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BACKGROUND: As promising biomarkers of diabetes, α-glucosidase (α-Glu) and ß-glucosidase (ß-Glu) play a crucial role in the diagnosis and management of diseases. However, there is a scarcity of techniques available for simultaneously and sensitively detecting both enzymes. What's more, most of the approaches for detecting α-Glu and ß-Glu rely on a single-mode readout, which can be affected by multiple factors leading to inaccurate results. Hence, the simultaneous detection of the activity levels of both enzymes in a single sample utilizing multiple-readout sensing approaches is highly attractive. RESULTS: In this work, we constructed a facile sensing platform for the simultaneous determination of α-Glu and ß-Glu by utilizing a luminescent covalent organic framework (COF) as a fluorescent indicator. The enzymatic hydrolysis product common to both enzymes, p-nitrophenol (PNP), was found to affect the fluorometric signal through an inner filter effect on COF, enhance the colorimetric response by intensifying the absorption peak at 400 nm, and induce changes in RGB values when analyzed using a smartphone-based color recognition application. By combining fluorometric/colorimetric measurements with smartphone-assisted RGB mode, we achieved sensitive and accurate quantification of α-Glu and ß-Glu. The limits of detection for α-Glu were determined to be 0.8, 1.22, and 1.85 U/L, respectively. Similarly, the limits of detection for ß-Glu were 0.16, 0.42, and 0.53 U/L, respectively. SIGNIFICANCE: Application of the proposed sensing platform to clinical serum samples revealed significant differences in the two enzymes between healthy people and diabetic patients. Additionally, the proposed sensing method was successfully applied for the screening of α-Glu inhibitors and ß-Glu inhibitors, demonstrating its viability and prospective applications in the clinical management of diabetes as well as the discovery of antidiabetic medications.
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Inhibidores de Glicósido Hidrolasas , Estructuras Metalorgánicas , alfa-Glucosidasas , beta-Glucosidasa , Estructuras Metalorgánicas/química , Humanos , Inhibidores de Glicósido Hidrolasas/farmacología , Inhibidores de Glicósido Hidrolasas/química , beta-Glucosidasa/antagonistas & inhibidores , beta-Glucosidasa/metabolismo , alfa-Glucosidasas/metabolismo , alfa-Glucosidasas/sangre , Colorimetría/métodos , Límite de Detección , Nitrofenoles/metabolismo , Nitrofenoles/química , Nitrofenoles/análisis , Evaluación Preclínica de Medicamentos , Colorantes Fluorescentes/químicaRESUMEN
Herein, we reported the dual functions of molybdenum disulfide/sulfur-doped graphitic carbon nitride (MoS2/SGCN) composite as a sensing material for electrochemical detection of 4-NP and a catalyst for 4-NP degradation. The MoS2 nanosheet, sulfur-doped graphitic carbon nitride (SGCN) and MoS2/SGCN were characterized using field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) spectroscopy and X-ray photoelectron spectroscopy (XPS). Electrochemical characterization of these materials with electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) in 1â¯mM K4[Fe(CN)6]3-/4- show that the composite has the lowest charge transfer resistance and the best electrocatalytic activity. The limit of detection (LOD) and the linear range of 4-nitrophenol at MoS2/SGCN modified glassy carbon electrode (MoS2/SGCN/GCE) were computed as 12.8â¯nM and 0.1 - 2.6 µM, respectively. Also, the percentage recoveries of 4-NP in spiked tap water samples ranged from 97.8 - 99.1â¯%. The electroanalysis of 4-NP in the presence of notable interferons shows that the proposed electrochemical sensor features outstanding selectivity toward 4-NP. Additionally, the results of the catalytic degradation of 4-NP at MoS2/SGCN show that the nanocatalyst catalyzed the transformation of 4-NP to 4-aminophenol (4-AP) with a first-order rate constant (k) estimated to be 4.2 ×10-2 s-1. The results of this study confirm that the MoS2/SGCN nanocatalyst is a useful implement for electroanalytical monitoring and catalytic degradation of the hazardous 4-NP in water samples.
