RESUMO
A label-free electrochemical immunosensor has advantages of real-time and rapid detection, but it is weak in detection of small molecular toxins such as aflatoxin B1 (AFB1). The greatest obstacle to achieving this is that small molecules bound to a common immunosensing interface cannot interfere with electron transfer effectively and the detection signal is so weak. Therefore, a sensitive electrochemical immunosensing interface for small molecules is urgently needed. Here, we employed functionalized black phosphorene (BP) as electrode modification materials and anti-AFB1 nanobody (Nb) as a biorecognition element to construct a very sensitive immunosensing interface towards small molecular AFB1. The BP functionalized by carboxylic multi-walled carbon nanotubes (MWCNTs-COOH) via P-C bonding behaved with a satisfactory stability and good catalytic performance for the ferricyanide/ferrocyanide probe, while the small-sized Nb showed good compatibility with the functionalized BP and also had less influence on electron transfer than monoclonal antibody (mAb). Expectedly, the as-prepared immunosensing interface was very sensitive to AFB1 detection by differential pulse voltammetry (DPV) in a redox probe system. Under optimized conditions, a linear range from 1.0 pM to 5.0 nM and an ultralow detection limit of 0.27 pM were obtained. Additionally, the fabricated immunosensor exhibited satisfactory stability, specificity, and reproducibility. The strategy proposed here provides a more reliable reference for label-free sensing of small molecules in food samples.
Assuntos
Aflatoxina B1/análise , Técnicas Eletroquímicas/métodos , Compostos de Fósforo/química , Anticorpos de Domínio Único/química , Técnicas Biossensoriais/métodos , Limite de DetecçãoRESUMO
Coumarin possesses the aromatic group and showed plentiful activities, such as antioxidant, preventing asthma and antisepsis. In addition, coumarin derivatives usually possess good solubility, low cytotoxicity and excellent cell permeability. In our study, we synthesized the compound bridge methylene tacrine (BMT), which has the classical pharmacophore structure of Tacrine (THA). Based on the principle of active substructure splicing, BMT was used as a lead compound and synthesized coumarin-BMT hybrids by introducing coumarin to BMT. In this work, 21 novel hybrids of BMT and coumarin were synthesized and evaluated for their inhibitory activity on AChE. All obtained compounds present preferable inhibition. Compound 8b was the most active compound, with the value of Ki as 49.2 nM, which was higher than Galantamine (GAL) and lower than THA. The result of molecular docking showed that the highest binding free energy was -40.43 kcal/mol for compound 8b, which was an identical trend with the calculated Ki.
Assuntos
Doença de Alzheimer , Tacrina , Acetilcolinesterase/metabolismo , Doença de Alzheimer/metabolismo , Inibidores da Colinesterase/química , Cumarínicos/química , Cumarínicos/farmacologia , Simulação de Acoplamento Molecular , Relação Estrutura-Atividade , Tacrina/química , Tacrina/farmacologiaRESUMO
The essential oil extracted from Cinnamomum camphora leaves is a mixture of volatile compounds, mainly terpenes, and is widely used in medicine, perfume and chemical industries. In this study, the extraction processes of essential oil from Cinnamomum camphora leaves by steam distillation and supercritical CO2 extraction were summarized and compared, and the camphor tree essential oil was detected by GC/MS. The extraction rate of essential oil extracted by steam distillation is less than 0.5%, while that of supercritical CO2 extraction is 4.63% at 25 MPa, 45 °C and 2.5 h. GC/MS identified 21 and 42 compounds, respectively. The content of alcohols in the essential oil is more than 35%, and that of terpenoids is more than 80%. The steam extraction method can extract volatile substances with a low boiling point and more esters and epoxides; The supercritical method is suitable for extracting weak polar substances with a high alcohol content. Supercritical CO2 extraction can selectively extract essential oil components and effectively prevent oxidation and the escape of heat sensitive substances.
