmonella Typhimurium detection in food samples
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-25 DOI: 10.1016/j.microc.2025.113144
Sakda Jampasa , Natthawut Sangthong , Tugba Ozer , Wattana Panphut , Sarida Naorungroj , Nattaya Ngamrojanavanich , Takashi Kaneta , Orawon Chailapakul , Wanida Wonsawat
Salmonella Typhimurium (S. Typhimurium) is a pathogenic bacterium associated with food contamination and severe illnesses. Given its low infectious dose, monitoring this bacterium is critical. Conventional detection methods often involve labor-intensive and time-consuming enzyme-linked immunoassays, further highlighting the need for more efficient alternatives. In this study, we developed a paper-based electrochemical aptasensor utilizing a label-free format, enhanced with carboxyl (COOH)-functionalized cellulose nanocrystals, as an innovative platform for detecting S. Typhimurium. The device was custom-designed and fabricated using a wax printing technique on Whatman filter paper, yielding a disposable and desirable paper-based analytical device (PAD). COOH-cellulose nanocrystals were applied to the PAD surface to directly immobilize an aptamer probe specific to Salmonella, employing effective EDC/NHS standard chemistry without requiring additional modifications. The subsequent formation of a half-sandwich immunocomplex (aptamer/Salmonella) induces a highly insulated layer on the PAD surface, suppressing the redox mediator signal response of [Fe(CN)6]3-/4- in a Salmonella concentration-dependent manner, with detectable ranges from 10 to 109 CFU/mL and an ultra-low detection limit of 3.50 CFU/mL, as evaluated by differential pulse voltammetry. This aptasensor successfully detects the presence of Salmonella in food samples, demonstrating remarkable sensitivity, selectivity, rapid response times (30 min), and portability.
{"title":"Label-free electrochemical aptasensor based on cellulose nanocrystal-modified paper-based device for Salmonella Typhimurium detection in food samples","authors":"Sakda Jampasa ,&nbsp;Natthawut Sangthong ,&nbsp;Tugba Ozer ,&nbsp;Wattana Panphut ,&nbsp;Sarida Naorungroj ,&nbsp;Nattaya Ngamrojanavanich ,&nbsp;Takashi Kaneta ,&nbsp;Orawon Chailapakul ,&nbsp;Wanida Wonsawat","doi":"10.1016/j.microc.2025.113144","DOIUrl":"10.1016/j.microc.2025.113144","url":null,"abstract":"<div><div><em>Salmonella Typhimurium</em> (<em>S. Typhimurium</em>) is a pathogenic bacterium associated with food contamination and severe illnesses. Given its low infectious dose, monitoring this bacterium is critical. Conventional detection methods often involve labor-intensive and time-consuming enzyme-linked immunoassays, further highlighting the need for more efficient alternatives. In this study, we developed a paper-based electrochemical aptasensor utilizing a label-free format, enhanced with carboxyl (COOH)-functionalized cellulose nanocrystals, as an innovative platform for detecting <em>S. Typhimurium</em>. The device was custom-designed and fabricated using a wax printing technique on Whatman filter paper, yielding a disposable and desirable paper-based analytical device (PAD). COOH-cellulose nanocrystals were applied to the PAD surface to directly immobilize an aptamer probe specific to <em>Salmonella</em>, employing effective EDC/NHS standard chemistry without requiring additional modifications. The subsequent formation of a half-sandwich immunocomplex (aptamer/<em>Salmonella</em>) induces a highly insulated layer on the PAD surface, suppressing the redox mediator signal response of [Fe(CN)<sub>6</sub>]<sup>3-/4-</sup> in a <em>Salmonella</em> concentration-dependent manner, with detectable ranges from 10 to 10<sup>9</sup> CFU/mL and an ultra-low detection limit of 3.50 CFU/mL, as evaluated by differential pulse voltammetry. This aptasensor successfully detects the presence of <em>Salmonella</em> in food samples, demonstrating remarkable sensitivity, selectivity, rapid response times (30 min), and portability.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"211 ","pages":"Article 113144"},"PeriodicalIF":4.9,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143487965","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