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Disulfuros , Técnicas Electroquímicas , Grafito , Límite de Detección , Molibdeno , Nitrofenoles , Contaminantes Químicos del Agua , Molibdeno/química , Molibdeno/análisis , Nitrofenoles/análisis , Nitrofenoles/química , Técnicas Electroquímicas/métodos , Disulfuros/química , Catálisis , Contaminantes Químicos del Agua/análisis , Grafito/química , Compuestos de Nitrógeno/química , Compuestos de Nitrógeno/análisis , ElectrodosRESUMEN
A wearable glove-based sensor is a portable and practical approach for onsite detection/monitoring of a variety of chemical threats. Herein, we report a flexible and sensitive wearable sensor fabricated on the nitrile glove fingertips by stencil-printing technique. The working electrodes were modified with multiwalled carbon nanotubes (MWCNTs)/poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) for sensitive and real-time analyses of hazardous or chemical treats, as picric acid (PA) explosive, diazepam (DZ) as drug-facilitated crimes and the emerging pollutant 4-nitrophenol (4-NP). The multi-sensing platform towards PA, 4-NP, and DZ offers the ability of in-situ qualitative and quantitative analyses of powder and liquid samples. A simple sampling by touching or swiping the fingertip sensor on the sample or surface under investigation using an ionic hydrogel combined with fast voltammetry measurement provides timely point-of-need analyses. The wearable glove-based sensor uses the square wave voltammetry (SWV) technique and exhibited excellent performance to detect PA, 4-NP, and DZ, resulting in limits of detection (LOD) of 0.24 µM, 0.35 µM, 0.06 µM, respectively, in a wide concentration range (from 0.5 µM to 100 µM). Also, we obtained excellent manufacturing reproducibility with relative standard deviations (RSD) in the range of 3.65%-4.61% using 7 different wearable devices (n = 7) and stability in the range of 4.86%-6.61% using different electrodes stored for 10 days at room temperature (n = 10), demonstrating the excellent sensor-to-sensor reproducibility and stability for reliable in-field measurements. The stretchable sensor presented great mechanical robustness, supporting up to 80 bending or stretching deformation cycles without significant voltammetric changes. Collectively, our wearable glove-based sensor may be employed for analyses of chemical contaminants of concern, such as explosives (PA), drugs (DZ), and emerging pollutants (4-NP), helping in environmental and public safety control.
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Diazepam , Técnicas Electroquímicas , Nanotubos de Carbono , Nitrofenoles , Dispositivos Electrónicos Vestibles , Nanotubos de Carbono/química , Nitrofenoles/análisis , Técnicas Electroquímicas/instrumentación , Técnicas Electroquímicas/métodos , Diazepam/análisis , Electrodos , Humanos , Límite de Detección , Sustancias Explosivas/análisis , Polímeros/química , PicratosRESUMEN
Nitrophenols, a versatile intermediate, have been widely used in leather, medicine, chemical synthesis, and other fields. Because these components are widely applied, they can enter the environment through various routes, leading to many hazards and toxicities. There has been a recent surge in the development of simple, rapid, environmentally friendly, and effective techniques for determining these environmental pollutants. This review provides a comprehensive overview of the latest research progress on the pretreatment and analysis methods of nitrophenols since 2017, with a focus on environmental samples. Pretreatment methods include liquid-liquid extraction, solid-phase extraction, dispersive extraction, and microextraction methods. Analysis methods mainly include liquid chromatography-based methods, gas chromatography-based methods, supercritical fluid chromatography. In addition, this review also discusses and compares the advantages/disadvantages and development prospects of different pretreatment and analysis methods to provide a reference for further research.
