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1.
In this paper, Fe3O4@ZnO core/shell magnetic nanoparticles (MNPs) have been synthesized by a simple method, to modify carbon paste/glassy carbon electrode and improve its efficiency for determination of quercetin. The synthesized MNPs were characterized by X-ray powder diffraction (XRD), transmission electronic microscope (TEM), and scanning electronic microscope (SEM). SEM and TEM results show that the prepared Fe3O4@ZnO MNPs are made of the spherical shape particles with an average size of about 15 nm. The electrochemical behavior of quercetin at the surface of modified electrode was investigated. Under the optimal conditions, a linearity range of quercetin was 7.9?×?10?7 to 6.1?×?10?5 mol/L (0.24–18.44 mg/L) with detection limit (S/N?=?3) and sensitivity of 0.16 μmol/L (0.048 mg/L) and 0.04 μA/μM, respectively. The validated method was applied successfully for determination of quercetin in some foods and human breast milk.  相似文献   

2.
An indirect competitive chemiluminescence (CL) immunoassay based on Fe3O4@SiO2@Au magnetic nanoparticles (Au-SCMPs) has been optimized and developed for the detection of aflatoxin B1 (AFB1). To improve the detection sensitivity and efficiency, this method combines 2′,6′-dimethylcarbonylphenyl-10-sulfopropyl acridinium-9-carboxylate 4′-NHS ester (NSP-DMAE-NHS) as a new kind of high efficient luminescence reagent with a simplified separation procedure based on the optimized Au-SCMPs. Superparamagnetic nanoparticles were coated with different sizes of Au colloids (18, 30, and 50 nm), and their capacities in immobilization of bovine serum albumin (BSA) were investigated. The BSA-AFB1 conjugate (BSA-AFB1) was immobilized on the optimized Au-SCMPs and competed with the free AFB1 for specially binding the NSP-DAME-NHS-labeled anti-AFB1 antibody (mAb-AFB1). After the indirect competitive immunoreactions and magnetic separation, the CL of the nanoparticles was measured by a homemade luminescent measurement system. Under the optimum conditions, the IC50 value was 0.07 ng mL?1 and the limit of detection (LOD) of AFB1 was 0.01 ng mL?1, respectively. The result shows a much lower IC50 and LOD than that typically achieved by ELISA. This proposed immunoassay method was rapid, low-cost, and suitable for the detection of AFB1.  相似文献   

3.
A novel electrochemical method to detect riboflavin was proposed using a multi-walled carbon nanotubes and ionic liquid N-butyl-N-methyl-piperidinium hexafluorophosphate composite film modified glassy carbon electrode (MWNTs-[BMPi]PF6/GCE). A well-defined CV behavior with a pair of sensitive and well-shaped redox peak was observed, and the response value of riboflavin at MWNTs-[BMPi]PF6/GCE is much higher than that at MWNTs/GCE in 0.1 mol L?1 HAc-NaAc buffer solution (pH 4.5). The electrochemical approach based on a sensitive DPV analytical signal exhibits an excellent analytical performance with a wide linear range (2.6 × 10?8 to 1.3 × 10?6 mol L?1) and low detection limit (4.7 × 10?9 mol L?1) for the riboflavin. Moreover, the proposed method possesses a potential practical application value and can be employed for the quantitative analysis of trace riboflavin with a recovery of 95.8–102.4 % in food samples such as milk and soymilk powder.  相似文献   

