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Ion-pairing chromatography coupled with inductively coupled plasma mass spectrometry (ICP-MS) used for the speciation of phosphorus is limited as the mobile phase containing organic solvents changes in detection sensitivity and the carbon precipitates on torch and cones. To address this issue, anion-exchange chromatography with ICP-MS has been used for the speciation of glyphosate, phosphate and aminomethylphosphonic...
In this work, a large-volume on-column injection method for the analysis of 21 organochlorine pesticides, including HCH isomers, DDT derivatives and cyclodiene derivatives, was optimized. The solvent selected to carry out the study was ethyl acetate and the injection volume was 100μl. Some factors were introduced in a Plackett–Burman design to determine their influence in the vaporization efficiency...
A quartz crystal microbalance (QCM) immunosensor was developed for the determination of the insecticide carbaryl and 3,5,6-trichloro-2-pyridinol (TCP), the main metabolite of the insecticide chlorpyrifos and of the herbicide triclopyr. The detection was based on a competitive conjugate-immobilized immunoassay format using monoclonal antibodies (MAbs). Hapten conjugates were covalently immobilized,...
Laser-induced breakdown spectroscopy (LIBS) has been developed for determining the percentage of uranium in thorium–uranium mixed oxide fuel samples required as a part of the chemical quality assurance of fuel materials. The experimental parameters were optimized using mixed oxide pellets prepared from 1:1 (w/w) mixture of thorium–uranium mixed oxide standards and using boric acid as a binder. Calibration...
A sandwich-type immunoassay linked with inductively coupled plasma mass spectrometry (ICP-MS) has been developed for the detection of anti-erythropoietin antibodies (anti-EPO Abs). Recombinant human erythropoietin (rhEPO) was immobilized on the solid phase to capture anti-rhEPO Abs specifically. After the immunoreactions with Au-labeled goat-anti-rabbit IgG, a diluted HNO 3 (2%) was used to...
Capillary electrophoresis (CE) coupled with fiber-optic light-emitting diode-induced fluorescence detection has been developed for the separation of tyrosine (Tyr) enantiomers. R(−)-4-(3-isothiocyanatopyrrolidin-1-yl)-7-(N,N-dimethylaminosulfonyl)-2,1,3-benzoxadiazole was used as a chiral fluorescence tagged reagent for derivatization of Tyr. The effect of pH, running buffer concentration and applied...
The rise of monolithic stationary phases offers to routine and research laboratories several advantages. In spite of their recent discovery, they have rapidly become highly popular separation media for liquid chromatography. Time reduction and economic reasons like e.g. a diminished use of mobile phase are the most important ones. At the same time, it was reported that these columns offer a faster...
Size-exclusion chromatography (SEC) coupled with online laser light-scattering (LS) and refractive index (RI) detection provides an excellent approach to determine the molecular weights (Mw) of proteins by the “two-detector” approach. Mw is determined only at the maximum of a peak, using either peak heights or area ratio from the two detectors. However, proper calibration of the SEC/LS/RI system is...
Perovskite type LaCo x Fe 1−x O 3 nanoparticles was synthesized by a sol–gel citrate method. The structural, electrical and sensing characteristics of the LaCo x Fe 1−x O 3 system were investigated. The structural characteristics were performed by using X-ray diffraction (XRD) and transmission electron microscopy (TEM) to examine the phase and morphology...
On-line preconcentration and determination of transition and rare-earth metals in water samples was performed using a Multi-Auto-Pret system coupled with inductively coupled plasma-atomic emission spectrometry (ICP-AES). The Multi-Auto-Pret AES system proposed here consists of three Auto-Pret systems with mini-columns that can be used for the preconcentration of trace metals sequentially or simultaneously,...
The electrochemical behaviors of guanosine on the ionic liquid of N-butylpyridinium hexafluorophosphate (BPPF 6 ) modified carbon paste electrode (CPE) was studied in this paper and further used for guanosine detection. Guanosine showed an adsorption irreversible oxidation process on the carbon ionic liquid electrode (CILE) with the oxidation peak potential located at 1.12V (vs. SCE) in a...
A novel fluorescent peptide sensor containing tryptophan (donor) and dansyl fluorophore (acceptor) was synthesized for monitoring heavy and transition metal (HTM) ions on the basis of metal ion binding motif (Cys-X-X-X-Cys). The peptide probe successfully exhibited a turn on and ratiometric response for several heavy metal ions such as Hg 2+ , Cd 2+ , Pb 2+ , Zn 2+ ...
Interaction of luminol with phosphomolybdic, phosphovanadomolybdic and silicomolybdic acids was studied by examination of chemiluminescence spectra, measurement of ESR spectra, investigation of reaction order, and elucidation of inhibition effects. A scheme of the reaction mechanism is proposed.
A novel on-line preconcentration method based on liquid–liquid (L–L) extraction with room temperature ionic liquids (RTILs) coupled to flame atomic absorption spectrometry (FAAS) was developed for cadmium determination in plastic food packaging materials. The methodology is based on the complexation of Cd with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) reagent after sample digestion...
A sensor array system consisting of five quartz crystal microbalance (QCM) sensors (four for measuring and one for reference) and an artificial neural network (ANN) method is presented for on-line detection of volatile organic compounds. Three ionic liquids, 1-butyl-3-methylimidazolium chloride (C 4 mimCl), 1-butyl-3-methylimidazolium hexafluorophosphate (C 4 mimPF 6 ), 1-dedocyl-3-methylimidazolium...
Characterisation of phytoplankton communities in aquatic ecosystems is a costly task in terms of time, material and human resources. The general objective of this paper is not to replace microscopic counts but to complement them, by fine-tuning a technique using absorption spectra measurements that reduces the above-mentioned costs. Therefore, the objective proposed in this paper is to assess the...
A sensitive, label free electrochemical aptasensor for small molecular detection has been developed in this work based on gold nanoparticles (AuNPs) amplification. This aptasensor was fabricated as a tertiary hybrid DNA–AuNPs system, which involved the anchored DNA (ADNA) immobilized on gold electrode, reporter DNA (RDNA) tethered with AuNPs and target-responsive DNA (TRDNA) linking ADNA and RDNA...
Developments carried out in the Laboratory of Isotopic, Nuclear and Elementary Analyses in order to quantify 147 Pm in spent nuclear fuels analyzed at the CEA within the framework of the Burn Up Credit research program for neutronic code validation are presented here. This determination is essential for safety-criticality studies.The quantity and the nature of the radionuclides in irradiated...
In this work, a simple and sensitive electroanalytical method was developed for the determination of enrofloxacin (ENRO) by adsorptive cathodic stripping voltammetry (ADSV) using Cu(II) as a suitable probe. The complex of copper(II) with ENRO was accumulated at the surface of a hanging mercury drop electrode at −0.10V for 40s. Then, the preconcentrated complex was reduced and the peak current was...
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