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1.
Chemosphere ; 359: 142297, 2024 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-38729443

RESUMO

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.


Assuntos
Hidrazonas , Nitrofenóis , Poluentes Químicos da Água , Nitrofenóis/análise , Nitrofenóis/química , Hidrazonas/química , Poluentes Químicos da Água/análise , Cisteína/análise , Cisteína/química , Limite de Detecção , Corantes Fluorescentes/química , Estruturas Metalorgânicas/química , Papel , Fluorescência , Monitoramento Ambiental/métodos , Espectrometria de Fluorescência , Rios/química
2.
J Dairy Sci ; 107(1): 288-300, 2024 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-38353472

RESUMO

A systematic literature review of in vitro studies was performed to identify methane (CH4) mitigation interventions with a potential to reduce CH4 emission in vivo. Data from 277 peer-reviewed studies published between 1979 and 2018 were reviewed. Individual CH4 mitigation interventions were classified into 14 categories of feed additives based on their type, chemical composition, and mode of action. Response variables evaluated were absolute CH4 emission (number of treatment means comparisons = 1,325); total volatile fatty acids (n = 1,007), acetate (n = 783), propionate (n = 792), and butyrate (n = 776) concentrations; acetate to propionate ratio (n = 675); digestibility of dry matter (n = 489), organic matter (n = 277), and neutral detergent fiber (n = 177). Total gas production was used as an explanatory variable in the model for CH4 production. Relative mean difference between treatment and control means reported in the studies was calculated and used for statistical analysis. The robust variance estimation method was used to analyze the effects of CH4 mitigation interventions. In vitro CH4 production was decreased by antibodies (-38.9%), chemical inhibitors (-29.2%), electron sinks (-18.9%), essential oils (-18.2%), plant extracts (-14.5%), plant inclusion (-11.7%), saponins (-14.8%), and tannins (-14.5%). Overall effects of direct-fed microbials, enzymes, macroalgae, and organic acids supplementation did not affect CH4 production in the current meta-analysis. When considering the effects of individual mitigation interventions containing a minimum number of 4 degrees of freedom within feed additives categories, Enterococcus spp. (i.e., direct-fed microbial), nitrophenol (i.e., electron sink), and Leucaena spp. (i.e., tannins) decreased CH4 production by 20.3%, 27.1%, and 23.5%, respectively, without extensively, or only slightly, affecting ruminal fermentation and digestibility of nutrients. It should be noted, however, that although the total number of publications (n = 277) and treatment means comparisons (n = 1,325 for CH4 production) in the current analysis were high, data for most mitigation interventions were obtained from less than 5 observations (e.g., maximum number of observations was 4, 7, and 22 for nitrophenol, Enterococcus spp., and Leucaena spp., respectively), because of limited data available in the literature. These should be further evaluated in vitro and in vivo to determine their true potential to decrease enteric CH4 production, yield, and intensity. Some mitigation interventions (e.g., magnesium, Heracleum spp., nitroglycerin, ß-cyclodextrin, Leptospermum pattersoni, Fructulus Ligustri, Salix caprea, and Sesbania grandiflora) decreased in vitro CH4 production by over 50% but did not have enough observations in the database. These should be more extensively investigated in vitro, and the dose effect must be considered before adoption of mitigation interventions in vivo.


Assuntos
Dieta , Leite , Feminino , Animais , Dieta/veterinária , Leite/química , Lactação , Propionatos/metabolismo , Metano/metabolismo , Taninos/farmacologia , Rúmen/metabolismo , Acetatos/análise , Nitrofenóis/análise , Nitrofenóis/metabolismo , Nitrofenóis/farmacologia , Fermentação , Digestão , Ração Animal/análise
3.
Chemosphere ; 331: 138813, 2023 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-37127202

RESUMO

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.


Assuntos
Grafite , Poluentes da Água , Humanos , Celulose , Poluentes da Água/análise , Nitrofenóis/análise , Grafite/química , Eletrodos , Técnicas Eletroquímicas/métodos
4.
Biomed Chromatogr ; 36(10): e5444, 2022 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-35792558

RESUMO

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.


Assuntos
Resíduos de Praguicidas , Ziziphus , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida/métodos , Nitrofenóis/análise , Resíduos de Praguicidas/análise , Sódio/análise , Espectrometria de Massas em Tandem/métodos
5.
Mikrochim Acta ; 189(1): 25, 2021 12 11.
Artigo em Inglês | MEDLINE | ID: mdl-34897555

RESUMO

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..