Assuntos
Cromatografia com Fluido Supercrítico , Cinnamomum camphora , Óleos Voláteis , Dióxido de Carbono , Cromatografia com Fluido Supercrítico/métodos , Destilação/métodos , Óleos Voláteis/química , Extratos Vegetais , Vapor , Terpenos/análiseRESUMO
Electrochemical sensor has great potential in the detection of small molecules by virtues of low cost, fast response, and easy to miniaturization. However, electrochemical sensing of ochratoxin A (OTA) was seriously hindered by the heavy electrode-fouling effect and poor electrochemical activity inherent from OTA molecular. Herein, two-dimensional titanium carbide (2D Ti3C2) MXene incorporated with carboxylic multiwalled carbon nanotubes (cMWCNTs) was developed as a glassy carbon electrode modifier for rapid and sensitive detection of OTA. Physical characterizations combined with electrochemical techniques revealed that cMWCNTs can not only prevent the restacking of 2D Ti3C2nanosheets but also facile its electron transfer, leading to a nanohybrid with a high specific surface and good electrocatalytic activity to OTA. Under optimal conditions, the electrochemical sensor showed a good linear response to OTA in a concentration range from 0.09 to 10µmol·l-1and a low detection limit (LOD) of 0.028µmol·l-1. The proposed sensor was impelled successive times to detect OTA, a good repeatability was obtained, indicating the constructed sensor possessed good anti-fouling property. Moreover, satisfactory recoveries between 91.8% and 103.2% were obtained in the real sample analysis of grape and beer, showing that the developed sensing technique is reliable for the screening of trace OTA in food resources.
Assuntos
Técnicas Biossensoriais/instrumentação , Nanotubos de Carbono/química , Ocratoxinas/análise , Titânio/química , Incrustação Biológica , Técnicas Biossensoriais/métodos , Técnicas Eletroquímicas/instrumentação , Limite de DetecçãoRESUMO
A novel electrochemical sensor has been fabricated for sensitive determination of zearalenone (ZEA) in food samples based on molybdenum disulfide quantum dots (MoS2 QDs) and two-dimensional titanium carbide (2D-Ti3C2Tx MXene) co-modified multi-walled carbon nanotube (MWCNT) heterostructure. Physical and electrochemical characterizations reveal that 2D-Ti3C2Tx and MoS2 QDs co-modified MWCNTs yields synergistic signal amplification effect, together with large specific surface area and excellent conductivity for the heterostructure, endowing the developed sensor with high detection performance to ZEA. Under optimized conditions, the sensor shows a wide linear range from 3.00 to 300 ng mL-1 and a low limit of detection (LOD) of 0.32 ng mL-1, which is far lower than the maximum residue limits (MRLs) settled by the European Commission. In addition, it exhibits excellent selectivity, high reproducibility with a relative standard deviation (RSD) of 1.1%, and good repeatability (RSD 1.1%). In real sample analysis recoveries ranged from 94.8 to 105% showing the proposed electrochemical sensor has high potential in practical applications. This work presents an effective and valuable pathway for the use of novel heterostructure in the biosensing field.
Assuntos
Dissulfetos/química , Técnicas Eletroquímicas/métodos , Molibdênio/química , Nanotubos de Carbono/química , Pontos Quânticos/química , Titânio/química , Zearalenona/análise , Técnicas Eletroquímicas/instrumentação , Eletrodos , Farinha/análise , Contaminação de Alimentos/análise , Limite de Detecção , Reprodutibilidade dos Testes , Zea mays/químicaRESUMO
A choline chloride-formic acid (ChCl-FA) pretreatment followed by enzymatic hydrolysis and fermentation were developed in this work for co-produce bioethanol, xylose, and lignin from eucalyptus. Results showed that ChCl-FA pretreatment can simultaneously degrade the xylan (â¼95.2%) and lignin (â¼74.4%) in eucalyptus, and obtained the pretreated eucalyptus having high glucan content and a numbers of cracks and holes, which was conducive to follow-up cellulase attacking. The hydrolysis experiments showed the maximum yield of glucose of 100 g eucalyptus was 35.3 g, which was equivalent to 90.3% of glucan in eucalyptus feedstock. The fermentation of enzymatic hydrolysate finally achieved the ethanol yield of 16.5 g, which corresponded to 74.5% theoretical ethanol yield from initial glucan in eucalyptus. In addition, 12.1 g xylose and 23.9 g lignin also could be obtained in pretreated liquid or/and hydrolysis residue, which represented for 61.4% xylan and 80.7% lignin in eucalyptus feedstock, respectively.
