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Heterocyclic aromatic hydrocarbons are concerned pollutants with carcinogenic toxicity, which exist universally in various environmental matrices and have great harm to environmental and human health. In present work, magnetic resorcinol-formaldehyde composites (Fe3O4@SiO2@R-F) were fabricated via aldol condensation reaction under alkaline condition. The prepared magnetic materials were examined and analyzed with Fourier transform infrared spectroscopy and other related instruments. The Fe3O4@SiO2@R-F composites were utilized to develop an efficient magnetic solid phase extraction (MSPE) method for extracting six heteropolyclic aromatic hydrocarbons from environmental water samples including carbazole (CB), 7-methylquinoline (7-MQL), 9-methylcarbazole (9-MCB), dibenzothiophene (DBT), 4-methyldibenzothiophene (4-MDBT), and 4,6-dimethyldibenzothiophene (4,6-DMDBT). The analytes were analyzed by high performance liquid chromatography-ultraviolet variable wavelength detector (HPLC-VWD). The main factors affecting MSPE were optimized. With the optimal parameters, 9-MCB and 4-MDBT have good linearity over the concentration range of 0.1-300 µg L-1, and 7-MQL, CB, DBT and 4,6-DMDBT have good linearity over the concentration range of 0.5-300 µg L-1. The limits of detection were over the concentration range of 0.012-0.031 µg L-1. This method was successfully employed to measure real waters, and the spiked recoveries ranged from 89.4% to 99.9%. The results confirmed that the developed method was reliable, robust and could be employed as a usefully alternate way for analyzing such pollutants in waters.
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Antibiotics are widely used in clinical medicine due to their excellent antibacterial abilities. As typical emerging pollutants, their misuse can lead to excess antibiotics entering the environment, causing antimicrobial resistance and leading to serious health problems via food chain. Herein, a nano-fluorescent probe based on nitrogen-doped carbon dots (N-CDs) was constructed for the sensitive detection of chlortetracycline (CTC). N-CDs with stable fluorescence were synthesized by hydrothermal method using alizarin red and melamine as raw materials. The N-CDs exhibited significant independence to excitation wavelength. The fluorescence of N-CDs was significantly quenched by CTC ascribing to the fluorescence resonance energy transfer mechanism. The concentration of N-CDs, solution pH and incubation time were optimized to obtain the optimal detection parameters. Under optimal conditions, CTC exhibited excellent linearity over the range of 20-1200 µg/L, and the detection limit was 8.74 µg/L. The method was validated with actual water samples and achieved satisfied spiked recoveries of 97.6-102.6%. Therefore, the proposed method has significant application value in the detection of CTC in waters.
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Antibacterianos , Carbono , Clortetraciclina , Corantes Fluorescentes , Limite de Detecção , Nitrogênio , Pontos Quânticos , Poluentes Químicos da Água , Clortetraciclina/análise , Nitrogênio/química , Nitrogênio/análise , Carbono/química , Corantes Fluorescentes/química , Poluentes Químicos da Água/análise , Pontos Quânticos/química , Antibacterianos/análise , Transferência Ressonante de Energia de Fluorescência , FluorescênciaRESUMO
In this study, a novel COFTABT@COFTATp modified magnetic MXene composite (CoFe2O4 @Ti3C2 @COFTABT@COFTATp) was synthesized by Schiff base reaction and irre-versible enol-keto tautomerization, and employed to establish a sensitive monitoring method for six thiophene compounds in oilfield produced water samples based on magnetic solid-phase extraction (MSPE) prior to gas chromatography coupled with a triple quadruple mass spectrometer (GC-MS/MS). The designed magnetic materials exhibited unexpected enrichment ability to target thiophene compounds and achieved good extraction efficiencies ranging from 83 % to 98 %. The developed MSPE/GC-MS/MS method exhibited good linearity in the range of 0.001-100 µg L-1, and obtained lower limits of detection ranging from 0.39 to 1.9 ng L-1. The spiked recoveries of thiophene compounds obtained in three oilfield produced water samples were over the range of 96.26 %-99.54 % with relative standard deviations (RSDs) less than 3.7 %. Notably, benzothiophene, 4-methyldibenzothiophene and 4,6-dimethyldibenzothiophene were detected in three oilfield-produced water samples. Furthermore, the material still kept favorable stability after six recycling experiments. The adsorption kinetics, adsorption isotherms as well as adsorption thermodynamics of thiophene compounds were investigated in detail to provide insight into the mechanisms. Overall, the present work contributed a promising strategy for designing and synthesizing new functionalized materials for the enrichment and detection of typical pollutants in the environment.