Assuntos
Água Potável/análise , Corantes Fluorescentes/química , Indóis/química , Polímeros Molecularmente Impressos/química , Nitrofenóis/análise , Polímeros/química , Poluentes Químicos da Água/análise , Corantes Fluorescentes/síntese química , Indóis/síntese química , Limite de Detecção , Polímeros Molecularmente Impressos/síntese química , Polímeros/síntese química , Espectrometria de Fluorescência
6.
Microbiol Res ; 253: 126893, 2021 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-34678684

RESUMO

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.


Assuntos
Ecossistema , Herbivoria , Solo , Animais , Brasil , Microbiota/fisiologia , Nitrofenóis/análise , Solo/química , Microbiologia do Solo
7.
Nanotechnology ; 33(4)2021 Nov 05.
Artigo em Inglês | MEDLINE | ID: mdl-34598165

RESUMO

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.


Assuntos
Sequestradores de Radicais Livres , Química Verde/métodos , Nanopartículas de Magnetita , Extratos Vegetais , Punica granatum/química , Animais , Sobrevivência Celular/efeitos dos fármacos , Corantes , Sequestradores de Radicais Livres/química , Sequestradores de Radicais Livres/farmacologia , Sequestradores de Radicais Livres/toxicidade , Nanopartículas de Magnetita/química , Nanopartículas de Magnetita/toxicidade , Camundongos , Nitrofenóis/análise , Nitrofenóis/metabolismo , Extratos Vegetais/química , Extratos Vegetais/farmacologia , Extratos Vegetais/toxicidade , Células RAW 264.7 , Espécies Reativas de Oxigênio/análise , Espécies Reativas de Oxigênio/metabolismo
8.
Carbohydr Polym ; 271: 118446, 2021 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-34364581

RESUMO

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.


Assuntos
Técnicas Eletroquímicas/métodos , Grafite/química , Nitrofenóis/análise , beta-Ciclodextrinas/química , Carbono/química , Técnicas Eletroquímicas/instrumentação , Eletrodos , Isomerismo , Limite de Detecção , Nanoestruturas/química , Nitrofenóis/química , Reprodutibilidade dos Testes
9.
J Chromatogr A ; 1651: 462347, 2021 Aug 16.
Artigo em Inglês | MEDLINE | ID: mdl-34166861

RESUMO

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.


Assuntos
Indóis/química , Nanosferas/química , Nitrofenóis/isolamento & purificação , Hidrocarbonetos Policíclicos Aromáticos/isolamento & purificação , Polímeros/química , Extração em Fase Sólida/métodos , Águas Residuárias/química , Cromatografia Líquida de Alta Pressão , Interações Hidrofóbicas e Hidrofílicas , Limite de Detecção , Fenômenos Magnéticos , Nitrofenóis/análise , Hidrocarbonetos Policíclicos Aromáticos/análise , Porosidade
10.
Nanotechnology ; 32(19): 195705, 2021 May 07.
Artigo em Inglês | MEDLINE | ID: mdl-33545692

RESUMO

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.


Assuntos
DNA/química , Nanopartículas Metálicas/química , Nitrobenzenos , Prata/química , Catálise , Temperatura Alta , Nitrobenzenos/análise , Nitrobenzenos/química , Nitrobenzenos/metabolismo , Nitrofenóis/análise , Nitrofenóis/química , Nitrofenóis/metabolismo
11.
Dalton Trans ; 50(5): 1874-1886, 2021 Feb 09.
Artigo em Inglês | MEDLINE | ID: mdl-33475098

RESUMO

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.


Assuntos
Cobre/análise , Elementos da Série dos Lantanídeos/química , Substâncias Luminescentes/química , Nitrofenóis/análise , Água/química , Ligantes , Modelos Moleculares , Conformação Molecular
12.
Food Chem ; 348: 129126, 2021 Jun 30.
Artigo em Inglês | MEDLINE | ID: mdl-33515947

RESUMO

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.


Assuntos
Análise de Alimentos/métodos , Magnetismo , Impressão Molecular , Nitrofenóis/análise , Carbono/química , Limite de Detecção , Polímeros/química , Pontos Quânticos/química , Reprodutibilidade dos Testes , Silanos/química , Espectrometria de Fluorescência
13.
Analyst ; 146(2): 683-690, 2021 Jan 21.
Artigo em Inglês | MEDLINE | ID: mdl-33210668

RESUMO

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.


