Fluorescence Enhancement Method for Enrofloxacin Extraction by Core–Shell Magnetic Microspheres

2020 ◽  
Vol 73 (11) ◽  
pp. 1105
Author(s):  
Linyan Yang ◽  
Leiming Fu ◽  
Boxin Li ◽  
Jifei Ma ◽  
Cun Li ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Solid Phase ◽  
Metal Organic Framework ◽  
Sodium Dodecyl ◽  
Covalent Modification ◽  
Magnetic Microspheres ◽  
Magnetic Characteristics ◽  
Fluorescent Properties ◽  
Xps Spectra ◽  
X Ray

In this work, we present novel kinds of γ-Fe2O3@SiO2-NH2-CMC/MOF5 and γ-Fe2O3@SiO2-NH2-CMC/IRMOF3 magnetic metal–organic framework (MOF) nanoparticles which possess both magnetic characteristics and fluorescent properties. Here, [Zn4O(bdc)3] (MOF-5, bdc=1,4-benzenedicarboxylate) is a kind of shell. IRMOF3, a known MOF with a cubic topology prepared from Zn(NO3)2⋅4H2O and 2-amino-1,4-benzene dicarboxylic acid, is another kind of shell which is attractive due to its highly porous, crystalline structure and the presence of non-coordinating amino groups on the benzenedicarboxylate (bdc) linker, which are amenable to post-synthetic modification. γ-Fe2O3@SiO2-NH2-CMC magnetic nanoparticles (MNPs) could be prepared by covalent modification of sodium carboxymethyl cellulose (CMC). The structure of γ-Fe2O3 nanoparticles could be determined by X-ray powder diffraction (XRD). X-ray photoelectron spectroscopy (XPS) spectra could be used for the characterisation of γ-Fe2O3@SiO2-NH2, γ-Fe2O3@SiO2-NH2-CMC, γ-Fe2O3@SiO2-NH2-CMC/MOF5, and γ-Fe2O3@SiO2-NH2-CMC/IRMOF3 nanoparticles. Magnetic solid-phase extraction (MSPE) of enrofloxacin (Enr) experiments exhibited that, for γ-Fe2O3@SiO2-NH2-CMC/IRMOF3, the best effects of adsorption could be obtained at pH 4 and 6, while elution conditions of 0.1mol L−1 NaOH and 1% sodium dodecyl sulfate could achieve the best elution effect. The addition of Tb3+ ions could sensitise the fluorescence of Enr. At the same time, via the addition of Tb3+ ions, coordination could occur between nanoparticles and Tb3+ ions, which could be verified by XPS.

scholarly journals NH2-MIL-53(Al) Polymer Monolithic Column for In-Tube Solid-Phase Microextraction Combined with UHPLC-MS/MS for Detection of Trace Sulfonamides in Food Samples

Molecules ◽  
2020 ◽  
Vol 25 (4) ◽  
pp. 897 ◽  
Author(s):  
Qian-Chun Zhang ◽  
Guang-Ping Xia ◽  
Jun-Yi Liang ◽  
Xiao-Lan Zhang ◽  
Li Jiang ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Solid Phase Microextraction ◽  
In Situ Polymerization ◽  
Solid Phase ◽  
Monolithic Column ◽  
Metal Organic Framework ◽  
Food Samples ◽  
X Ray ◽  
Polymer Monolithic Column ◽  
Relative Standard

In this study, a novel monolithic capillary column based on a NH2-MIL-53(Al) metal–organic framework (MOF) incorporated in poly (3-acrylamidophenylboronic acid/methacrylic acid-co-ethylene glycol dimethacrylate) (poly (AAPBA/MAA-co-EGDMA)) was prepared using an in situ polymerization method. The characteristics of the MOF-polymer monolithic column were investigated by scanning electron microscopy, Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray diffractometry, Brunauer-Emmett-Teller analysis, and thermogravimetric analysis. The prepared MOF-polymer monolithic column showed good permeability, high extraction efficiency, chemical stability, and good reproducibility. The MOF-polymer monolithic column was used for in-tube solid-phase microextraction (SPME) to efficiently adsorb trace sulfonamides from food samples. A novel method combining MOF-polymer-monolithic-column-based SPME with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was successfully developed. The linear range was from 0.015 to 25.0 µg/L, with low limits of detection of 1.3–4.7 ng/L and relative standard deviations (RSDs) of < 6.1%. Eight trace sulfonamides in fish and chicken samples were determined, with recoveries of the eight analytes ranging from 85.7% to 113% and acceptable RSDs of < 7.3%. These results demonstrate that the novel MOF-polymer-monolithic-column-based SPME coupled with UHPLC-MS/MS is a highly sensitive, practical, and convenient method for monitoring trace sulfonamides in food samples previously extracted with an adequate solvent.