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As a typical kind of new pollutants, there are still some challenges in the rapid detection of antibiotics. In this work, a sensitive fluorescent probe based on boron-doped carbon dots (B-CDs) in combination with thermo-responsive magnetic molecularly imprinted polymers (T-MMIPs) was constructed for the detection of oxytetracycline (OTC) in tea drinks. T-MMIPs were designed, fabricated and employed to enrich OTC at trace level from tea drinks, and B-CDs were utilized as the fluorescent probe to detect the concentration of OTC. The proposed method exhibited good linear relationship with OTC concentration from 0.2 to 60 µg L-1 and the limit of detection was 0.1 µg L-1. The established method has been successfully validated with tea beverages. Present work was the first attempt application of T-MMIPs in combination with CDs in detection of OTC, and demonstrated that the proposed method endowed the detection of OTC with high selectivity, sensitivity, reliability and wide application prospect, meanwhile offered a new strategy for the method establishment of rapid and sensitive detection of trace antibiotics in food and other matrices.
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Impressão Molecular , Oxitetraciclina , Oxitetraciclina/análise , Boro , Impressão Molecular/métodos , Carbono , Corantes Fluorescentes , Reprodutibilidade dos Testes , Polímeros , Antibacterianos , Extração em Fase Sólida/métodos , Chá , Fenômenos Magnéticos , Limite de DetecçãoRESUMO
Present work reported a novel nanozyme g-C3N4@Cu, N-CDs with excellent peroxidase-like activity obtained by loading Cu and N co-doped carbon dots on g-C3N4 (graphitic carbon nitride). g-C3N4@Cu, N-CDs can catalyze H2O2 to generate hydroxyl radical â¢OH, which oxidizes o-phenylenediamine to 2,3-diaminophenazine, which emits orange fluorescence under ultraviolet light irradiation. The experimental results confirmed that 1,4-benzenedithiol (BDT) could inhibit the peroxidase-like activity of g-C3N4@Cu, N-CDs. Based the principle above, a colorimetric-fluorescence dual-mode sensor for rapidly sensing of BDT was creatively constructed with assisting of a smartphone. The sensor showed excellent linearity over ranges of 0.75-132 µM and 0.33-60.0 µM with detection limits of 0.32 µM and 0.25 µM for colorimetric and fluorescence detection, respectively. Moreover, a smartphone-assisted colorimetric array sensor was constructed to distinguish six sulfur-containing compounds according to the difference in the degree of inhibition of nanozyme activity by different sulfur-containing compounds. The array sensor could distinguish sulfur-containing compounds at low concentration as low as 0.4 µM. The results validated that the designed sensor was a convenient and fast platform, which could be utilized as a reliably portable tool for the efficient and accurate detection of BDT and the discrimination of multiple sulfur compounds in real water samples.