Integrating hydroponic and soil-cultivated lettuce to understand the translocation, accumulation, subcellular distribution, and metabolism of chiral fungicide mandipropamid
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-25 DOI: 10.1016/j.microc.2025.113167
Ye You , Fanxia Liao , Aihui Zhang , Qin Tang , Jing Shi , Kankan Zhang
The accumulation and translocation of pesticides in crops can lead to several environmental hazards and pose potential threats to food safety and human health. This study demonstrated a strong absorption capacity of mandipropamid by soil-cultivated and hydroponic lettuce roots through an active symplastic pathway, as indicated by high root concentration and quasi-equilibrium factors. Mandipropamid moved minimally, with translocation factors < 1, and was primarily distributed in cell walls of lettuce tissues due to its hydrophobicity (logKow = 3.2) and low solubility (4.2 mg/L). Mandipropamid-contaminated cultivation media were remediated by planting lettuce, resulting in a reduction of half-lives by > 10 %, and enantioselectivity can be observed, with the R-enantiomer preferentially dissipating (enantiomeric factors < 0.5). Eleven potential metabolites were identified by high-resolution mass spectrometry during the cultivation process. This work provides integrated insights into the translocation, distribution, metabolism, and remediation of mandipropamid enantiomers in lettuce under soil-cultivated and hydroponic conditions.
{"title":"Integrating hydroponic and soil-cultivated lettuce to understand the translocation, accumulation, subcellular distribution, and metabolism of chiral fungicide mandipropamid","authors":"Ye You ,&nbsp;Fanxia Liao ,&nbsp;Aihui Zhang ,&nbsp;Qin Tang ,&nbsp;Jing Shi ,&nbsp;Kankan Zhang","doi":"10.1016/j.microc.2025.113167","DOIUrl":"10.1016/j.microc.2025.113167","url":null,"abstract":"<div><div>The accumulation and translocation of pesticides in crops can lead to several environmental hazards and pose potential threats to food safety and human health. This study demonstrated a strong absorption capacity of mandipropamid by soil-cultivated and hydroponic lettuce roots through an active symplastic pathway, as indicated by high root concentration and quasi-equilibrium factors. Mandipropamid moved minimally, with translocation factors &lt; 1, and was primarily distributed in cell walls of lettuce tissues due to its hydrophobicity (logK<sub>ow</sub> = 3.2) and low solubility (4.2 mg/L). Mandipropamid-contaminated cultivation media were remediated by planting lettuce, resulting in a reduction of half-lives by &gt; 10 %, and enantioselectivity can be observed, with the <em>R</em>-enantiomer preferentially dissipating (enantiomeric factors &lt; 0.5). Eleven potential metabolites were identified by high-resolution mass spectrometry during the cultivation process. This work provides integrated insights into the translocation, distribution, metabolism, and remediation of mandipropamid enantiomers in lettuce under soil-cultivated and hydroponic conditions.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113167"},"PeriodicalIF":4.9,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143527290","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
High-throughput mercury speciation analysis of breast milk using HPLC-ICP-MS
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-25 DOI: 10.1016/j.microc.2025.113142
Kenta Iwai , Miyuki Iwai-Shimada , Nozomi Tatsuta , Yayoi Kobayashi , Kaname Asato , Mitsuo Nishimoto , Kunihiko Nakai , Shoji F. Nakayama
Despite concerns regarding infant exposure to methylmercury (MeHg+), few studies have investigated the separate determination of mercury species in breast milk, and breast milk collection methodology has not been adequately examined.
In this study, a high-throughput analytical method was developed for the simultaneous quantification of inorganic mercury (Hg2+) and MeHg+ in human breast milk using high-performance liquid chromatography equipped with inductively coupled plasma mass spectrometry (HPLC-ICP-MS).