scholarly journals Optical, XPS and XRD Studies of Semiconducting Copper Sulfide Layers on a Polyamide Film

2009 ◽  
Vol 2009 ◽  
pp. 1-8 ◽  
Author(s):  
Valentina Krylova ◽  
Mindaugas Andrulevičius
Keyword(s):  
Photoelectron Spectroscopy ◽  
Copper Sulfide ◽  
Diffusion Method ◽  
X Ray Diffraction ◽  
Xps Spectra ◽  
X Ray ◽  
Xrd Studies ◽  
Polyamide Film ◽  
Indirect Band Gap ◽  
Xrd Method

Copper sulfide layers were formed on polyamide PA 6 surface using the sorption-diffusion method. Polymer samples were immersed for 4 and 5 h in 0.15 mol⋅  solutions and acidified with HCl (0.1 mol⋅) at . After washing and drying, the samples were treated with Cu(I) salt solution. The samples were studied by UV/VIS, X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) methods. All methods confirmed that on the surface of the polyamide film a layer of copper sulfide was formed. The copper sulfide layers are indirect band-gap semiconductors. The values of are 1.25 and 1.3 eV for 4 h and 5 h sulfured PA 6 respectively. Copper XPS spectra analyses showed Cu(I) bonds only in deeper layers of the formed film, while in sulfur XPS S 2p spectra dominating sulfide bonds were found after cleaning the surface with ions. It has been established by the XRD method that, beside , the layer contains as well. For PA 6 initially sulfured 4 h, grain size forchalcocite, , was  nm and fordjurleite, , it was 54.17 nm. The sheet resistance of the obtained layer varies from 6300 to 102 .

scholarly journals Highly Efficient Adsorption of Aqueous Pb(II) with Mesoporous Metal-Organic Framework-5: An Equilibrium and Kinetic Study

2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
José María Rivera ◽  
Susana Rincón ◽  
Cherif Ben Youssef ◽  
Alejandro Zepeda
Keyword(s):  
Kinetic Study ◽  
Photoelectron Spectroscopy ◽  
Metal Organic Framework ◽  
Isotherm Models ◽  
Ionic Exchange ◽  
Order Kinetic ◽  
X Ray ◽  
Metal Organic ◽  
Mesoporous Metal ◽  
Organic Framework

Mesoporous metal-organic framework-5 (MOF-5), with the composition Zn4O(BDC)3, showed a high capacity for the adsorptive removal of Pb(II) from 100% aqueous media. After the adsorption process, changes in both morphology and composition were detected using a scanning electron microscope (SEM) equipped with an energy dispersive X-ray (EDX) system, Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS) analysis. The experimental evidence showed that Zn(II) liberation from MOF-5 structure was provoked by the water effect demonstrating that Pb(II) removal is not due to ionic exchange with Zn. A kinetic study showed that Pb(II) removal was carried out in 30 min with a behavior of pseudo-second-order kinetic model. The experimental data on Pb(II) adsorption were adequately fit by both the Langmuir and BET isotherm models with maximum adsorption capacities of 658.5 and 412.7 mg/g, respectively, at pH 5 and 45°C. The results of this work demonstrate that the use of MOF-5 has great potential for applications in environmental protection, especially regarding the removal of the lead present in industrial wastewaters and tap waters.

29Si NMR and XPS Investigation of the Structure of Silicon Oxycarbide Glasses Derived from Polysiloxane Precursors

1994 ◽  
Vol 346 ◽  
Author(s):  
R.J.P. Corriu ◽  
D. Leclercq ◽  
P.H. Mutin ◽  
A. Vioux
Keyword(s):  
Solid State ◽  
Photoelectron Spectroscopy ◽  
Solid State Nmr ◽  
Random Distribution ◽  
Silicon Oxycarbide ◽  
29Si Nmr ◽  
Xps Spectra ◽  
Excess Carbon ◽  
X Ray ◽  
Silicon Oxycarbide Glasses