4.
A glassy carbon electrode (GCE) was modified with eosin Y that was electrodeposited on GCE via continuous cycling between ??1.6 and 1.5 V (vs Ag/AgCl). This electrode was characterized by scanning electron microscopy and electrochemical impedance spectra. The resulting electrode exhibited excellent electrocatalytic activity toward the oxidation of butylated hydroxyanisole (BHA) and tert-butyl hydroquinone (TBH2Q); in addition, the oxidation products of BHA and TBH2Q were found to be the same, which was studied by CV and in situ FT-IR spectroelectrochemistry. Under the optimized condition, the oxidation peak currents were linear to BHA/TBH2Q in the range from 0.10 to 7.00 μg mL?1 with the detection limits of 0.01 μg mL?1 (S/N?=?3) for BHA and 0.015 μg mL?1 (S/N?=?3) for TBH2Q, respectively. Moreover, the reproducibility and repeatability of the electrode were determined. The proposed method was successfully applied in the simultaneous determination of BHA and TBH2Q in several edible oil samples, and satisfactory results when compared with those obtained using high-performance liquid chromatography.  相似文献   

5.
In this paper, a novel electrochemical sensor for the detection of H2O2 was proposed based on gold nanochains and prussian blue nanorods (PB@MWCNTs), which were synthesized with multiwall carbon nanotubes (MWCNTs) as a template. With the introduction of MWCNTs and the gold nanochains, the proposed system shows synergy among the Prussian blue (PB), MWCNTs, and the gold nanochains, which amplifies the H2O2 sensitivity greatly. A linear range from 1.75 × 10−6 to 1.14 × 10−3 M with a detection limit of 0.5 × 10−6 M (S/N = 3) and a high sensitivity 300 μA mM−1 cm−2 for H2O2 detection is obtained. Moreover, the sensor exhibits good repeatability and stability.  相似文献   

6.
Reports from the US media have raised the attention towards a possible contamination of apple juices by As. The study here described presents the development of an analytical procedure using inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) for determination of As in apple and orange juices commercialized in the Tetra Pack® package. The microwave-assisted acid digestion of juice was carried out using closed vessels and 2 mol/L HNO3 plus H2O2. These conditions are favorable for a better analytical blank control. Suitable recoveries were reached when promoting reaction with O2 inside the octopole reaction system (ORS3), and the monitoring of 75As16O+ significantly improved the accuracy of the analysis reaching a limit of detection of 0.013 μg/L. Recoveries varied from 88 to 109 % in the MS/MS mass-shift mode. The As concentrations determined in fruit juices ranged from 0.126 to 1.45 μg/L, and they were significantly lower than the maximum tolerable limits imposed by the US and Brazilian legislations. Thus, ICP-MS/MS operated in the reaction mode was an effective instrumental strategy for overcoming spectral interferences, such as 40Ar35Cl+, in As determination as 75As16O+ and allowed the accurate determination of As at trace levels.  相似文献   

7.
Salmonella typhimurium is one of the most common causes of food-associated disease. A colorimetric nanosensor was developed to detect S. typhimurium which was based on the gold nanoparticles’ (GNPs) color change effect. Fe3O4 magnetic nanoparticles (MNPs) and GNPs were synthesized separately. Two complementary sequences of the S. typhimurium target DNA were combined to Fe3O4 MNPs and GNPs to fabricate capture probes and signal probes. Fe3O4 MNPs could achieve the rapid separation and enrichment of target DNA. With the addition of S. typhimurium target DNA sequences, the sandwich-like structures were formed via the DNA hybridization recognition effect. The original good dispersion of GNPs was broken. GNPs showed different degrees of aggregation with different amount of S. typhimurium target DNA. The color changed from red, purple to blue which could be characterized by UV-Vis spectrophotometer. The absorbance spectra of GNPs red shifted constantly with the intensity ratio of A700/A521 changed regularly. There was a linear correlation between the ratio of A700/A521 and the amount of S. typhimurium target DNA. Thus, this was calculated for the basis of quantitative detection of S. typhimurium. This method is simple and rapid with high sensitivity and specificity which could be used to detect actual samples.  相似文献   