Quality control was performed using NIST SRM 1953, a certified reference material for breast milk containing Hg2+ and MeHg+, and the accuracy was 99 %. Furthermore, a 4-month study was conducted in which monthly breast milk samples from 10 participants were analyzed to examine the effects of the collection method (foremilk or hindmilk) and collection time. The median concentrations (ng g−1) for the 80 samples were 0.109 (5th-95th percentile: 0.014–0.365) for Hg2+ and 0.220 (5th–95th percentile: 0.046–0.792) for MeHg+. The total mercury concentrations obtained via HPLC-ICP-MS analysis were compared with those measured using inductively coupled plasma mass spectrometry (ICP-MS), and a high correlation was achieved (Pearson’s correlation coefficient = 0.946).
ICP-MS analysis was conducted to determine the content of several additional elements in the breastmilk samples, and an association was found between the Selenium and Hg2+ contents. In contrast, the MeHg+ and fat contents were correlated, with the MeHg+ concentration being higher in hindmilk.
{"title":"High-throughput mercury speciation analysis of breast milk using HPLC-ICP-MS","authors":"Kenta Iwai ,&nbsp;Miyuki Iwai-Shimada ,&nbsp;Nozomi Tatsuta ,&nbsp;Yayoi Kobayashi ,&nbsp;Kaname Asato ,&nbsp;Mitsuo Nishimoto ,&nbsp;Kunihiko Nakai ,&nbsp;Shoji F. Nakayama","doi":"10.1016/j.microc.2025.113142","DOIUrl":"10.1016/j.microc.2025.113142","url":null,"abstract":"<div><div>Despite concerns regarding infant exposure to methylmercury (MeHg<sup>+</sup>), few studies have investigated the separate determination of mercury species in breast milk, and breast milk collection methodology has not been adequately examined.</div><div>In this study, a high-throughput analytical method was developed for the simultaneous quantification of inorganic mercury (Hg<sup>2+</sup>) and MeHg<sup>+</sup> in human breast milk using high-performance liquid chromatography equipped with inductively coupled plasma mass spectrometry (HPLC-ICP-MS).</div><div>Quality control was performed using NIST SRM 1953, a certified reference material for breast milk containing Hg<sup>2+</sup> and MeHg<sup>+</sup>, and the accuracy was 99 %. Furthermore, a 4-month study was conducted in which monthly breast milk samples from 10 participants were analyzed to examine the effects of the collection method (foremilk or hindmilk) and collection time. The median concentrations (ng g<sup>−1</sup>) for the 80 samples were 0.109 (5th-95th percentile: 0.014–0.365) for Hg<sup>2+</sup> and 0.220 (5th–95th percentile: 0.046–0.792) for MeHg<sup>+</sup>. The total mercury concentrations obtained via HPLC-ICP-MS analysis were compared with those measured using inductively coupled plasma mass spectrometry (ICP-MS), and a high correlation was achieved (Pearson’s correlation coefficient = 0.946).</div><div>ICP-MS analysis was conducted to determine the content of several additional elements in the breastmilk samples, and an association was found between the Selenium and Hg<sup>2+</sup> contents. In contrast, the MeHg<sup>+</sup> and fat contents were correlated, with the MeHg<sup>+</sup> concentration being higher in hindmilk.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"211 ","pages":"Article 113142"},"PeriodicalIF":4.9,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143510525","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A highly specific colorimetric detection of sulfur mustard and nitrogen mustard at room temperature with iodine–starch system
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-25 DOI: 10.1016/j.microc.2025.113169
Lav Kumar Yadav, G. Raviraju, Tuhin Roy, Vinod Kumar
In this investigation, we have developed a novel, selective, and cost-effective colorimetric detection of blister agents e.g., sulfur mustard and nitrogen mustard. This protocol enables the detection at room temperature using ‘everyday reagents’ such as sodium thiosulfate, iodine, and starch. The sensing method utilizes sodium thiosulfate as a receptor and the combination of iodine and starch as an indicator, resulting in a colorimetric response to both mustard agents. The method offers selective detection of these chemical agents over relevant interferences such as nerve agents’ simulant, acylating agent, and alkylating agent. Furthermore, the analyses of these agents in the contaminated environmental samples and Na2S2O3-coated silica gel suggest that this testing technique can be directly applied to real-time investigation. We have also determined the limit of detection for SM and NM to be 0.02 mg visually, and 0.002 mg spectroscopically, both of which are below levels harmful to human skin. This highlights the potential utility and safety of our approach for detecting CW agents in diverse scenarios.