ABSTRACTTwo silicon oxycarbide glasses with different compositions (O/Si ratio 1.2 and 1.8) were prepared by pyrolysis at moderate temperature (900 °C) of polysiloxane precursors. Their structure was investigated using quantitative 29Si solid-state NMR and X-ray photoelectron spectroscopy (XPS). The environment of the silicon atoms in the oxycarbide phase corresponded to a purely random distribution of Si-O and Si-C bonds depending on the O/Si ratio of the glass only and not on the structure of the precursors. At the light of the NMR results, the Si2p XPS spectra of the glasses may be interpreted using the contribution of the five possible SiOxC4-x tetrahedra. The Cls spectra of these glasses indicated the presence of oxycarbide carbon in CSi4 tetrahedra, similar to carbide carbon, and graphitic-like excess carbon.

Preparation and Characterization of Ni2+-Montmorillonite/Polyvinyl Alcohol Water-Soluble Nanocomposite Film

2005 ◽  
Vol 13 (8) ◽  
pp. 839-846 ◽  
Author(s):  
Li-Ping Wang ◽  
Yun-Pu Wang ◽  
Fa-Ai Zhang
Keyword(s):  
Polyvinyl Alcohol ◽  
Photoelectron Spectroscopy ◽  
Thermal Characteristics ◽  
Water Soluble ◽  
Scanning Calorimetry ◽  
Xps Spectra ◽  
X Ray ◽  
Alcohol Water ◽  
Ft Ir ◽  
Silicate Layers

A new type of nano-composite film was prepared from polyvinyl alcohol, Ni2+-montmorillonite (Ni2+-MMT), defoamer, a levelling agent and a plasticizer. Its thermal characteristics were studied by Differential Scanning Calorimetry (DSC). The intermolecular interactions were measured by Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS), and the tensile strength (TS) and elongation at break (%E) were measured. The microstructures were studied by X-ray diffraction (XRD) and atomic force microscopy (AFM). FT-IR and XPS spectra indicated that cross-linking has taken place between PVA and Ni2+-MMT. XRD and AFM indicate that the PVA molecules had inserted themselves into the silicate layers of MMT, exfoliating them and dispersing them randomly into the PVA matrix. Compared to pure PVA film, the TS of the films was increased and %E decreased when the Ni2+-Montmorillonite was added and the dissolution temperature of the film was also reduced.

scholarly journals Following excited-state chemical shifts in molecular ultrafast x-ray photoelectron spectroscopy

2022 ◽  
Vol 13 (1) ◽  
Author(s):  
D. Mayer ◽  
F. Lever ◽  
D. Picconi ◽  
J. Metje ◽  
S. Alisauskas ◽  
...  
Keyword(s):  
Excited State ◽  
Chemical Shift ◽  
Photoelectron Spectroscopy ◽  
Chemical Shifts ◽  
Excited Molecule ◽  
Charge Motion ◽  
Core Electron ◽  
Xps Spectra ◽  
X Ray ◽  
State Chemical

AbstractThe conversion of photon energy into other energetic forms in molecules is accompanied by charge moving on ultrafast timescales. We directly observe the charge motion at a specific site in an electronically excited molecule using time-resolved x-ray photoelectron spectroscopy (TR-XPS). We extend the concept of static chemical shift from conventional XPS by the excited-state chemical shift (ESCS), which is connected to the charge in the framework of a potential model. This allows us to invert TR-XPS spectra to the dynamic charge at a specific atom. We demonstrate the power of TR-XPS by using sulphur 2p-core-electron-emission probing to study the UV-excited dynamics of 2-thiouracil. The method allows us to discover that a major part of the population relaxes to the molecular ground state within 220–250 fs. In addition, a 250-fs oscillation, visible in the kinetic energy of the TR-XPS, reveals a coherent exchange of population among electronic states.