8.
The authors describe a novel sensor for chlorogenic acid (CGA) detection/quantification in food samples. The photosensor is based on a composite of titanium dioxide (TiO2) and acridine orange (AO). The synergism between AO and TiO2 was revealed under visible LED light irradiation by high photocurrents for CGA, when compared to each component of the composite material. A detection limit of 0.54 μmol L?1 and a linear response range from 2 to 200 μmol L?1 for CGA detection were achieved. The selectivity of the sensor was tested by using common interferents on samples containing chlorogenic acid and results suggested that there is no significant interference in the analyte response, indicating a good selectivity. Finally, the photosensor was successfully applied in the determination of CGA in samples of coffee, tea, and apple juice, with recoveries ranging from 100.9 to 102.4%, suggesting a good accuracy for the proposed method.  相似文献   

9.
In this study, we designed and synthesized Fe3O4/reduced graphene oxide (Fe3O4/rGO) and MIL@MIP, which were characterized using transmission electron microscopy (TEM), X-ray diffraction, Fourier transform infrared (FT-IR), cyclic voltammetry (CV), and differential pulse voltammetry (DPV). Here, reports a novel biomimetic electrochemical sensor (BECS) sensitized with Fe3O4/reduced graphene oxide (Fe3O4/rGO) nanocomposite using MIL@MIP film as recognition element for ultrasensitive quantification of methamidophos or omethoate. The BECS offered fast responses for methamidophos and omethoate with wide linear response ranges of 1.0 × 10?7–1.0 × 10?12 and 1.0 × 10?7–1.0 × 10?13 mol/L, respectively. Under optimized conditions, the limit of detection (LOD; S/N = 3) of the BECS method was 2.67 × 10?13 mol/L for methamidophos and 2.05 × 10?14 mol/L for omethoate. The BECS was applied to detection of methamidophos and omethoate in spiked cucumber and kidney bean samples, and good recoveries varied from 88.2 to 96.9 %. This proposed method was adopted for the determination of the methamidophos or omethoate residues in the rape sample, and the results were also verified using the method of gas chromatography.  相似文献   

10.
A protease from sorghum malt variety KSV8–11 was purified by a combination of dialysis against 4 M sucrose, ion‐exchange chromatography on Q‐Sepharose (Fast flow), gel filtration chromatography on Sephadex G‐100 and hydrophobic interaction chromatography on Phenyl Sepharose CL‐4B. The enzyme was purified 5‐fold to give a 14.1% yield relative to the total activity in the crude extract and a final specific activity of 1348.9 U mg?1 protein. SDS‐PAGE revealed a single migrating protein band corresponding to a relative molecular mass of 16 KDa. Using casein as substrate, the purified protease had optimal activity at 50°C and maximal temperature stability between 30°C and 40°C but retained over 64% of its original activity after incubation at 60°C for 30 min. The pH optimum was 5.0 with maximum stability at pH 6.0 but 60% of the activity remained after 24 h between pH 5.0 and 8.0. The protease was inhibited by Ag+, Ca2+, Co2+, Fe2+, Mg2+, iodoacetic acid (IAA) and p‐chloromercuribenzoate (p‐CMB), stimulated by Cu2+, Sr2+, phenylmethylsulfonyl‐fluoride (PMSF) and 2‐mercaptoethanol (2‐ME) while Mn2+ and ethylenediaminetetraacetic acid (EDTA) had no effect. The purified enzyme had a Km of 18 mg·mL?1 and a Vmax of 11.1 μmol · mL?1 · min?1 with casein as substrate.  相似文献   

11.
Seaweeds are considered as a health food partly due to the polysaccharide composition of the cell wall. Because conventional extraction methods have low yields and lead to environmental pollution, enzymatic methods have been proposed. In this study, a new strain of Bacillus sp. was isolated from cattle feces that produced a mannanase, a polysaccharide-degrading enzyme active against the green seaweed Codium fragile. The purified 39-kDa mannanase exhibited maximum activity at 55 °C and pH 6.0, and maintained its catalytic activity stably at temperatures up to 60 °C and at a broad pH range (5.0–11.0). Enzymatic activity was slightly enhanced by Cu2+ and Na+ but strongly inhibited by Fe2+, Ag+, and EDTA. The mannanase showed the highest specificity to the inexpensive substrates such as konjac powder and locust bean gum, and efficiently released various manno-oligosaccharides. This novel mannanase can thus be applicable in the food, feed, and pulp industries.  相似文献   