{"title":"A highly specific colorimetric detection of sulfur mustard and nitrogen mustard at room temperature with iodine–starch system","authors":"Lav Kumar Yadav,&nbsp;G. Raviraju,&nbsp;Tuhin Roy,&nbsp;Vinod Kumar","doi":"10.1016/j.microc.2025.113169","DOIUrl":"10.1016/j.microc.2025.113169","url":null,"abstract":"<div><div>In this investigation, we have developed a novel, selective, and cost-effective colorimetric detection of blister agents <em>e.g</em>., sulfur mustard and nitrogen mustard. This protocol enables the detection at room temperature using ‘everyday reagents’ such as sodium thiosulfate, iodine, and starch. The sensing method utilizes sodium thiosulfate as a receptor and the combination of iodine and starch as an indicator, resulting in a colorimetric response to both mustard agents. The method offers selective detection of these chemical agents over relevant interferences such as nerve agents’ simulant, acylating agent, and alkylating agent. Furthermore, the analyses of these agents in the contaminated environmental samples and Na<sub>2</sub>S<sub>2</sub>O<sub>3</sub>-coated silica gel suggest that this testing technique can be directly applied to real-time investigation. We have also determined the limit of detection for SM and NM to be 0.02 mg visually, and 0.002 mg spectroscopically, both of which are below levels harmful to human skin. This highlights the potential utility and safety of our approach for detecting CW agents in diverse scenarios.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"211 ","pages":"Article 113169"},"PeriodicalIF":4.9,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143511307","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
Chitosan composited covalent organic framework nanoparticles for the dispersive micro-solid-phase extraction of chlorpyrifos pesticide from environmental water samples prior to spectrophotometric determination
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-25 DOI: 10.1016/j.microc.2025.113153
Ahmad Reza Bagheri, Ardeshir Shokrollahi
In this study, chitosan (CS), as a green, low- or negligible toxic, low-cost, biocompatible, biodegradable, and environmentally friendly compound, was composited with covalent organic framework (COF) nanoparticles. Following the synthesis, the nanocomposite (COF-CS) was characterized and identified by diverse techniques such as Fourier-transform infrared spectroscopy (FT-IR), field emission-scanning electron microscopy-energy dispersive spectroscopy (FESEM-EDS), and Brunauer-Emmett-Teller (BET) surface area analysis. The COF-CS was subsequently employed for dispersive micro-solid-phase extraction (D-µ-SPE) of the chlorpyrifos (CPF) pesticide from environmental water samples prior to spectrophotometric determination. The factors that affect the extraction process were examined and optimized through the application of central composite design-based response surface methodology (CCD-RSM). The primary benefit of the COF-CS nanocomposite lies in its ability to address several significant limitations of CS, including its inadequate adsorption capacity, limited specific surface area, and low stability. Moreover, the COF-CS nanocomposite has the potential to resolve the primary issues associated with COF nanoparticles, specifically their propensity for aggregation and the challenges in separation due to their low density. Another key benefit of the COF-CS nanocomposite is that it provides multiple interaction sites, including hydrogen bonding and π-π interaction with CPF, to further improve the extraction efficiency. According to the CCD-RSM, the optimum parameters were pH (4.5), elution volume (300 µL of methanol), sorbent dosage (10 mg), and extraction time (12 min). Under the optimized conditions, the linear range of the method was from 10.0 to 700.0 µg L−1. In addition, the limit of detection of the method was achieved to be 3.9 µg L−1.