Assuntos
Eucalyptus , Xilose , Colina , Etanol/metabolismo , Eucalyptus/química , Fermentação , Formiatos , Glucanos/metabolismo , Hidrólise , Lignina/química , Xilanos/química , Xilose/metabolismoRESUMO
In this work, functionalized alkyl imidazolium hexafluorophosphate ILs were synthesized and characterized; then, they were applied in the conversion of xylose to furfural under the microwave method. The results showed that when CnMF was used as a catalyst, an acidic environment was provided to promote the formation of furfural. In addition, the heating method, the solvent, and the different structures of cations in the ionic liquid influenced their catalytic activity. In an aqueous solution, the yield of furfural obtained using the microwave method was better than that of the conventional heating method, and the catalytic activity of diimidazole hexafluorophosphate was better than that of monoimidazole. Meanwhile, for the diimidazole hexafluorophosphate, the change of the carbon chain length between the imidazole rings also slightly influenced the yield. Finally, the optimal yield of 49.76% was obtained at 205°C for 8 min using 3,3'-methylenebis(1-methyl-1H-imidazol-3-ium), C1MF, as a catalyst. Mechanistic studies suggested that the catalytic activity of C1MF was mainly due to the combined effect of POFn (OH)3-n and imidazole ring. Without a doubt, the catalytic activity of C1MF was still available after five cycles, which not only showed its excellent catalytic activity in catalyzing the xylose to prepare the biomass platform compound furfural but also could promote the application of functionalized ionic liquids.
RESUMO
Carbendazim, a very common contamination to the traditional Chinese medicines (TCMs), has posed serious threat to the environment and human health. However, sensitive and selective detection of carbendazim (MBC) in the TCMs is a big challenge for their complex chemical constituents. In this work, a 0D/1D nanohybrid was developed by anchoring 1T-phased MoS2 quantum dots (QDs) over multiwall carbon nanotubes (MWCNTs) via a facile assembly method. High-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, X-ray photoelectron spectroscopy, and thermogravimetric analysis (TGA) together with EIS reveal that the 1T-phased QDs can anchor over MWCNTs via van der Waals forces, and the anchoring improves the nanohybrid surface area and conductivity. Therefore, the electrochemical sensor fabricated based on the MoS2 QDs@MWCNT nanohybrid shows excellent catalytic activity to MBC oxidation. Under optimized conditions, the sensor presents a linear voltammetry response to MBC concentration from 0.04 to 1.00 µmol·L-1, a low detection limit of 2.6 × 10-8 mol·L-1, as well as high selectivity, good reproducibility, and long-term stability. Moreover, the sensor has been successfully employed to determine MBC in two typical TCMs and the obtained recoveries are in good accordance with the results achieved by HPLC, showing that the constructed sensor plate holds great practical application in MBC analysis with complex matrix.
RESUMO
Pyrolysis-gas chromatography/mass-spectrometry (Py-GC/MS) was employed to achieve fast pyrolysis of cellulose and on-line analysis of the pyrolysis vapors. Three sulfated metal oxides (SO(4)(2-)/TiO(2), SO(4)(2-)/ZrO(2) and SO(4)(2-)/SnO(2)) were prepared and used for catalytic cracking of the pyrolysis vapors. The distribution of the pyrolytic products was significantly altered by the catalysts. Those important primary pyrolytic products, such as levoglucosan and hydroxyacetaldehyde, were significantly decreased or even completely eliminated. Meanwhile, the catalysis increased three light furan compounds (5-methyl furfural, furfural and furan) greatly. In regard to the selectivity of the three catalysts, the SO(4)(2-)/SnO(2) was the most effective catalyst for obtaining 5-methyl furfural, while the SO(4)(2-)/TiO(2) favored the formation of furfural and the SO(4)(2-)/ZrO(2) favored the formation of furan.