12.
Antibody preparation is the most important step in immunoassays. According to immunity theory (IT) “Antibody tends to recognize the furthest distance of side groups in the coupling league,”; immunogen must be well designed for high-specific antibody production for high-specific antibody preparation. In this research, a novel fumonisin B1 immunogen was synthesized in which protein was conjugated at C2 position to expose the distant two type–feature groups of side chains at C14 and C15 position. After immunization, a high-specific anti-FB1 monoclonal antibody (mAb) was produced with negligible CR value to analogues, including the most structure-related FB2 and FB3. Based on this mAb, a specific ELISA method was developed and validated for FB1 detection in rice with limit of detection at 0.0339 ng kg?1. In real-life samples, 20% were detected positive in 10 samples, with FB1 concentrations at 84 and 20 ng kg?1, respectively.  相似文献   

13.
This paper describes the synthesis and application of a novel magnetic metal–organic framework (MOF) [(Fe3O4-benzoyl isothiocyanate)/Cu3(benzene-1,3,5-tricarboxylate)2] to pre-concentrate trace amounts of Cd(II), Pb(II), Zn(II) and Cr(III) ions and their determination by flame atomic absorption spectrometry. A Box–Behnken design was used to find the parameters affecting the pre-concentration procedure through response surface methodology. Three factors including uptake time, amount of the magnetic sorbent and pH of the sample were selected as affecting factors in the sorption step, and four factors including type, volume and concentration of the eluent as well as the elution time were selected in the elution step for the optimisation study. The opted values were 30 mg, 10.1 min, 5.9, EDTA, 4.0 ml, 0.57 mol l–1 EDTA solution and 13.0 min for the amount of the magnetic sorbent, uptake time, pH of the sample, type, volume, concentration of the eluent, and elution time, respectively. The limits of detection (LODs) were 0.12, 0.7, 0.16, and 0.4 ng ml?1 for Cd(II), Pb(II), Zn(II) and Cr(III) ions, respectively. The relative standard deviations (RSDs) of the method were less than 7.2% for five separate batch experiments for the determination of 30 μg l?1 of Cd(II), Pb(II), Zn(II) and Cr(III) ions. The sorption capacity of the [(Fe3O4-benzoyl isothiocyanate)/MOF] was 175 mg g?1 for Cd(II), 168 mg g?1 for Pb(II), 210 mg g?1 for Zn(II) and 196 mg g?1 for Cr(III). It was found that the magnetic MOF nanocomposite demonstrated a higher capacity compared with Fe3O4-benzoyl isothiocyanate. Finally, the magnetic MOF nanocomposite was successfully applied to the rapid extraction of trace amounts of the heavy metal ions from vegetable samples.  相似文献   

14.
A photodegradation study of aflatoxin B1 (AFB1) in peanut oil was performed under UV irradiation at different AFB1 initial concentrations and UV irradiation intensities. The UV intensity and the irradiation duration on the AFB1 photodegradation ratio is more effective, when compared with AFB1 initial concentration, and AFB1 with initial concentration of 2 mg/kg can be degraded thoroughly within 30 min under the intensity of 800 μw/cm2. The photodegradation of AFB1 between the selected ranges of concentrations was proved to follow first-order reaction kinetics well (R 2 ≥ 0.99). The Ames test, employing Salmonella typhimurium tester strains TA98 and TA100, was employed to evaluate the residual toxicity of the AFB1 subproducts in peanut oil, and the results indicated that the mutagenic activity of UV-treated samples (800 μw/cm2 × 30 min) was completely lost compared with that of untreated samples, providing clues to the assessment of safety issues of UV method applied in AFB1 decontamination.  相似文献   