{"title":"Chitosan composited covalent organic framework nanoparticles for the dispersive micro-solid-phase extraction of chlorpyrifos pesticide from environmental water samples prior to spectrophotometric determination","authors":"Ahmad Reza Bagheri,&nbsp;Ardeshir Shokrollahi","doi":"10.1016/j.microc.2025.113153","DOIUrl":"10.1016/j.microc.2025.113153","url":null,"abstract":"<div><div>In this study, chitosan (CS), as a green, low- or negligible toxic, low-cost, biocompatible, biodegradable, and environmentally friendly compound, was composited with covalent organic framework (COF) nanoparticles. Following the synthesis, the nanocomposite (COF-CS) was characterized and identified by diverse techniques such as Fourier-transform infrared spectroscopy (FT-IR), field emission-scanning electron microscopy-energy dispersive spectroscopy (FESEM-EDS), and Brunauer-Emmett-Teller (BET) surface area analysis. The COF-CS was subsequently employed for dispersive micro-solid-phase extraction (D-µ-SPE) of the chlorpyrifos (CPF) pesticide from environmental water samples prior to spectrophotometric determination. The factors that affect the extraction process were examined and optimized through the application of central composite design-based response surface methodology (CCD-RSM). The primary benefit of the COF-CS nanocomposite lies in its ability to address several significant limitations of CS, including its inadequate adsorption capacity, limited specific surface area, and low stability. Moreover, the COF-CS nanocomposite has the potential to resolve the primary issues associated with COF nanoparticles, specifically their propensity for aggregation and the challenges in separation due to their low density. Another key benefit of the COF-CS nanocomposite is that it provides multiple interaction sites, including hydrogen bonding and π-π interaction with CPF, to further improve the extraction efficiency. According to the CCD-RSM, the optimum parameters were pH (4.5), elution volume (300 µL of methanol), sorbent dosage (10 mg), and extraction time (12 min). Under the optimized conditions, the linear range of the method was from 10.0 to 700.0 µg L<sup>−1</sup>. In addition, the limit of detection of the method was achieved to be 3.9 µg L<sup>−1</sup>.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"211 ","pages":"Article 113153"},"PeriodicalIF":4.9,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143511442","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
Development of solid-phase microextraction fibers based on hybrid MIL-68(Fe)@MIL-101(Fe) for the analysis of polycyclic aromatic hydrocarbons in surface waters 开发基于混合 MIL-68(Fe)@MIL-101(Fe)的固相微萃取纤维,用于分析地表水中的多环芳烃
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-25 DOI: 10.1016/j.microc.2025.113143
Sol Giovannoni , Gabriela A. Ortega-Moreno , Griselda Narda , Mario Reta , Carlina Lancioni
The development of solid-phase microextraction fibers (SPME) using a MOF-based hybrid material as sorbent is presented. Even though different metal–organic frameworks (MOFs) have been reported as extractant phases, it is the first time that a hybrid material consisting of two iron-based MOFs is used with this purpose. In this work, the synthesis and characterization of the hybrid MIL-68(Fe)@MIL-101(Fe), as well as, the construction and characterization of the SPME fibers, is detailed. The assessment of its analytical performance, was studied by analyzing five polycyclic aromatic hydrocarbons (PAHs) in aqueous solution by means of gas chromatography coupled to flame ionization and mass spectrometry detectors. The developed analytical method exhibited detection limits between 3 to 10 μg·L−1, good linearity (R2 > 0.96) and remarkable intra-day (average RSD%=10) and inter-day (average RSD% = 14) precision. Moreover, enrichment factors ranged from 187 to 273-fold while accuracies (expressed as percentage recoveries) ranged from 64 to 111 %, and 84 to 123 % for low and high concentration levels, respectively. The developed method was successfully applied to the determination and quantification of PAHs in surface water samples, collected from two streams located in La Plata (Buenos Aires Province, Argentina).
