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A new fast and reproducible approach is described for the application of the enzymatic probe sonication (EPS) methodology [J.L. Capelo, P. Ximénez-Embún, Y. Madrid-Albarrán, C. Cámara, Anal. Chem. 76 (2004) 233–237] for total selenium determination by electrothermal atomic absorption spectrometry, ET-AAS. Ni(NO 3 ) 2 and Pd(NO 3 ) 2 were studied as matrix modifiers...
The performance of two different types of inductively coupled plasma mass spectrometry (ICP-MS) instruments for resolving spectral overlaps on Se isotopes was compared by means of selenium isotopic ratio measurements. Examined were a quadrupole-based, hexapole collisions cell CC-ICP-MS and a double-focusing sector field SF-ICP-MS. Due to the importance of precise and accurate isotope ratio determination...
This paper focuses on the analytical performance improvement of the coupled technique HPLC–ICPMS using on-line collision/reaction cell technology for selenium elemental and speciation analyses at the ng (Se) l −1 level in aquatic environment. Collision/reaction cell operating parameters were optimised, resulting in selected conditions of 5.5mlmin −1 H 2 and 0.5mlmin −1...
A simple and robust flow injection system which permits low sample and reagent consumption is described for rapid and reliable hydride generation atomic absorption spectrometric determination of selenium, arsenic and bismuth. The system, which composed of one peristaltic pump and one four channel solenoid valve, used water as the carrier streams for both sample and NaBH 4 solution. Rapid off-line...
A sequential extraction procedure was developed for the fractionation of different classes of selenium species present in garlic. The consecutive steps included leaching with water, extraction of cell-wall bound species after lysis with a mixture of cellulase, chitinase and β-glucanase completed by a proteolytic attack, extraction with HCl to liberate the residual organic bound species and finally,...
The combination of headspace–solid phase microextraction (HS–SPME) and gas chromatography–inductively coupled plasma mass spectrometry (GC–ICPMS) was evaluated for the determination of volatile selenium metabolites in normal urine samples, i.e. without selenium supplementation. HS–SPME operating conditions were optimised and a sampling time of 10min was found to be suitable for simultaneous extraction...
A procedure has been developed for the determination of bioavailable concentrations of selenium and arsenic in estuarine sediments employing inductively coupled plasma optical emission spectrometry (ICP OES) using a concomitant metals analyzer device to perform hydride generation. The optimization of hydride generation was done in two steps: using a two-level factorial design for preliminary evaluation...
An enzyme-assisted extraction used to extract all species of selenium in rice sample and a sensitive analytical method for the determination of ultratrace Se(VI), Se(IV), SeCys 2 (selenocystine) and SeMet (selenomethionine) with capillary electrophoresis-inductively coupled plasma mass spectrometry were firstly described in this study. The extraction method is simple, effective and can be...
The present investigation is the first part of an initiative to prepare a regional map of the natural abundance of selenium in various areas of Brazil, based on the analysis of bean and soil samples. Continuous-flow hydride generation electrothermal atomic absorption spectrometry (HG-ET AAS) with in situ trapping on an iridium-coated graphite tube has been chosen because of the high sensitivity and...
A non-chromatographic separation and preconcentration method for Se species determination based on the use of an on-line ionic liquid (IL) dispersive microextraction system coupled to electrothermal atomic absorption spectrometry (ETAAS) is proposed. Retention and separation of the IL phase was achieved with a Florisil ® -packed microcolumn after dispersive liquid–liquid microextraction (DLLME)...
Yeast (Saccharomyces cerevisiae) and lactic bacteria have shown their ability to accumulate and transform inorganic selenium into organo Se compounds. The objective of this work was to evaluate selenium biotransformation during brewing by using S. cerevisiae and Saccharomyces uvarum for Ale and Lager fermentation, respectively. Se-enriched beer was produced by the addition of sodium selenite (0, 0...
Dynamic fractionation is considered to be an attractive alternative to conventional batch sequential extraction procedures for partitioning of trace metals and metalloids in environmental solid samples. This paper reports the first results on the continuous-flow dynamic fractionation of selenium using two different extraction systems, a microcolumn (MC) packed with the solid sample and a rotating...
A novel adsorbent was developed by coating Mg–FeCO 3 layered double hydroxides (LDHs) on cellulose fibre. The LDHs take up significant amount of selenite and selenate in a wide pH range with similar sorption capacities (pH 3.8–8.0 for selenite and pH 5.8–7.0 for selenate). A mini-column packed with Mg–FeCO 3 LDHs layer coated cellulose fibre particles was incorporated into a sequential...
Sec 2 -containing oligopeptide was synthesized directly from Sec 2 with the traditional liquid phase peptide synthesis without addressing the usually applied and complex solid phase (SPPS) protocol driving through a protected Sec residue and site-oriented oxidation into a diselenide bridge. Effective solubilization of Sec 2 in dimethylformamide and its pH-controlled access...
A simplified speciation method for the determination of selenite, selenate and three selenoaminoacids (selenocystine, selenomethylselenocysteine and selenomethionine) has being developed, based on the coupling of high performance liquid chromatography (HPLC), thermoreduction (TR), hydride generation (HG) and atomic fluorescence spectrometry (AFS). Most of the existing methods based on AFS detection...
The HPLC (anion exchange)–ICP-MS technique was used for the identification (based on retention time of standards) and determination of four selenium species (selenite, selenate, selenomethionine and selenocystine) in plankton (BCR-414), Brazil nuts and urine samples. A recovery of 91% was attained for certified reference materials (BCR-414). Se(IV) was the predominant species in plankton, with the...
A novel method based on dispersive liquid liquid microextraction (DLLME) followed by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) determination was proposed for the speciation of inorganic selenium by using 5-mercapto-3-phenyl-1,3,4-thiadiazole-2-thione potassium salt (Bismuthiol II) as both chelating reagent and chemical modifier. In this method, 500μL ethanol...
Being common in chromatographic techniques internal standard method is rarely applied in electrochemical stripping determinations. One of the reasons for such rare use of this elegant quantification method is because optimal conditions of accumulation at the electrode for individual compounds producing a reproducible signal may vary significantly. These criteria are much stricter when selenium is...
A method for the simultaneous determination of Co, Cu, Pb and Se in crude oil, gasoline and diesel samples using emulsion-based sampling and GF AAS is proposed. 400mg of sample was weighted in volumetric flask following the sequential addition of 125µL of hexane and 7.5mL of Triton X-100 ® (20% mv −1 ). Subsequently, the mixture was stirred in ultrasonic bath, during 30min, before...
In this work the possibility of determination of selenium in water samples was studied by on-line coupling of electrochemical pre-concentration flow through unit and GFAAS. The pre-concentration unit was created from a commercial electrochemical flow through analyser EcaFlow (Istran Ltd.) and a special two-electrode electrochemical flow through cell. The pre-concentration cell consisted of a working...
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