15.
A reversed phase high-performance liquid chromatography method (HPLC) with coulometric electrochemical detection has been applied and validated for the simultaneous analysis of pyridoxamine (PM), pyridoxal (PL), and pyridoxine (PN) in cereal products. Isocratic separation was achieved using a C18 column with a mobile phase consisting of methanol-phosphate buffer (10:90) and 0.018 M trimethylamine adjusted to pH 3.55 with 85% orthophosphoric acid. The limits of detection for PM, PL, and PN were 0.28, 0.36, and 0.43 ng mL?1, respectively, with vitamins recoveries ranging from 90.4 to 98.1%. The applied method for the analysis of B6 vitamins naturally present in grain products, offers a simple and fast sample preparation without derivatization. To understand vitamer separation further, methods of computational chemistry were employed. Specifically, density functional theory (DFT) was used to determine electrostatic potentials, as well as the charges of each vitamer. A number of correlations were established between these properties and elution order.  相似文献   

16.
Casting method was used to prepare bovine gelatin based bio-nanocomposite films with halloysite nanoclay and nano-SiO2 as the reinforcing materials. The composition included gelatin with 20% (w/w) of glycerol (as plasticizer) compounded with halloysite nanoclay and nano-SiO2 (0%, 2%, 3%, 4%, 5% w/w), respectively. Both types of nanocomposite films showed better mechanical and water solubility than the pristine gelatin films. On comparison with the control, increase in the nanoparticles content resulted in higher tensile strength (9.19 to 13.39 and 12.22 MPa in nanoclay and nano-SiO2, respectively) and elastic modulus (1.32 to 2.99 and 3.02 MPa% in nanoclay and nano-SiO2, respectively) with lower elongation at break (80.80 to 55.72 and 40.31% in nanoclay and nano-SiO2, respectively) and water solubility (85.99 to 69.67 and 69.59% in nanoclay and nano-SiO2, respectively). Even though a decrease in water vapor permeability was recorded, it was statistically non-significant (1.94 to 1.50 and 1.73 g mm/m2 h kPa in nanoclay and nano-SiO2, respectively). Studies on the heat sealing and peel seal test, conducted to determine the seal strength of the nanocomposite films, revealed lower seal strength compared to control (739.59 to 304.95 and 397.85 N/m in nanoclay and nano-SiO2, respectively). Between the two nanomaterials used, halloysite nanoclay showed the best results in terms of mechanical properties. The results obtained support the concept of nanocomposite technology and can be employed to improve the barrier and mechanical properties of bovine gelatin films with high potential to be used for food packaging purposes.  相似文献   

17.
The polyphenol oxidase (PPO) enzyme was purified and characterized from Hem?in Apple (Malus communis L.), which was organically grown in Hem?in, in the Rize province of Turkey. Enzyme (PPO) activation was determined with catechol substrate. Apples were homogenized with homogenate buffer (pH 8.5). This process was followed by precipitation with (20–80%) saturated solid (NH4)2SO4 and dialysis. Finally, purification with DE52-Cellulose ion-exchange and Sephadex G-25 columns was performed. Experiments were performed at an optimum pH (5.5) and optimum temperature (30–40°C). The kinetic and thermal parameters Km (3.40 mM), Vmax (333.3 EU/mL.min), Ea (3.57 kcal), ?H (2.968 kcal/mol), Q10 (1.33), kcat (24.57 min?1) and V0 (7.2x103 mM?1.min?1) were assessed. Additionally, the effects of Mg2+, Pb 2+, Fe2+, Fe3+, Cd2+, Cu2+, Zn2+, Co2+, Al3+, Mn2+ and Na+ on enzyme activity was recorded, and the IC50 values, K? values and inhibition types were determined.  相似文献   