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Colorimetria , Cobre , Smartphone , Sulfetos , Colorimetria/métodos , Cobre/química , Sulfetos/química , Compostos de Cádmio/química , Poluentes Químicos da Água/análise , Peroxidase/química , Peroxidase/metabolismo , Fluorescência , Compostos de Enxofre/análise , Compostos de Enxofre/química , Limite de Detecção , Espectrometria de Fluorescência/métodos , Compostos de Sulfidrila/química , Compostos de Sulfidrila/análise , Carbono/química , Peróxido de Hidrogênio/química , Peróxido de Hidrogênio/análise , Grafite , Compostos de NitrogênioRESUMO
In this study, a hydrophobic covalent organic framework-functionalized magnetic composite (CoFe2O4@Ti3C2@TAPB-TFTA) with a high specific area with 1,3,5-tris(4-aminophenyl)benzene (TAPB) and 2,3,5,6-tetrafluoroterephthalaldehyde (TFTA) was designed and synthesized through Schiff base reaction. An efficient magnetic solid-phase extraction method was established and combined with gas chromatography-triple quadrupole mass spectrometry to sensitively determine 10 organochlorine and organophosphorus pesticides in tea samples. The established method exhibited good linearity in the range of 0.05-120 µg/L and had low limits of detection (0.013-0.018 µg/L). The method was evaluated with tea samples, and the spiked recoveries of pesticides in different tea samples reached satisfactory values of 85.7-96.8%. Moreover, the adsorption of pesticides was spontaneous and followed Redlich-Peterson isotherm and pseudo-second-order kinetic models. These results demonstrate the sensitivity, effectiveness, and reliability of the proposed method for monitoring organochlorine and organophosphorus pesticides in tea samples, providing a preliminary basis for researchers to reasonably design adsorbents for the efficient extraction of pesticides.
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Contaminação de Alimentos , Cromatografia Gasosa-Espectrometria de Massas , Hidrocarbonetos Clorados , Estruturas Metalorgânicas , Nanocompostos , Compostos Organofosforados , Praguicidas , Extração em Fase Sólida , Chá , Chá/química , Compostos Organofosforados/química , Compostos Organofosforados/análise , Hidrocarbonetos Clorados/química , Hidrocarbonetos Clorados/análise , Contaminação de Alimentos/análise , Nanocompostos/química , Estruturas Metalorgânicas/química , Extração em Fase Sólida/métodos , Praguicidas/química , Praguicidas/análise , Adsorção , Limite de Detecção , Resíduos de Praguicidas/química , Resíduos de Praguicidas/análise , Resíduos de Praguicidas/isolamento & purificaçãoRESUMO
Polycyclic aromatic hydrocarbons (PAHs) are commonly found in various environmental matrices and have received significant attention due to their toxic effects on ecosystems and environmental health. In this study, a specific magnetic composite material derived from MXene, known as phenyl-functionalized NiFe2O4@Ti3C2TX, was designed and synthesized using a simple method. This composite material was used to develop an effective magnetic solid-phase extraction (MSPE) method for enriching trace polycyclic aromatic hydrocarbons (PAHs) in tea and coffee samples. The eluted PAHs were analyzed via gas chromatography-tandem mass spectrometry. Under optimal conditions, this method exhibited excellent linear relationships for 16 PAHs within the ranges of 0.001-25 and 0.0005-25 µg/L, with correlation coefficients exceeding 0.9979. The limits of detection for the target PAHs ranged from 0.1 to 0.3 ng/L. The effectiveness of the proposed method was evaluated by analyzing tea and coffee samples, and the satisfactory spiked recoveries of PAHs ranged from 84.5% to 112.6%.
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Café , Contaminação de Alimentos , Hidrocarbonetos Policíclicos Aromáticos , Extração em Fase Sólida , Chá , Chá/química , Hidrocarbonetos Policíclicos Aromáticos/análise , Hidrocarbonetos Policíclicos Aromáticos/isolamento & purificação , Hidrocarbonetos Policíclicos Aromáticos/química , Café/química , Extração em Fase Sólida/métodos , Contaminação de Alimentos/análise , Níquel/química , Níquel/análise , Níquel/isolamento & purificação , Compostos Férricos/química , Cromatografia Gasosa-Espectrometria de Massas , Limite de DetecçãoRESUMO
The residual carbaryl in crops can cause serious damage to the human kidney and nervous system after entering the human body, which may be metabolized to 1-naphthol (1-NAP) and excreted through urine. 1-NAP is often used as the biomarker for carbaryl exposure, so the intake or leakage of carbaryl can be monitored by detecting the concentration of 1-NAP. Herein, Co, N, P ternary co-doped carbon dots (CoNP-CDs) derived from vitamin B12 were synthesized by a facile hydrothermal method. CoNP-CDs exhibited oxidase-like activity and excellent peroxidase-like activity, which was attributed to the Fenton-like reaction of Co2+/Co3+ and the presence of pyrrole N and P elements, which together provided multiple active sites for chromogenic substrates. Due to the dual enzyme-like activity of CoNP-CDs, hydroxyl radicals (OH) and superoxide radicals (O2-) were generated during the catalytic process, which could rapidly oxidize colorless 3,3',5,5'-tetramethyl benzidine (TMB) to blue oxidation products (oxTMB). The α-carbon in 1-NAP can be attacked by OH, and the catalytic oxidation process of TMB can be inhibited by the consumption of OH, so that the blue color of the solution became lighter. Based on this principle, a smartphone-assisted colorimetric sensing platform was constructed for the detection of 1-NAP, and which resulted in a linear range of 1.07-37.3 µM and a visual detection limit of 0.68 µM. Moreover, the colorimetric sensing system showed satisfactory recoveries in the detection of human urine samples. The colorimetric sensing system owned the advantages of fast response, strong selectivity and simple operation, and provided a potential strategy for the on-site detection of 1-NAP.