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Contaminantes Ambientales , Nitrofenoles , Contaminantes Ambientales/análisis , Nitrofenoles/análisis , Monitoreo del Ambiente/métodos , Extracción Líquido-Líquido/métodos , Extracción en Fase Sólida , Cromatografía Liquida , Cromatografía de Gases , Cromatografía con Fluido Supercrítico/métodosRESUMEN
Fluorescent microspheres are of significant interests due to their wide applications in biotechnology fields. However, their preparation presents several challenges, such as the need for dye labeling, the complexity of materials and often sophisticated preparation conditions. Here a simple process for hydrophilic and crosslinked polyurethane (CPU) microspheres, with carboxyl groups on the surface via one-step precipitation polymerization in 40 min, is presented. The microsphere size is easily adjusted by varying experimental conditions. CPU microspheres exhibit high thermal and pH stability with good redispersibility in water, and emit fluorescence without any modification or dye labeling. The emission mechanism is discussed. CPU microspheres are used as fluorescent probe to detect 4-nitrophenol (4-NP) based on their emission in UV light region, with excellent selectivity and sensitivity. In addition, they are reusable with detection limit unchanged after 7 cycles of reuses, a significant feature of this work. The mechanism of fluorescence detection is thoroughly explored and ascribed to the internal filtration effect. Based on the emission in visible light region, CPU microspheres are used as a model of PU microplastics (MPs) to visualize their biodistribution in HeLa and macrophage cells, as well as in zebrafish larvae, providing a reliable tracer for the visualization and tracking of PU MPs in organisms.
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Colorantes Fluorescentes , Microplásticos , Microesferas , Nitrofenoles , Poliuretanos , Pez Cebra , Poliuretanos/química , Animales , Nitrofenoles/análisis , Nitrofenoles/química , Humanos , Células HeLa , Colorantes Fluorescentes/química , Microplásticos/análisis , Tamaño de la Partícula , Propiedades de Superficie , Ratones , Imagen ÓpticaRESUMEN
The large use and emission of p-nitrophenol (p-NP) seriously pollute the environment and endanger human health. In this work, a hydrazone-linked fluorescent covalent organic framework (BATHz-COF) was simply synthesized at room temperature and covalently linked N-acetyl-L-cysteine (NALC) via the "thiol-ene" click reaction, where carboxyl groups were introduced to improve dispersion and fluorescence intensity. As a rapid, good selectivity and reusability fluorescence sensor, the obtained COF-NALC has been used for quantitative analysis of p-NP predicated on the internal filtering effect (IFE). Under optimal conditions, COF-NALC enabled quantitative detection of p-NP with a linear range of 5-50 µM and the detection limit was 1.46 µM. The application of COF-NALC to the detection of p-NP in river water samples was successful, and the satisfactory recoveries were 98.0%-109.3%. Furthermore, the fluorescent COF paper chips constructed by in situ growth were combined with a smartphone to build a visual platform for the quick and real-time detection of p-NP, providing an excellent illustration for the development of intelligent fluorescence sensing in environmental analysis.
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Hidrazonas , Nitrofenoles , Contaminantes Químicos del Agua , Nitrofenoles/análisis , Nitrofenoles/química , Hidrazonas/química , Contaminantes Químicos del Agua/análisis , Cisteína/análisis , Cisteína/química , Límite de Detección , Colorantes Fluorescentes/química , Estructuras Metalorgánicas/química , Papel , Fluorescencia , Monitoreo del Ambiente/métodos , Espectrometría de Fluorescencia , Ríos/químicaRESUMEN
The detection and quantification of p-Nitrophenol in environmental samples are important for understanding the extent and impact of environmental pollution, protecting human health, ensuring regulatory compliance, and guiding remediation efforts. The main objective of this work was to investigate the electrochemical performance of a graphene oxide/cellulose nanofibril composite (GO/CNF) modified carbon paste electrode (GO/CNF/CPE) for the sensitive and reliable detection of p-nitrophenol in water samples. The transmission electron microscopy (TEM) technique was employed to enlighten the structure of nanocomposites. The electrochemical behavior of the fabricated electrochemical sensor was characterized via differential pulse voltammetry (DPV), linear sweep voltammetry (LSV), and electrochemical impedance spectroscopy (EIS). Under optimized analytical conditions, the peak current of the analyte showed a wide linear relationship with its concentration in a range of 3.0 nM-210 µM with a low amount of the limit of detection (LOD) value of 0.8 nM determined by the DPV method. The proposed electrochemical sensor demonstrated excellent sensitivity, selectivity, and accuracy metrics in real sample analysis of p-nitrophenol.
