Development of an extraction procedure and analysis of electrostatically stabilized silanates from aqueous solutions

2020 ◽  
Vol 49 (3) ◽  
pp. 247-254
Author(s):  
Joanna Jabłońska ◽  
Mariusz Kluska ◽  
Nikolai Erchak ◽  
Stanisław Popiel

AbstractThe analyzed organosilicon derivatives of electrostatically stabilized silanates belong to a group of pentacoordinated compounds. These derivatives are: 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at, 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxa-4-methylcyclopentan-3-on)at, 1-(N-morpholiniomethyl) spirobi(1-sila-2,5-dioxa-4-(i-propyl)cyclopentan-3-on)at.In the course of the work, the extraction process and optimization of conditions for separation and determination of a mixture of electrostatically stabilized silanates were carried out using capillary isotachophoresis. Proper leading electrolytes were elaborated developed and the terminating electrolyte: 4,4’-bis[(1-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at] was proposed. The extraction process involved the use of three stationary phases: octadecyl, octyl and phenylpropyl. The highest recovery values, approx. 94%, were obtained on the phenylpropyl column. The optimum time of analysis by the isotachophoretic technique did not exceed 12 min. The developed method of separation and determination of electrostatically stabilized silanates expands the possibility of research on biological activity of this group of compounds in aqueous solutions and surface water vegetation.

2017 ◽  
Vol 1141 ◽  
pp. 39-43 ◽  
Author(s):  
A.M. Maharramov ◽  
M.A. Ramazanov ◽  
G.A. Guliyeva ◽  
A.E. Huseynzada ◽  
U.A. Hasanova ◽  
...  

2012 ◽  
Vol 1269 ◽  
pp. 143-153 ◽  
Author(s):  
Carla Fernandes ◽  
Pedro Brandão ◽  
Alexandre Santos ◽  
Maria Elizabeth Tiritan ◽  
Carlos Afonso ◽  
...  

1995 ◽  
Vol 78 (2) ◽  
pp. 437-444 ◽  
Author(s):  
Hesg-Biu Lee ◽  
Thomas E Peart ◽  
Arthur J Niimi ◽  
Charles R Knipe

Abstract An efficient and environmentally friendly supercritical fluid extraction (SFE) method for the determination of naturally contaminated polychlorinated biphenyls (PCBs) in fish tissues is described. The effect of various SFE conditions on lipid content and PCB recovery in fish extracts was studied. Optimal conditions for PCB extraction were nonmodified carbon dioxide at 100°C, pressure of 5000 psi, and flow rate of 2.5 mL/min. Recoveries of PCBs were ≥95% for both naturally contaminated and spiked fish, and this extraction procedure required less than 40 min per sample. By incorporating activated basic alumina with the sample in the extraction process, fish lipid was selectively retained by the adsorbent. The lipid content in the SFE extract varied from <0.1% to 2.2% for the fish samples tested, including those samples with over 30% lipid by weight. In most cases, the remaining lipid was conveniently removed from PCBs by a down-sized Florisil column cleanup. The commonly found chlorinated insecticides, hexachlorobenzene, p,p′-DDE, and mirex were also extracted and determined simultaneously with PCBs.


2019 ◽  
Vol 2019 ◽  
pp. 1-5
Author(s):  
Sergei Yu. Zaitsev ◽  
Marina S. Tsarkova ◽  
Ilia S. Zaitsev

The design of polymeric composite materials (PCM) for the optical control of chemical substances is currently one of the actively developing fields of science “at the junction” of polymer, organic, and analytical chemistry. The purpose of this work is the preparation of PCM containing derivatives of crown ethers for the optical determination of barium ions. The polymeric composite materials containing a novel optical molecular sensor have been obtained and investigated on the basis of a number of film-forming polymers. The best results have been obtained for PCM based on polyvinyl butyral films (since the fluorescence and absorption maxima shifted by 9 and 16 nm, respectively) in the fluorescence and absorption spectra of this PCM in the presence of barium ions. This makes the proposed PCM highly promising as sensor elements for the detection of the barium ions in the aqueous solutions.


1991 ◽  
Vol 74 (6) ◽  
pp. 932-939
Author(s):  
Alain Quinsac ◽  
Daniel Ribaillier ◽  
Claire Elfakir ◽  
Michel Lafosse ◽  
Michel Dreux

Abstract Liquid chromatographic (LC) analysis of desulfated derivatives of rapeseed glucosinolates has been carried out under isocratic elution conditions with different CN-bonded stationary phases. The effects of the eluant composition (water, acetonitrile, and methanol) with the stationary phase (Zorbax CN, Lichrospher CN, and Ultrasphere CN) and temperature (20 and 50°C) are described. An isocratic LC method performed at room temperature using a Lichrospher CN column and water as mobile phase is proposed. The chromatographic analysis can be done in less than 12 min, and it is easier and less expensive than the traditional gradient mode. Four commercial samples of rapeseed containing various quantities of other cruciferous seeds (wild mustard and stinkweed) as an admixture have been analyzed to determine the total giucosinolate content. Relative standard deviations of repeatability of the isocratic and gradient LC methods ranged from 0.4 to 1.7% and from 2.7 to 4.7%, respectively. Comparison of the results showed good agreement between the 2 methods (better than 98%).


2019 ◽  
Vol 15 (5) ◽  
pp. 528-534
Author(s):  
Asiye Aslıhan Avan ◽  
Hayati Filik

Background: Monitoring of DA, in the presence of other chemical analogues such as epinephrine, norepinephrine, serotonin, ascorbic acid, uric acid, catechol, phenethylamine, tyramine, and tyrosine, is crucial in the diagnosis and mechanistic understanding of human neuropathology. Therefore, the determination of DA at trace levels has become a very important analytical task, as part of health safety and forensic analysis. Introduction: A cloud point extraction (CPE) process was developed for the isolation and detection of dopamine in food, urine, and pharmaceutical samples. Methods: In this procedure, dopamine was derivatized with o-phthalaldehyde (OPA) and sodium sulphite in aqueous solution. The isoindole derivative was synthesized by the reaction of OPA and sodium sulphite with the amino group of dopamine and the resulted isoindole derivatives were extracted by cloud point extraction. After extraction process, the concentration of enriched analyte was measured by UV-VIS spectrophotometry. The parameters affecting the CPE such as concentration of surfactant and electrolyte, equilibration temperature and time and pH of sample solution were investigated. Results: After optimization of the CPE conditions, the linear range of 8-80 µM (without extraction 100- 1000 µM) was established for dopamine with detection limit at 2.6 µM. Conclusion: The developed extraction procedure was applied to the quantification of dopamine in chocolate, urine, and pharmaceutical samples. The study ensures a promising strategy for the detection of dopamine in the presence of biological constituents, e.g. ascorbic acid, uric acid, and serotonin.


Author(s):  
Sylwia Kowalska ◽  
Edward Szłyk ◽  
Aneta Jastrzębska

AbstractThe simple extraction of flours samples followed by free amino acids determination procedures was studied and optimised. The conditions of amino acids derivatisation reaction with ninhydrin for chromatographic determination of free amino acids sum was discussed. The developed method was processed in terms of linearity, precision, accuracy, and limits of detection and quantification. Moreover, capillary isotachophoresis and HPLC methods were applied for individual free amino acids determination. The proposed extraction procedure is simple, fast and convenient for different flours samples. Studied procedures were used for free amino acids determination in twelve gluten-free flour samples (corn, oat, soy, rice, pumpkin, millet, peanut, hemp seed, buckwheat, amaranth, pea and chickpea) and the obtained results were compared with wheat flour.


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