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In this study, nitrogen-doped carbon dots (N-CDs) were facilely fabricated by one-pot hydrothermal method with levulinic acid and triethanolamine. A fluorescent sensor array was established for identifying azo compounds including Sudan Orange G (SOG), p-diaminoazobenzene, p-aminoazobenzene, azobenzene and quantitative detection of SOG. Experimental results revealed that azo compounds could quench the fluorescent intensity of N-CDs. Owing to various azo compounds showing different affinities to N-CDs, the sensor array exhibited different fluorescence quenching changes, which were further analyzed with principal component analysis to discriminate azo compounds. The sensor array was able to differentiate and recognize diverse concentrations of azo compounds from 0.25 to 2 mg/L. Simultaneously, a variety of factors affecting the detection of SOG were optimized. Under the optimized conditions, the sensor showed excellent stability and sensitivity. The sensor possessed marvelous linearity in the range of 0.1-1 mg/L and 1-4 mg/L and the detection limit was 27.82 µg/L. Spiked recoveries of 90.8-98.2 % were attained at spiked levels of 0.2 mg/L and 1 mg/L, demonstrating that the constructed fluorescence sensor was dependable and feasible for sensing SOG in environmental water samples.
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Doxycycline (DOX), a typical tetracycline antibiotic, is widely used because of its excellent antibacterial activity. To develop effective method for DOX has attracted much more attention. Herein, a new detection technology integrating magnetic solid phase extraction (MSPE) based on thermosensitive magnetic molecularly imprinted polymers (T-MMIPs) and fluorescence spectrometry based on carbon dots (CDs) was established. Thermosensitive magnetic molecularly imprinted polymers (T-MMIPs) was designed for selective enrichment of trace DOX. The synthesized T-MMIPs showed excellent selectivity for DOX. The adsorption performance of T-MMIPs varied with temperature in different solvents, which could achieve the enrichment and rapid desorption of DOX. In addition, the synthesized CDs had stable fluorescent property and better water-solubility, and the fluorescence of CDs was significantly quenched by DOX due to the internal filtration effect (IFE). Under the optimized conditions, the method resulted in good linearity over the range from 0.5 to 30 µg L-1, and the limit of detection was 0.2 µg L-1. The constructed detection technology was validated with real water samples, and excellent spiked recoveries from 92.5 % to 105.2 % were achieved. These data clearly indicated that the proposed technology was rapid, highly selective, environmentally friendly, and possessed significant potential application and development prospects.