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Grafito , Contaminantes del Agua , Humanos , Celulosa , Contaminantes del Agua/análisis , Nitrofenoles/análisis , Grafito/química , Electrodos , Técnicas Electroquímicas/métodosRESUMEN
Through field trials and residue analysis, the dissipation behaviour and final residue levels of sodium nitrophenol on jujube were clarified to provide a basis for its safe application and the development of maximum residue limits. The samples were extracted with acetonitrile, cleaned up by a hydrophilic-lipophilic balanced solid-phase extraction column, determined by ultra-high LC-tandem mass spectrometry and quantified by the external standard method. The mean recoveries of sodium 5-nitroguaiacolate, sodium o-nitrophenol and sodium p-nitrophenol were 88.9%-103.8%, with relative standard deviations less than 13.6% at 0.002-0.2 mg/kg spiked levels. Sodium nitrophenol in jujube was dissipated according to the first-order kinetic equation with half-lives of 12.7-17.4 days. At a harvesting interval of 7 days, the residues of sodium nitrophenol in jujube were lower than the limit of 0.03 mg/kg established by the European Food Safety Authority. Residues of jujube were acceptable at a harvest interval of 7 days when sodium nitrophenol was sprayed twice at 9.0 mg/kg with an interval of 7 days. Therefore, the safety interval for sodium nitrophenol application on jujube can be set as 7 days.
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Residuos de Plaguicidas , Ziziphus , Cromatografía Líquida de Alta Presión/métodos , Cromatografía Liquida/métodos , Nitrofenoles/análisis , Residuos de Plaguicidas/análisis , Sodio/análisis , Espectrometría de Masas en Tándem/métodosRESUMEN
A highly effective fluorescent molecularly imprinted sensor (F-PDA-MIS) based on fluorescent polydopamine (F-PDA) was successfully synthesized for selective and ultrafast detection of p-nitrophenol (P-NP) in drinking water. F-PDA with abundant surface functional groups has been artfully modified to firstly serve as both fluorescent monomer and functional monomer in the synthesis of a uniform luminous F-PDA-MIS, which can greatly improve the detection efficiency. As expected, F-PDA-MIS had an obvious emission wavelength of 535 nm with the optimal excitation wavelength at 400 nm. Specially, F-PDA-MIS could detect P-NP in the range 100 to 1100 nM with much lower detection limit of 24.2 nM within 120 s compared with other conventional imprinted fluorescent sensors based on pure quantum dots (QDs) or dyes. This excellent test phenomenon is mainly ascribed to the rapid electron transfer between F-PDA and P-NP. Satisfactory recovery of 98.0-104% for mineral water and 98.6-106% for boiling water were obtained with relative standard deviations (RSDs) of 2.7-3.4% and 2.6-3.5% respectively. The detection reliability of F-PDA-MIS was verified by the comparison with high-performance liquid chromatography (HPLC-UV). Consequently, F-PDA as a fluorescence functional monomer has been shown to be a possible strategy to effectively improve the detection limit and shorten response time of the target determination in water..
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Agua Potable/análisis , Colorantes Fluorescentes/química , Indoles/química , Polímeros Impresos Molecularmente/química , Nitrofenoles/análisis , Polímeros/química , Contaminantes Químicos del Agua/análisis , Colorantes Fluorescentes/síntesis química , Indoles/síntesis química , Límite de Detección , Polímeros Impresos Molecularmente/síntesis química , Polímeros/síntesis química , Espectrometría de FluorescenciaRESUMEN
Phenolic compounds (like 4-nitrophenol) and dyes (like methyl orange) are common by-products discharged by many industries as wastes; they are toxic and may induce discomfort and irritation in humans when ingested. Most of these compounds can be made less toxic through catalytic degradation. Metal oxide nanoparticles are found to have high catalytic activity and can degrade toxic phenolic compounds and dyes. In the current study, pomegranate rind extract was used for the green synthesis of iron oxide nanoparticles that exhibited an octahedron morphology revealed by scanning electron microscopy analysis. Energy dispersive x-ray analysis showed 47.96% content of Fe (by weight); high resolution-transmission electron microscopy analysis confirmed that the nanoparticles had a particle size of 22.54 ± 4.13 nm. The particles were further characterized by x-ray diffraction, fourier transform-infrared spectroscopy, vibrating sample magnetometer, and thermogravimetric analysis. The nanoparticle proved to be efficient in reducing 4-nitrophenol and methyl orange. It was also found to be non-toxic towards murine macrophages, RAW 264.7 with good ROS-scavenging potential compared to control.