{"title":"Development of solid-phase microextraction fibers based on hybrid MIL-68(Fe)@MIL-101(Fe) for the analysis of polycyclic aromatic hydrocarbons in surface waters","authors":"Sol Giovannoni ,&nbsp;Gabriela A. Ortega-Moreno ,&nbsp;Griselda Narda ,&nbsp;Mario Reta ,&nbsp;Carlina Lancioni","doi":"10.1016/j.microc.2025.113143","DOIUrl":"10.1016/j.microc.2025.113143","url":null,"abstract":"<div><div>The development of solid-phase microextraction fibers (SPME) using a MOF-based hybrid material as sorbent is presented. Even though different metal–organic frameworks (MOFs) have been reported as extractant phases, it is the first time that a hybrid material consisting of two iron-based MOFs is used with this purpose. In this work, the synthesis and characterization of the hybrid MIL-68(Fe)@MIL-101(Fe), as well as, the construction and characterization of the SPME fibers, is detailed. The assessment of its analytical performance, was studied by analyzing five polycyclic aromatic hydrocarbons (PAHs) in aqueous solution by means of gas chromatography coupled to flame ionization and mass spectrometry detectors. The developed analytical method exhibited detection limits between 3 to 10 μg·L<sup>−1</sup>, good linearity (R<sup>2</sup> &gt; 0.96) and remarkable intra-day (average RSD%=10) and inter-day (average RSD% = 14) precision. Moreover, enrichment factors ranged from 187 to 273-fold while accuracies (expressed as percentage recoveries) ranged from 64 to 111 %, and 84 to 123 % for low and high concentration levels, respectively. The developed method was successfully applied to the determination and quantification of PAHs in surface water samples, collected from two streams located in La Plata (Buenos Aires Province, Argentina).</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"211 ","pages":"Article 113143"},"PeriodicalIF":4.9,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143487285","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
Classifying cell viability using a label-free approach: Integration of phase-contrast imaging, Raman spectroscopy, and deep learning
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-25 DOI: 10.1016/j.microc.2025.113159
Yi-Ting Lai , Yi-Chen Li , Yih-Fan Chen , Ji-Yen Cheng
Cell viability assays have been widely used to discover and evaluate a compound in drug development and cancer research. The conventional cell viability assays usually rely on colorimetric and fluorescence techniques to quantify cellular metabolism and viability. However, these techniques may potentially damage cells, affecting the accuracy of cell viability measurements. To address these concerns, we developed an automatic cell viability classification system based on a simple biological microscope to predict cell viability from label-free phase-contrast images. The system automatically obtains single-cell positions and images, which are then analyzed by a trained deep-learning model to classify cell viability. After image acquisition, the single-cell viability was used to Raman spectroscopy to quantify the MTT formazan, which correlated to cellular metabolic activity. For classifying cell viability, three CNN-based models (VGG-16, DenseNet-121, and Xception) were employed. According to the results, the VGG-16 model achieved the highest performance, with an average accuracy and sensitivity of 89 % in 3-fold cross-validation to classify cell viability between non- and minor-damaged conditions. The results therefore demonstrated that the developed system provides a simple and efficient solution for classifying cell viability, with promising applications in biomedical research and drug screening.
{"title":"Classifying cell viability using a label-free approach: Integration of phase-contrast imaging, Raman spectroscopy, and deep learning","authors":"Yi-Ting Lai ,&nbsp;Yi-Chen Li ,&nbsp;Yih-Fan Chen ,&nbsp;Ji-Yen Cheng","doi":"10.1016/j.microc.2025.113159","DOIUrl":"10.1016/j.microc.2025.113159","url":null,"abstract":"<div><div>Cell viability assays have been widely used to discover and evaluate a compound in drug development and cancer research. The conventional cell viability assays usually rely on colorimetric and fluorescence techniques to quantify cellular metabolism and viability. However, these techniques may potentially damage cells, affecting the accuracy of cell viability measurements. To address these concerns, we developed an automatic cell viability classification system based on a simple