X-ray photoelectron spectroscopy characterization of barium titanate ceramics prepared by the citric route. Residual carbon study

1997 ◽  
Vol 12 (9) ◽  
pp. 2388-2392 ◽  
Author(s):  
C. Miot ◽  
E. Husson ◽  
C. Proust ◽  
R. Erre ◽  
J. P. Coutures
Keyword(s):  
Barium Titanate ◽  
Single Crystals ◽  
Photoelectron Spectroscopy ◽  
Residual Carbon ◽  
Ion Etching ◽  
Xps Spectra ◽  
X Ray ◽  
Titanate Ceramics

Powder and ceramics of barium titanate prepared by the citric process were studied by x-ray photoelectron spectroscopy (XPS). Spectra of C1s, O1s, Ti2p, Ba3d, and Ba4d levels are analyzed in powder and ceramics immediately after the sintering step and after several months of exposure in the air. Ar-ion etching allowed one to characterize the material intrinsic carbon. The results are discussed in comparison with works previously published on oxide single crystals.

scholarly journals Bacterial Compatibility/Toxicity of Biogenic Silica (b-SiO2) Nanoparticles Synthesized from Biomass Rice Husk Ash

Nanomaterials ◽  
2019 ◽  
Vol 9 (10) ◽  
pp. 1440 ◽  
Author(s):  
Sanjeev K. Sharma ◽  
Ashish R. Sharma ◽  
Sudheer D. V. N. Pamidimarri ◽  
Jyotshana Gaur ◽  
Beer Pal Singh ◽  
...  
Keyword(s):  
Rice Husk ◽  
Photoelectron Spectroscopy ◽  
Biogenic Silica ◽  
Rice Husk Ash ◽  
Sio2 Nanoparticles ◽  
High Porosity ◽  
Xps Spectra ◽  
X Ray ◽  
Xrd Patterns ◽  
Sio2 Nanopowder

Biogenic silica (b-SiO2) nanopowders from rice husk ash (RHA) were prepared by chemical method and their bacterial compatibility/toxicity was analyzed. The X-ray diffractometry (XRD) patterns of the b-SiO2 nanopowders indicated an amorphous feature due to the absence of any sharp peaks. Micrographs of the b-SiO2 revealed that sticky RHA synthesized SiO2 nanopowder (S1) had clustered spherical nanoparticles (70 nm diameter), while b-SiO2 nanopowder synthesized from red RHA (S2) and b-SiO2 nanopowder synthesized from brown RHA (S3) were purely spherical (20 nm and 10 nm diameter, respectively). Compared to the S1 (11.36 m2g−1) and S2 (234.93 m2g−1) nanopowders, the S3 nanopowders showed the highest surface area (280.16 m2g−1) due to the small particle size and high porosity. The core level of the X-ray photoelectron spectroscopy (XPS) spectra showed that Si was constituted by two components, Si 2p (102.2 eV) and Si 2s (153.8 eV), while Oxygen 1s was observed at 531.8 eV, confirming the formation of SiO2. The anti-bacterial activity of the b-SiO2 nanopowders was investigated using both gram-positive (Escherichia coli) and gram-negative (Staphylococcus aureus) microorganisms. Compared to S2 and S3 silica nanopowders, S1 demonstrated enhanced antibacterial activity. This study signifies the medical, biomedical, clinical, and biological importance and application of RHA-mediated synthesized b-SiO2.

scholarly journals Fabrication of Flexible, Lightweight, Magnetic Mushroom Gills and Coral-Like MXene–Carbon Nanotube Nanocomposites for EMI Shielding Application

Nanomaterials ◽  
2019 ◽  
Vol 9 (4) ◽  
pp. 519 ◽  
Author(s):  
Kanthasamy Raagulan ◽  
Ramanaskanda Braveenth ◽  
Lee Ro Lee ◽  
Joonsik Lee ◽  
Bo Kim ◽  
...  
Keyword(s):  
Carbon Nanotube ◽  
Photoelectron Spectroscopy ◽  
Electromagnetic Interference ◽  
Sodium Dodecyl ◽  
Spray Coating ◽  
Emi Shielding ◽  
X Ray ◽  
Good Thermal Stability ◽  
Potential Applications ◽  
Oxidized Carbon

MXenes, carbon nanotubes, and nanoparticles are attractive candidates for electromagnetic interference (EMI) shielding. The composites were prepared through a filtration technique and spray coating process. The functionalization of non-woven carbon fabric is an attractive strategy. The prepared composite was characterized using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDX), and Raman spectroscopy. The MXene-oxidized carbon nanotube-sodium dodecyl sulfate composite (MXCS) exhibited 50.5 dB (99.999%), and the whole nanoparticle-based composite blocked 99.99% of the electromagnetic radiation. The functionalization increased the shielding by 15.4%. The composite possessed good thermal stability, and the maximum electric conductivity achieved was 12.5 S·cm−1. Thus, the composite shows excellent potential applications towards the areas such as aeronautics, mobile phones, radars, and military.

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