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Depuradores de Radicales Libres , Tecnología Química Verde/métodos , Nanopartículas de Magnetita , Extractos Vegetales , Granada (Fruta)/química , Animales , Supervivencia Celular/efectos de los fármacos , Colorantes , Depuradores de Radicales Libres/química , Depuradores de Radicales Libres/farmacología , Depuradores de Radicales Libres/toxicidad , Nanopartículas de Magnetita/química , Nanopartículas de Magnetita/toxicidad , Ratones , Nitrofenoles/análisis , Nitrofenoles/metabolismo , Extractos Vegetales/química , Extractos Vegetales/farmacología , Extractos Vegetales/toxicidad , Células RAW 264.7 , Especies Reactivas de Oxígeno/análisis , Especies Reactivas de Oxígeno/metabolismoRESUMEN
Soil degradation is a global issue that affects both plant productivity and human life. Intensive grazing practices can accelerate this process, mainly due to rapid removal of biomass from the soil surface. However, the long-term effects of grazing on biological, chemical, and physical properties remain poorly understood, particularly in tropical drylands, such as the Caatinga biome. Our aim was to evaluate the soil properties and combine both culture-dependent and -independent analyses to assess metabolic activity and bacterial community structure. We collected samples (0-20 cm) of three different types of soil in the Caatinga biome: secondary Caatinga forest (NC), grazing exclusion (GE), and degraded areas by overgrazing (OG). We sought to investigate how grazing affects soil properties to determine the effectiveness of grazing exclusion in the restoration of soil fertility/functions. Redundancy analysis demonstrated NC were positively correlated with organic carbon (λ = 0.18, p = 0.0012) and total nitrogen (λ = 0.16, p = 0.0011), while OG was correlated with harmful soil parameters such as Na+ (λ = 0.08, p = 0.0400), electric conductivity (λ = 0.13, p = 0.0060) and exchangeable acidity (λ = 0.11, p = 0.0030). In addition, GE showed lower aluminum content and saturation, reducing these harmful parameters by 48 % and 34 %, respectively. Also, GE showed the highest values for the ß-glucosidase (63.62 mg ρ-nitrophenol kg-1 h-1) and arylsulfatase (5.8 mg ρ-nitrophenol kg-1 h-1) activities. Changes in bacterial community structure were significant (p = 0.0096), with a higher difference comparing GE and OG (p = 0.0135). The GE area showed 20 % more phosphate solubilizers than OG, but there were no differences for siderophores production. All isolates were halotolerant and had at least 60 % nitrogen fixers. Our findings indicate that while soil recovery is slow, with grazing-exclusion areas presenting 18 years of implantation, it seems to improve in subsequent years. Finally, our results provide evidence that microbe-based technologies can mitigate soil degradation in the Caatinga biome.
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Ecosistema , Herbivoria , Suelo , Animales , Brasil , Microbiota/fisiología , Nitrofenoles/análisis , Suelo/química , Microbiología del SueloRESUMEN
The present study reports the development of an electrochemical sensor based on sulfobutylether-ß-cyclodextrin modified reduced graphene oxide hybrid (SBCD-rGO) for simultaneous detection of nitrophenol isomers. First, SBCD-rGO hybrid was synthesized and detailed characterized. Afterwards, a sensor was fabricated via the modification of glassy carbon electrode (GCE) with SBCD-rGO, and its electrochemical detection performances were also investigated. Then, the constructed electrochemical sensor was applied to detect nitrophenol isomers by voltammetry analysis. The results suggested that the sensitivities were 389.26, 280.88 and 217.19 µA/mM for p-nitrophenol (p-NP), m-nitrophenol (m-NP), and o-nitrophenol (o-NP), respectively, and their corresponding detection limits were all about 0.05 µM. Significantly, the combination of voltammetry analysis with the constructed sensor and data analysis by multiple linear regression realized the simultaneous detection of nitrophenol isomers.