biological microscope to predict cell viability from label-free phase-contrast images. The system automatically obtains single-cell positions and images, which are then analyzed by a trained deep-learning model to classify cell viability. After image acquisition, the single-cell viability was used to Raman spectroscopy to quantify the MTT formazan, which correlated to cellular metabolic activity. For classifying cell viability, three CNN-based models (VGG-16, DenseNet-121, and Xception) were employed. According to the results, the VGG-16 model achieved the highest performance, with an average accuracy and sensitivity of 89 % in 3-fold cross-validation to classify cell viability between non- and minor-damaged conditions. The results therefore demonstrated that the developed system provides a simple and efficient solution for classifying cell viability, with promising applications in biomedical research and drug screening.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113159"},"PeriodicalIF":4.9,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143547963","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
Acacia auriculiformis mediated synthesis of silver nanoparticles for the sensitive and rapid electrochemical sensing of nitrite in water sample
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-25 DOI: 10.1016/j.microc.2025.113162
Tafazzul Sheikh , Vasundra Nagendran , Kotian Shakshi Vasant , Ujwal Mallya , Srinivas Mutalik , Fasiulla Khan , Sneha Nayak , Sarvajith Malali Sudhakara
This study presents a novel and cost-effective approach for the detection of nitrite ions using biosynthesized silver nanoparticles from the aqueous leaf extract of Acacia auriculiformis. The use of phytochemicals from the plant extract to act as reducing agents is an eco-friendly and sustainable approach for the preparation of nanoparticles. The immobilization of the synthesized nanoparticles on the glassy carbon electrode (GCE) with a nafion binder resulted in a highly sensitive and selective nitrite sensor. The fabricated AcAgNPs/GCE sensor exhibited superior electrocatalytic activity towards nitrite ions with a low LOD of 71.2 nM (nanomolar concentrations) and a sensitivity of 0.3411 µA µM−1 cm−2 making it a promising sensor for the sensitive detection of nitrite in ecological samples. The study focuses on the potential of green-mediated silver nanoparticles in the development of cost-effective and eco-friendly sensors for environmental monitoring.
{"title":"Acacia auriculiformis mediated synthesis of silver nanoparticles for the sensitive and rapid electrochemical sensing of nitrite in water sample","authors":"Tafazzul Sheikh ,&nbsp;Vasundra Nagendran ,&nbsp;Kotian Shakshi Vasant ,&nbsp;Ujwal Mallya ,&nbsp;Srinivas Mutalik ,&nbsp;Fasiulla Khan ,&nbsp;Sneha Nayak ,&nbsp;Sarvajith Malali Sudhakara","doi":"10.1016/j.microc.2025.113162","DOIUrl":"10.1016/j.microc.2025.113162","url":null,"abstract":"<div><div>This study presents a novel and cost-effective approach for the detection of nitrite ions using biosynthesized silver nanoparticles from the aqueous leaf extract of <em>Acacia auriculiformis</em>. The use of phytochemicals from the plant extract to act as reducing agents is an eco-friendly and sustainable approach for the preparation of nanoparticles. The immobilization of the synthesized nanoparticles on the glassy carbon electrode (GCE) with a nafion binder resulted in a highly sensitive and selective nitrite sensor. The fabricated AcAgNPs/GCE sensor exhibited superior electrocatalytic activity towards nitrite ions with a low LOD of 71.2 nM (nanomolar concentrations) and a sensitivity of 0.3411 µA µM<sup>−1</sup> cm<sup>−2</sup> making it a promising sensor for the sensitive detection of nitrite in ecological samples. The study focuses on<!--> <!-->the potential of green-mediated silver nanoparticles in the development of cost-effective and eco-friendly sensors for environmental monitoring.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"211 ","pages":"Article 113162"},"PeriodicalIF":4.9,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143509912","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
A ratiometric fluorescence probe based on porphyrin-based MOF for phosphate ions detection
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-25 DOI: 10.1016/j.microc.2025.113156
Yuanfeng Zhang , Baoping Ren , Wenyue Dong , Qian Duan , Teng Fei