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Impressão Molecular , Nanoestruturas , Impressão Molecular/métodos , Doxiciclina , Polímeros Molecularmente Impressos , Corantes Fluorescentes , Polímeros/química , Antibacterianos , Adsorção , Água/química , CarbonoRESUMO
Due to the strong metal-sulfur interaction between mercapto groups and metal ions, which can be used to functionalize polyamidoamine dendrimer decorated Fe3O4 nanoparticles for high enrichment of trace heavy metal ions from waters. Based on this concept, polyamidoamine dendrimer modified Fe3O4 nanomaterials were functionalized with l-Cysteine and a new magnetic solid phase extraction for rapid adsorption and separation of Hg2+, Pb2+, Co2+ and Cd2+ from waters was established. The factors affecting extraction efficiency have been optimized. Upon the optimal parameters, the established method provided good linear ranges of 0.1-200 µg L-1 for Hg2+ and 0.05-200 µg L-1 for Pb2+, Co2+ and Cd2+, and high sensitivity with limits of detection (LOD) of 0.018 µg L-1, 0.014 µg L-1, 0.013 µg L-1 and 0.025 µg L-1 for Cd2+, Pb2+, Co2+ and Hg2+, respectively. Real water samples were utilized to validate the proposed method, and achieved results revealed that the proposed method was sensitive, effective, stable and suitable for monitoring Pb2+, Cd2+, Co2+and Hg2+ in environmental waters. This work provided a novel strategy for the simultaneous analysis of target cations in waters, and a new direction for developing decoration method of nanomaterials according to specific purpose.
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Dendrímeros , Mercúrio , Metais Pesados , Oligoelementos , Dendrímeros/química , Cisteína , Cádmio/análise , Cromatografia Líquida de Alta Pressão/métodos , Chumbo , Metais Pesados/análise , Mercúrio/análise , Oligoelementos/análise , Cátions , Adsorção , Água/química , Extração em Fase Sólida/métodos , Fenômenos MagnéticosRESUMO
Pesticides are useful products for agriculture and human life, but they are often released into surface waters and are hazardous to aquatic ecosystems. Pesticides monitoring in surface waters is challenging due to the great variety, ultratrace levels and nonpoint source pollution of pesticides; however, continuous passive sampling may be conducive to solving these problems. This work evaluated the performance of a newly developed passive sampler (hydrophilic-lipophilic balance sorbent-embedded cellulose acetate membrane, HECAM) for six types of currently used/present pesticides. The uptake kinetics and equilibrium partitioning of nineteen pesticides in different dissolved concentrations were studied by dynamic accumulation and equilibrium partitioning experiments, respectively. In the dynamic accumulation experiments, pesticides gradually accumulated in the HECAM and followed a first-order kinetic model. The same type of pesticides had roughly comparable accumulation concentrations. The estimated uptake rate constants ranged from 1.04 to 13.5 L g-1 d-1, and sampling rates ranged from 0.02 to 0.31 L d-1 for the pesticides in the HECAM (size of 2 cm × 3 cm). Pesticide accumulation concentrations in the HECAM increased linearly with increasing dissolved concentrations, which means that varying concentrations can also be monitored by the HECAM. In the equilibrium partitioning experiments, the pesticide partitioning behavior at varying dissolved concentrations can be described by the Freundlich model. The calculated equilibrium partition coefficients (log KD) for pesticides ranged from 3.32 to 4.54, and different pesticide types showed different changes with log Kow. Comparable results were found when estimating chemical equilibrium partition coefficients by the dynamic accumulation and equilibrium partitioning methods. Field deployment of the HECAM in river waters resulted in the detection of four pesticides, and the measured results were comparable to those of active sampling coupled with liquid-liquid extraction. These results suggest that the HECAM would be a promising strategy for simultaneously monitoring diverse pesticides in waters.
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Polyaniline (PANI) is a useful conductive polymer material, and has good adsorption property, which makes it a good modification material. In this work, for the sake of highly enhancing the utilization of visible region in sunlight and accelerating photocatalytic degradation of tetrabromobisphenol A (TBBPA), a typical polybrominated flame retardant, titanium dioxide nanotube arrays (TiO2 NTAs) were modified with PANI by chemical and electrochemical polymerization. The coated amount of PANI was controlled via adjusting the polymerization time and the amount of aniline in the electrochemical method. The results demonstrate that the EC-PANI/TiO2 NTAs (synthesized electrochemically) exhibit higher catalytic activity than bare TiO2 NTAs and C-PANI/TiO2 NTAs (synthesized chemically) in photoelectrocatalytic degradation of TBBPA under visible light, and the degradation efficiency for TBBPA could reach 94.37% within 120 min. The improved performance was contributed to the synergetic effect of PANI modification which integrated the broad absorption of PANI in visible light region and high catalytic property of TiO2 NTAs. Interestingly, it was also found that the degradation efficiency of TBBPA by EC-PANI/TiO2 was further enhanced by up to 95.74% when the ethanol was present in the reaction system as the hole scavenger. Furthermore, the EC-PANI/TiO2 exhibited excellent stability after 10 cycling experiments. All the results indicated that this new modified material presented strong potential as a photoelectrocatalyst and had great practical applications in the future.