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Técnicas Electroquímicas/métodos , Grafito/química , Nitrofenoles/análisis , beta-Ciclodextrinas/química , Carbono/química , Técnicas Electroquímicas/instrumentación , Electrodos , Isomerismo , Límite de Detección , Nanoestructuras/química , Nitrofenoles/química , Reproducibilidad de los ResultadosRESUMEN
Herein, we report the fabrication of a novel, well-defined core-double-shell-structured magnetic Fe3O4@polydopamine@naphthyl microporous organic network (MON), Fe3O4@PDA@NMON, for the efficient magnetic extraction of hydroxylated polycyclic aromatic hydrocarbons (OH-PAHs) and p-nitrophenol (p-Npn) from wastewater samples. The hierarchical nanospheres were designed and constructed with the Fe3O4 nanoparticle core, the inner shell of a polydopamine (PDA) layer, and the outer shell of a porous naphthyl MON (NMON) coating, allowing efficient and synergistic extraction of OH-PAHs and p-Npn via hydrophobic, hydrogen bonding, and π-π interactions. The Fe3O4@PDA@NMON nanospheres were well characterized and employed as an efficient sorbent for magnetic solid-phase extraction (MSPE) coupled with high performance liquid chromatography (HPLC) for analyzing of OH-PAHs and p-Npn. Under optimal conditions, the Fe3O4@PDA@NMON-based-MSPE-HPLC-UV method afforded wide linear range (0.18-500 µg L-1), low limits of detection (0.070 µg L-1 for p-Npn, 0.090 µg L-1 for 2-OH-Nap, 0.090 µg L-1 for 9-OH-Fluo and 0.055 µg L-1 for 9-OH-Phe, respectively), large enrichment factors (92.6-98.4), good precisions (intra-day and inter-day relative standard deviations (RSDs); <6.4%, n=6) and less consumption of the adsorbent. Furthermore, trace OH-PAHs and p-Npn with concentrations of 0.29-0.80 µg L-1 were successfully detected in various wastewater samples. Fe3O4@PDA@NMON also functioned as a good adsorbent to enrich a wide scope of trace contaminants containing hydrogen bonding sites and aromatic structures, highlighting the potential of functional MONs in sample pretreatment.
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Indoles/química , Nanosferas/química , Nitrofenoles/aislamiento & purificación , Hidrocarburos Policíclicos Aromáticos/aislamiento & purificación , Polímeros/química , Extracción en Fase Sólida/métodos , Aguas Residuales/química , Cromatografía Líquida de Alta Presión , Interacciones Hidrofóbicas e Hidrofílicas , Límite de Detección , Fenómenos Magnéticos , Nitrofenoles/análisis , Hidrocarburos Policíclicos Aromáticos/análisis , PorosidadRESUMEN
Nitrobenzene compounds are highly toxic pollutants with good stability, and they have a major negative impact on both human health and the ecological environment. Herein, it was found for the first time that fluorescent DNA-silver nanoclusters (DNA-AgNCs) can catalyze the reduction of toxic and harmful nitro compounds into less toxic amino compounds with excellent tolerance to high temperature and organic solvents. In this study, the reduction of p-nitrophenol (4-NP) as a model was systematically investigated, followed by expending the substrate to disclose the versatility of this reaction. This report not only expanded the conditions for utilizing catalytic reduction conditions of DNA-AgNCs as an efficient catalyst in the control of hazardous chemicals but also widened the substrate range of DNA-AgNCs reduction, providing a new angle for the application of noble metal nanoclusters.
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ADN/química , Nanopartículas del Metal/química , Nitrobencenos , Plata/química , Catálisis , Calor , Nitrobencenos/análisis , Nitrobencenos/química , Nitrobencenos/metabolismo , Nitrofenoles/análisis , Nitrofenoles/química , Nitrofenoles/metabolismoRESUMEN
In this study, surface imprinting, magnetic separation, and fluorescent detection were integrated to develop a dual-recognition sensor (MF-MIPs), which was used for highly selective and sensitive detection of 4-nitrophenol (4-NP) in food samples. Silane-functionalized carbon dots (Si-CDs) participated in the imprinting process and were uniformly distributed into the MIPs layers. MF-MIPs sensor exhibited a high fluorescence response and selectivity based on the dual-recognition mechanism of imprinting recognition and fluorescence identification. The relative fluorescence intensity of MF-MIPs sensor presented a good linear relationship in the range of 0.08-10 µmol·L-1 with a low limit of detection (23.45 nmol·L1) for 4NP. MF-MIPs sensor showed high anti-interference, as well as excellent stability and reusability. The 4-NP recovery from spiked food samples ranged from 93.20 to 102.15%, and the relative standard deviation was lower than 5.0%. Therefore, MF-MIPs sensor may be a promising method for 4-NP detection in food samples.