Porphyrin-based metal-organic frameworks (MOFs) are a type of periodic network framework materials constructed from porphyrin or metalloporphyrin as the structural unit with metal ions or metal clusters. Due to their unique photoelectric property, porphyrin-based MOFs have potential application in fluorescence (FL) sensing. In this study, we have successfully prepared porphyrin-based MOF (Zn-TCPP(BPDC)) using the hydrothermal method, based on 5,10,15,20-tetra(4-carboxyphenyl)porphyrin (TCPP) as first ligand, 4,4′-biphenyldicarboxylic acid (BPDC) as second ligand and Zn2+ as the metal node. The structure, morphology and porosity of Zn-TCPP(BPDC) were characterized using Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and N2 adsorption isotherms. Zn-TCPP(BPDC) exhibits a sheet-like structure with a side length of ca. 1 μm. The Brunauer-Emmett-Teller (BET) surface area is 98.5 m2/g, and the pore size is mainly concentrated at 2.5 nm. The porosity could provide channels for the adsorption and diffusion of analytes, which helps to improve sensing performance. Zn-TCPP(BPDC) exhibits high sensitivity and low detection limit towards phosphate ions (Pi), which is attributed to strong coordination of phosphate to Zn2+ that leads to the collapse of the layered structure of Zn-TCPP(BPDC), resulting in the release of TCPP monomers and enhanced FL emission. Additionally, FL sensing with single-wavelength is susceptible to environmental interference, which reduces the reliability. To address this, carbon dots (CDs) were introduced into the sensing system of Zn-TCPP(BPDC) aqueous solution to provide a reference FL signal, enabling visualization of the ratiometric FL sensing for Pi in aqueous solution with a low detection limit (0.13 μM), excellent anti-interference and selectivity. Finally, a portable sensing platform was constructed using a smart phone color recognizer, enabling real-time and visual ratiometric FL sensing of Pi.
{"title":"A ratiometric fluorescence probe based on porphyrin-based MOF for phosphate ions detection","authors":"Yuanfeng Zhang ,&nbsp;Baoping Ren ,&nbsp;Wenyue Dong ,&nbsp;Qian Duan ,&nbsp;Teng Fei","doi":"10.1016/j.microc.2025.113156","DOIUrl":"10.1016/j.microc.2025.113156","url":null,"abstract":"<div><div>Porphyrin-based metal-organic frameworks (MOFs) are a type of periodic network framework materials constructed from porphyrin or metalloporphyrin as the structural unit with metal ions or metal clusters. Due to their unique photoelectric property, porphyrin-based MOFs have potential application in fluorescence (FL) sensing. In this study, we have successfully prepared porphyrin-based MOF (Zn-TCPP(BPDC)) using the hydrothermal method, based on 5,10,15,20-tetra(4-carboxyphenyl)porphyrin (TCPP) as first ligand, 4,4′-biphenyldicarboxylic acid (BPDC) as second ligand and Zn<sup>2+</sup> as the metal node. The structure, morphology and porosity of Zn-TCPP(BPDC) were characterized using Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and N<sub>2</sub> adsorption isotherms. Zn-TCPP(BPDC) exhibits a sheet-like structure with a side length of ca. 1 μm. The Brunauer-Emmett-Teller (BET) surface area is 98.5 m<sup>2</sup>/g, and the pore size is mainly concentrated at 2.5 nm. The porosity could provide channels for the adsorption and diffusion of analytes, which helps to improve sensing performance. Zn-TCPP(BPDC) exhibits high sensitivity and low detection limit towards phosphate ions (Pi), which is attributed to strong coordination of phosphate to Zn<sup>2+</sup> that leads to the collapse of the layered structure of Zn-TCPP(BPDC), resulting in the release of TCPP monomers and enhanced FL emission. Additionally, FL sensing with single-wavelength is susceptible to environmental interference, which reduces the reliability. To address this, carbon dots (CDs) were introduced into the sensing system of Zn-TCPP(BPDC) aqueous solution to provide a reference FL signal, enabling visualization of the ratiometric FL sensing for Pi in aqueous solution with a low detection limit (0.13 μM), excellent anti-interference and selectivity. Finally, a portable sensing platform was constructed using a smart phone color recognizer, enabling real-time and visual ratiometric FL sensing of Pi.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"211 ","pages":"Article 113156"},"PeriodicalIF":4.9,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143511443","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
期刊
Microchemical Journal
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