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Nitrogen and sulfur element co-decorated carbon nanodots (N,S-CDs) were synthesized by solid state hydrothermal method utilizing mercaptoacetic acid and melamine as the precursors. The obtained N,S-CDs had wonderful optical and chemical stability. The experimental results demonstrated that silver nanoparticles (AgNPs) could noticeably quench the fluorescence of N,S-CDs. The quenching of fluorescence signal from the presence of AgNPs may be attributed to inner filter effect. The crafted nanoprobe for sensing AgNPs was endowed with some specialties such as simplicity, excellent selectivity and sensitivity, environmental friendliness and low cost. The probe exhibited specific linearity from 0.024 to 1.77 nM, and was endowed a good limit of detection down to 0.022 nM. The experimental results demonstrated that the built probe could be an efficient tool for AgNPs detection and had a prospective application, and also provided a new direction for establishing innovative method for determining and monitoring pollutants from nanoparticles.
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Poluentes Ambientais , Nanopartículas Metálicas , Pontos Quânticos , Carbono , Corantes , Corantes Fluorescentes , Limite de Detecção , Nitrogênio , Prata , Enxofre , Tioglicolatos , TriazinasRESUMO
Carbon nitride (CN) as the photocatalytic hydrogen production catalyst has attracted great attentions but suffering from a poor performance due to the unsatisfied energy band gap and the low separation efficiency of photogenerated carriers. Herein, we create a simple method to construct a novel CN-based photocatalyst, i.e., the N, P, O co-doped carbon filled CN microtube, which presents a narrow band gap, a high separation efficiency of photogenerated carriers, and a good stability. In this novel structure, the tubular morphology of CN ensures a narrow band gap, and the N, P, O co-doped carbon facilitates the transfer of photogenerated electrons. Coupling these two further reduces the energy band gap and improves the separation efficiency. For the photocatalytic hydrogen evolution under the visible light, the optimal sample presents an ultrahigh hydrogen evolution rate of 1149.71 µmol g-1 h-1 ranking at the top level, which is 112.60 times that of traditional bulk CN. In addition, it also has a high reusability and good stability after four cycle experiments. This study has provided a new viewpoint to design or develop the high-efficient photocatalysts for hydrogen production.
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Carbono , Nitrilas , Catálise , HidrogênioRESUMO
In this study, graphene oxide modified magnetic polyamidoamine dendrimers (MNPs@PAMAM-G2.0@GO) nanoparticles were successfully prepared by amidation method. The obtained MNPs@PAMAM-G2.0@GO nanocomposites were examined by fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), scanning electron microscope (SEM) and transmission electron microscopy (TEM), etc. MNPs@PAMAM-G2.0@GO exhibited excellent adsorption property and was investigated for magnetic solid phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) from water. The detection of extracted PAHs was accomplished by high performance liquid chromatography (HPLC) and gas chromatography tandem mass spectrometry (GC-MS/MS). The target PAHs included anthracene (ANT), pyrene (PYR), fluoranthene (FLT), carbazole (CB), 7-methylquinoline (7-MQL), 9-methylcarbazole (9-MCB), dibenzothiophene (DBT) and 4,6-dimethyldibenzothiophene (4,6-DBT). Important operation parameters for MSPE that could affect the extraction efficiencies of PAHs were investigated in detail. Under optimal parameters, the constructed method demonstrated excellent linear range with 0.001-10 µg L-1 for analytes and low limits of detection within the range of 0.11-0.9 ng L-1. The spiked average recoveries of PAHs in natural water samples ranged from 92.5% to 105.2%. The promising results indicated that MNPs@PAMAM-G2.0@GO could be employed to efficiently extract PAHs from aqueous samples.