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Análisis de los Alimentos/métodos , Magnetismo , Impresión Molecular , Nitrofenoles/análisis , Carbono/química , Límite de Detección , Polímeros/química , Puntos Cuánticos/química , Reproducibilidad de los Resultados , Silanos/química , Espectrometría de FluorescenciaRESUMEN
It is challenging to develop highly stable lanthanide luminescent sensors for detecting heavy metal ions and nitroaromatics in view of the human health and environmental security. To this end, two water stable Ln-MOFs with the chemical constitution of {[Ln(HL)]·3DMF·3H2O}n (Ln = Eu, LZG-Eu and Ln = Tb, LZG-Tb) have been developed solvothermally using a multidentate ligand (H4L) with the central phenyl backbone bisubstituted by 2,6-pyridine-dicarboxylic acid at the para-position, H4L = 1,4-bis(2',2'',6',6''-tetracarboxy-1,4':4,4''-pyridyl)benzene. Single crystal analysis demonstrates that two novel Ln-MOFs feature 4,4,4-connected nets with an unprecedented topology symbol of {42·6·83}2{42·62·82}{42·84} and contain two kinds of one-dimensional channels. Powder X-ray diffraction as well as the luminescence determination results indicate that they retain their crystallinity and structural integrity in harsh acidic and basic conditions with pH in the range of 4-11. Moreover, they are highly luminescent, which makes them excellent chemical sensors for detecting Cu2+ and 4-NP (4-nitrophenol) with high selectivity and sensitivity in aqueous media such as deionized water, tap water, and river water based on distinct quenching effects. To the best of our knowledge, their detection limits are lower than those documented so far. In addition, the quenching efficiency of 4-NP was retained in the presence of interfering ions even after the compounds were used for five cycles, which makes them attractive, reliable, visual, and recyclable luminescent Ln-MOF sensor materials for 4-NP. The recognition mechanism for Cu2+ could be attributed to the dissociation of the main framework induced by Cu2+ and the subsequent formation of a Cu2+ coordination species and that for 4-NP is considered to be multi-quenching mechanisms dominated by competition absorption.
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Cobre/análisis , Elementos de la Serie de los Lantanoides/química , Sustancias Luminiscentes/química , Nitrofenoles/análisis , Agua/química , Ligandos , Modelos Moleculares , Conformación MolecularRESUMEN
Two chromatographic methods were validated for the determination of the widely prescribed analgesic and antipyretic drug combination of paracetamol (PC) (recently integrated into the supportive treatment of COVID-19), propyphenazone (PZ) and caffeine (CF) in the presence of two PC impurities, namely 4-aminophenol and 4-nitrophenol. A "dual-mode" gradient high-performance liquid chromatography method was developed, where the separation was achieved via "dual-mode" gradient by changing both the ternary mobile phase composition (acetonitrile: methanol: water) and the flow rate. This enables a good resolution within a relatively shorter analysis time. The analysis was realized using Zorbax Eclipse XDB column C18, 5 µm (250 × 4.6 mm) and the UV detector was set at 220 nm. The other method is a thin-layer chromatography densitometry method, where the separation was achieved using a mobile phase composed of chloroform: toluene: ethyl acetate: methanol: acetic acid (6: 6: 1: 2: 0.1, by volume). Densitometric detection was performed at 220 nm on silica gel 60 F254 plates. The developed methods were fully validated as per the ICH guidelines and proved to be accurate, robust, specific and suitable for application as purity indicating methods for routine analysis of PC in pure form or in pharmaceuticals with PZ and CF in quality control laboratories.