Assuntos
Carbono/química , Corantes Fluorescentes/química , Imagem Molecular/métodos , Nanopartículas/química , Nitrofenóis/análise , Imagem Óptica/métodos , Serratia marcescens/química , Células HeLa , Humanos , Limite de Detecção , Nitrofenóis/química , Nitrofenóis/metabolismo
14.
J Chromatogr Sci ; 59(2): 140-147, 2021 Jan 14.
Artigo em Inglês | MEDLINE | ID: mdl-33221830

RESUMO

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.


Assuntos
Acetaminofen/análise , Antipirina/análogos & derivados , Cafeína/análise , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia em Camada Fina/métodos , Aminofenóis/análise , Antipirina/análise , Codeína/análise , Densitometria/métodos , Combinação de Medicamentos , Contaminação de Medicamentos , Limite de Detecção , Meprobamato/análise , Nitrofenóis/análise , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Solventes/química , Comprimidos/análise
15.
Chemosphere ; 262: 128015, 2021 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-33182116

RESUMO

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.


Assuntos
Cloro/química , Técnicas Eletroquímicas/métodos , Modelos Teóricos , Nitrofenóis/análise , Poluentes Químicos da Água/análise , Purificação da Água/métodos , Catálise , Eletrodos , Nitratos/análise , Oxirredução
16.
Artigo em Inglês | MEDLINE | ID: mdl-33119463

RESUMO

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.


Assuntos
Grafite/química , Luz , Modelos Teóricos , Nanoestruturas/química , Nitrofenóis/análise , Titânio/química , Poluentes Químicos da Água/análise , Catálise , Nitrofenóis/efeitos da radiação , Fotólise , Poluentes Químicos da Água/efeitos da radiação
17.
Chemosphere ; 254: 126899, 2020 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-32957294

RESUMO

In this study, the reduction of iron-carbon internal electrolysis was reinforced by persulfate for p-nitrophenol removal. The effects of persulfate dosage, initial pH and iron-carbon mass ratio were comprehensively studied in batch experiments. In the system of iron-carbon internal electrolysis coupled with persulfate, the iron-carbon internal electrolysis and persulfate had a significant mutual influence, exhibiting a wide range of pH in the treatment process. Moreover, the coupled system also showed the remarkable removal and degradation efficiency of p-nitrophenol according to the contrast experiments. The satisfactory results should be attributed to the potential reduction of iron-carbon internal electrolysis, which was stimulated by persulfate to transform the nitro group to the amine group, accompanying the subsequent oxidation. Furthermore, persulfate possessed the ability that the dynamically destructive effect on external and internal of Fe0 and the scavenging action on activated carbon, effectively strengthening the potential energy for release and transfer of reductive substances. Both HO• and SO4•- as the main free radicals were formed to mineralize the intermediates in the coupled system. These findings indicate that the system of iron-carbon internal electrolysis coupled with persulfate can be a promising strategy for the treatment of the toxic and refractory wastewater.


Assuntos
Carvão Vegetal/química , Eletrólise/métodos , Ferro/química , Nitrofenóis/análise , Sulfatos/química , Poluentes Químicos da Água/análise , Purificação da Água/métodos , Modelos Teóricos , Nitrofenóis/química , Oxirredução , Águas Residuárias/química , Poluentes Químicos da Água/química
18.
Molecules ; 25(17)2020 Aug 26.
Artigo em Inglês | MEDLINE | ID: mdl-32859012

RESUMO

Analysis of 4-cyanophenol and 3-nitrophenol was carried out using multi-walled carbon nanotubes-based solid-phase extraction (SPE) and capillary electrophoresis (CE) methods. Capillary electrophoresis was carried out with 18 kV voltage, 214 nm detection, and phosphate buffer (pH 7.0, 15 mM) as background electrolyte at 25 ± 1 °C temperature with 15.05 and 16.5 min migration times of 4-cyanophenol and 3-nitrophenol. The separation and resolution factors were 1.10 and 2.90. The optimized experimental conditions were 40 mg/L concentration, 1.0 g multi-walled carbon nanotubes (MWCNTs) per SPE cartridge, 5.0 mL/min flow rate of water, 0.1 mL flow rate of eluting solvent. The maximum recoveries were 91% and 98% at 0.1 mL/min flow rate of 4-cyanophenol and 3-nitrophenol. These methods were applied successfully for extraction and estimation of 4-cyanophenol and 3-nitrophenol in the municipal wastewater. The reported methods are reproducible, efficient, and practical for the estimation of these phenols in water.