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Dendrímeros , Hidrocarbonetos Policíclicos Aromáticos , Adsorção , Dendrímeros/química , Cromatografia Gasosa-Espectrometria de Massas , Grafite , Limite de Detecção , Fenômenos Magnéticos , Hidrocarbonetos Policíclicos Aromáticos/análise , Extração em Fase Sólida/métodos , Espectroscopia de Infravermelho com Transformada de Fourier , Espectrometria de Massas em Tandem , ÁguaRESUMO
Polychlorinated biphenyls (PCBs) are persistent organic pollutants which are widely present in environment and harmful to human health. In this study, an efficient and convenient magnetic solid phase extraction method with C60 modified magnetic polyamido-amine (PAMAM) dendrimers as sorbents was established for enriching trace amounts of PCBs in beverage samples. Gas chromatography-tandem mass spectrometry (GC-MS/MS) was utilized for analysis of PCBs. Parameters affecting extraction efficiency were optimized. Under optimal parameters, good linearity can be achieved in concentration range of 0.001-20 µg L-1 and 0.002-20 µg L-1 for nine selected PCBs. The limits of detection for PCBs were in the range of 0.1-0.2 ng L-1. The spiked recoveries were in the range of 87.0 %-115.1 % (n = 3). The results proved that this established method was reliable for monitoring trace PCBs in beverage samples.
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Dendrímeros , Bifenilos Policlorados , Aminas/análise , Bebidas/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Humanos , Fenômenos Magnéticos , Bifenilos Policlorados/análise , Extração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodosRESUMO
With the rapid consumption of fossil fuels, along with the ever-increasing environmental pollution, it is becoming a top priority to explore efficient photocatalysts for the production of renewable hydrogen and degradation of pollutants. Here, we fabricated a composite of g-C3N4/TiO2 via an in situ growth method under the conditions of high-temperature calcination. In this method, TiO2 nanowires with a large specific surface area could provide enough space for loading more g-C3N4 nanoparticles to obtain C3N4/TiO2 composites. Of note, the g-C3N4/TiO2 composite could effectively photocatalyze both the degradation of several pollutants and production of hydrogen, both of which are essential for environmental governance. Combining multiple characterizations and experiments, we found that the heterojunction constructed by the TiO2 and g-C3N4 could increase the photocatalytic ability of materials by prompting the separation of photogenerated carriers. Furthermore, the photocatalytic mechanism of the g-C3N4/TiO2 composite was also clarified in detail.
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A novel dual-signal ratiometric electrochemical aptasensor for highly sensitive and selective detection of thrombin has been designed on the basis of signal-on and signal-off strategy. Ferrocene labeled hairpin probe (Fc-HP), thrombin aptamer and methyl blue labeled bio-bar-coded AuNPs (MB-P3-AuNPs) were rationally introduced for the construction of the assay platform, which combined the advantages of the recognition of aptamer, the amplification of bio-bar-coded nanoprobe, and the ratiometric signaling readout. In the presence of thrombin, the interaction between thrombin and the aptamer leads to the departure of MB-P3-AuNPs from the sensing interface, and the conformation of the single stranded Fc-HP to a hairpin structure to take the Fc confined near the electrode surface. Such conformational changes resulted in the oxidation current of Fc increased and that of MB decreased. Therefore, the recognition event of the target can be dual-signal ratiometric electrochemical readout in both the "signal-off" of MB and the "signal-on" of Fc. The proposed strategy showed a wide linear detection range from 0.003 to 30nM with a detection limit of 1.1 pM. Moreover, it exhibits good performance of excellent selectivity, good stability, and acceptable fabrication reproducibility. By changing the recognition probe, this protocol could be easily expanded into the detection of other targets, showing promising potential applications in disease diagnostics and bioanalysis.