Asunto(s)
Acetaminofén/análisis , Antipirina/análogos & derivados , Cafeína/análisis , Cromatografía Líquida de Alta Presión/métodos , Cromatografía en Capa Delgada/métodos , Aminofenoles/análisis , Antipirina/análisis , Codeína/análisis , Densitometría/métodos , Combinación de Medicamentos , Contaminación de Medicamentos , Límite de Detección , Meprobamato/análisis , Nitrofenoles/análisis , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Solventes/química , Comprimidos/análisisRESUMEN
The important role of reactive chlorine species (RCS) in electrochemical system has been widely concerned for water disinfection recently. In this study, we built an electrochemical system using carbon nanotube as cathode and oxide precursor (Ti/SnO2-Sb2O5-IrO2) as anode, where RCS was produced from Cl-. This system was used to degrade nitrogen contaminants, i.e. NO3- and 4-nitrophenol. Optimization of the reaction conditions was carried out by a treatment of inorganic nitrogen contaminant NO3- and the optimal condition of the electrochemical system was determined at U = 5.5 V, and pH = 10 with a Cl- concentration of 2000 mg L-1, and the removal efficiency of NO3- can reach up to 60.6% in 150 min. Under the optimal condition, a common nitrogenous organic pollutant, 4-nitrophenol was treated and a removal efficiency of nearly 100% in 90 min. To investigate the detailed degradation mechanism in the applied electrochemical system, a combined method of products identification and density functional theory (DFT) calculation was employed. It concluded that Cl radicals' generation was stimulated was stimulated by the OH radicals after adding Cl- into the electrochemical system. These two radicals jointly promoted the transformation of 4-nitrophenol resulting in the formation of more toxic organic and inorganic substances. In addition, a conversion of organic nitro group to amino group leading to the formation of 4-aminophenol was found and explained by the indirect reduction theory.
Asunto(s)
Cloro/química , Técnicas Electroquímicas/métodos , Modelos Teóricos , Nitrofenoles/análisis , Contaminantes Químicos del Agua/análisis , Purificación del Agua/métodos , Catálisis , Electrodos , Nitratos/análisis , Oxidación-ReducciónRESUMEN
Carbon dots (CDs) have excellent application prospects in various fields such as fluorescent dyes, but expanding their application, especially in bioimaging and the detection of organic pollutants, is still a major research objective. In this study, fluorescent CDs were successfully synthesized via the hydrothermal method using Serratia marcescens KMR-3. The platform based on CDs-KMR3 exhibited excellent stability, good biocompatibility, and low biotoxicity, and can be effectively applied to the imaging of bacteria, fungi, plant cells, protozoa and mammalian cells, and can specifically stain the membranes of all tested cells. In this study, for the first time, bacteria-derived CDs were used to image the representative species of organisms ranging from lower-order to higher-order organisms, thereby proving the feasibility of the application of CDs in the fluorescence imaging of Paramecium caudatum. Additionally, CDs-KMR3 can rapidly diffuse into all the parts of the leaf through diffusion into the veins and intercellular interstitium in response to the induction of transpiration. Moreover, the data illustrate that CDs-KMR3 are likely to enter the digestive tracts of microworms by ingestion through the oral cavity and pharynx, and spread to the pseudocoelom and somatic cells, and finally to be excreted from microworms through the anus. Furthermore, this platform can be utilized as fluorescent probes for the rapid and highly selective detection of p-nitrophenol (p-NP). Moreover, this study contributed to the increased application of bacteria-derived CDs in bioimaging and detection of p-NP.
Asunto(s)
Carbono/química , Colorantes Fluorescentes/química , Imagen Molecular/métodos , Nanopartículas/química , Nitrofenoles/análisis , Imagen Óptica/métodos , Serratia marcescens/química , Células HeLa , Humanos , Límite de Detección , Nitrofenoles/química , Nitrofenoles/metabolismoRESUMEN
This investigation implemented the nanomaterial rGOTiO2 for photodegradation of 2-nitrophenol solution at high concentrations. The 2-nitrophenol photodegradation was carried out in the presence of three kinds of light sources in the visible range spectrum. The results demonstrate that the nanomaterial rGOTiO2 is capable of pollutant degradation even in the low power light source (10 W), and have high activity under sunlight. The degradation of 2-nitrophenol was monitored by UV-vis spectroscopy, adjusting method by least squares for nonlinear functions. The equation represents the material photocatalytic activity under sunlight, which excludes climatic and variance factors. This equation predicts the pure rGOTiO2 behavior under sunlight; this will enable future research to develop more advanced processes.