18.
A new chemically modified electrode is constructed by incorporating AlMCM-41 into carbon paste matrix (AlMCM-41-MCPE) and used as a sensitive sensor for detection of aluminum in aqueous and nonaqueous solutions. The rapid exchange kinetics in the membrane results in a near-Nernstian behavior of the modified electrode and makes it a suitable potentiometric sensor for detection of aluminum. A linear response in concentration range from 1.0?×?10?6 to 1.0?×?10?1 mol/L (0.027 μg/mL–2.7 mg/mL) was obtained with a detection limit of 4.6?×?10?7 mol/L for the potentiometric detection of aluminum. Selectivity coefficients of a number of interfering cations have been estimated. The interference from many of the investigated ions is negligible. The AlMCM-41-MCPE is suitable for use in aqueous solution of pH 2–6 and in partially nonaqueous medium. The modified electrode exhibited a fast response time (~8 s), good stability, and an extended lifetime. The developed sensor was used successfully for the determination of Al3+ in some alloys, drugs, and food products.  相似文献   

19.
《Journal of dairy science》2022,105(3):2108-2118
Foods contaminated by foodborne pathogens have always been a great threat to human life. Herein, we constructed an electrochemical immunosensor for Salmonella detection by using a Fe3O4@graphene modified electrode. Because of the excellent electrical conductivity and mechanical stability of graphene and the large specific surface area of Fe3O4, the Fe3O4@graphene nanocomposite exhibits an excellent electrical signal, which greatly increased the sensitivity of the immunosensor. Gold nanoparticles were deposited on Fe3O4@graphene nanocomposite by electrochemical technology for the immobilization of the antibody. Cyclic voltammetry was selected to electrochemically characterize the construction process of immunosensors. The microstructure and morphology of related nanocomposites were analyzed by scanning electron microscopy. Under optimized experimental conditions, a good linear relationship was achieved in the Salmonella concentration range of 2.4 × 102 to 2.4 × 107 cfu/mL, and the limit of detection of the immunosensor was 2.4 × 102 cfu/mL. Additionally, the constructed immunosensor exhibited acceptable selectivity, reproducibility, and stability and provides a new reference for detecting pathogenic bacteria in milk.  相似文献   

20.
The cytoprotective effects of five flavonoids (quercetin, rutin, catechin, kaempferol and morin) and four hydroxycinnamic acids (caffeic, ferulic, sinapic and chlorogenic acids) were evaluated by the degree of protection they provided against H2O2-induced damage to human neuroblastoma SH-SY5Y cells. All compounds exhibited protection against H2O2-mediated cytotoxicity in a dose dependent manner. The concentration required to give a 50% reduction in cell death (EC50 value) were derived from their dose–response relationships. The cytoprotective activities of these phenolic compounds in the order of quercetin > caffeic acid > rutin > chlorogenic acid > catechin > ferulic acid > sinapic acid > morin > kaempferol. The EC50 values of the phenolic compounds were strongly related to their chemical structures. The EC50 values were compared with the antioxidant activities as determined by five different chemically based antioxidant assays [2,2-azinobis (3-ethyl-benzothiazoline-6-sulfonic acid (ABTS), 1,1-diphenyl-2-picrylhydrazyl (DPPH), oxygen radical absorbance capacity (ORAC), ferric reducing antioxidant power (FRAP) and lipid peroxidation inhibition capacity (LPIC)]. The ability of these phenolic compounds to protect from H2O2-induced SH-SY5Y cell death correlated (r 2 = 0.85) with their determined LPIC values and weakly (r 2 = 0.44) with their ABTS activities. There was no correlation between EC50 values and ORAC, FRAP or DPPH activities. The cytoprotection assay is a more biologically relevant measurement than the chemically defined antioxidant activity assays because it uses human cells as a substrate and therefore accounts for some aspects of uptake, metabolism and location of antioxidant compounds within cells.  相似文献   

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