Assuntos
Nanotubos de Carbono/química , Nitrofenóis/análise , Fenóis/análise , Água/química , Eletroforese Capilar , Extração em Fase Sólida
19.
Ecotoxicol Environ Saf ; 201: 110862, 2020 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-32559691

RESUMO

In this study, a novel electrochemical sensor based on self-assembled rod-like lanthanum hydroxide-oxidized multi-walled carbon nanotubes (La(OH)3-OxMWCNTs) nanocomposite was developed for sensitive determination of p-nitrophenol (p-NP). The La(OH)3-OxMWCNTs nanocomposite with an interpenetrating networks structure was characterized by field emission electron microscope (FE-SEM), Fourier transform infrared (FT-IR) spectroscopy, Raman spectra and X-ray photoelectron spectroscopy (XPS). The cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) measurements were performed to study the electrochemical behaviors of La(OH)3-OxMWCNTs modified glassy carbon electrode (La(OH)3-OxMWCNTs/GCE). The La(OH)3-OxMWCNTs/GCE was used for sensitive determination of p-NP by CV and linear sweep voltammetry (LSV). Under the optimum conditions, the peak currents of LSV versus the concentrations of p-NP in the range 1.0-30.0 µmol L-1 showed a good linear relationship (R2=0.9971), and the limit of detection (LOD) was calculated to be 0.27 µmol L-1 (signal-to-noise ratio of 3, S/N=3). The recoveries of p-NP in real samples of industrial wastewater and Xiangjiang water at La(OH)3-OxMWCNTs/GCE were in the range of 95.62-110.75% with relative standard deviation (RSD) in the range of 1.65-3.85%. The intra-day and inter-day precisions were estimated to be less than 2.76% (n= 5), indicating that La(OH)3-OxMWCNTs/GCE possessed highly stability. In addition, La(OH)3-OxMWCNTs/GCE sensor showed good anti-interference ability for determination of p-NP in aqueous mixtures containing high concentrations of inorganic and organic interferents, and a decrease of oxidation peak currents by less than 3.57% relative to the initial levels indicated it possessed excellent selectivity. Therefore, La(OH)3-OxMWCNTs/GCE could be used as a fast, selective and sensitive electrochemical sensor platform for the selective determination and quantification of aqueous p-NP.


Assuntos
Técnicas Eletroquímicas/métodos , Lantânio/química , Nanocompostos/química , Nanotubos de Carbono/química , Nitrofenóis/análise , Eletrodos , Limite de Detecção , Oxirredução
20.
Talanta ; 211: 120742, 2020 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-32070560

RESUMO

A novel fluorescent Zn(II)-based metal-organic framework (Zn-MOF), [Zn2(oba)4(4,4'-bpy)2]n, was successfully synthesized through a simple solvothermal route at 130 °C for 48 h, employing Zn(NO3)2·6H2O, 4,4'-Oxybis(benzoic acid) (oba) and 4,4'-Bipyridine (4,4'-bpy) as the initial reactants, dimethylacetamide (DMA) as the reaction medium. The as-obtained Zn-MOF was characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectrum (FTIR), Thermogravimetric analysis (TGA) and elemental analysis. The fluorescence tests showed that the as-obtained Zn-MOF emit a strong violet light centered at 445 nm under the excitation of 323 nm UV light. Intriguingly, the above strong violet emission could be highly selectively quenched by aromatic nitrophenols or antibiotic metronidazole (MET) in aqueous systems with fairly low detection limits. Other substituted phenols and antibiotics, as well as some cations, anions, amino acids and small organic molecules hardly affected the violet emission of the as-obtained Zn-MOF, indicating that this novel Zn-MOF could be prepared as a selective fluorescent probe for detections of aromatic nitrophenols and MET antibiotic in water solutions.


Assuntos
Antibacterianos/análise , Corantes Fluorescentes/química , Estruturas Metalorgânicas/química , Metronidazol/análise , Nitrofenóis/análise , Poluentes Químicos da Água/análise , Zinco/química , Fluorescência , Compostos Heterocíclicos/análise , Limite de Detecção
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