- Publikační typ
- abstrakt z konference MeSH
A method has been developed for the determination of iodide in mineral water, seawater, cooking salt, serum, and urine based on hyphenation of capillary ITP and zone electrophoresis. A commercially available instrumentation for capillary ITP with column-switching system was used. ITP served for removal of chloride present in the analyzed samples in a ratio of 10(6)-10(7):1 to iodide, zone electrophoresis was used for evaluation. Isotachophoretic separation proceeded in a capillary made of fluorinated ethylene-propylene copolymer of 0.8 mm id and 90 mm total length to the bifurcation point filled with a leading electrolyte (LE) composed of 8 mM HCl + 16 mM beta-alanine (beta-Ala) + 10% PVP + 2.86 mM N(2)H(4)x2HCl, pH 3.2; and a terminating electrolyte composed of 8 mM H(3)PO(4) + 16 mM beta-Ala + 10% PVP + 5 mM N(2)H(4), pH 3.85 for all the matrices except seawater. For ITP of seawater the LE consisted of 50 mM HCl + 100 mM beta-Ala + 10% PVP + 2.86 mM N(2)H(4)x2HCl, pH 3.52. Distance of conductivity detector from the injection point and bifurcation point was 52 and 38 mm, respectively. Zone electrophoresis was performed in a capillary made of fused silica of 0.3 mm id and 160 mm total length filled with LE from isotachophoretic step. LODs reached for all matrices were 2-3x10(-8) M concentration (2.5-4 microg/L) enabled monitoring of iodide in all analyzed samples with RSD 0.4-9.3%. Estimated concentrations of iodide in individual matrices were 10(-6)-10(-8) M.
The on-line combination of capillary zone electrophoresis (CZE) with capillary isotachophoresis (ITP) increases significantly the separation capability and sensitivity of capillary electrophoresis. This technique was used for separation and quantification of fourteen selected natural constituents in red wine belonging to flavonoids and phenolic acids. The leading electrolyte (LE) in the ITP pre-separation step was 10 mM HCl of pH* 7.2 with Tris as counterion, the terminating electrolyte (TE) was 50 mM boric acid of pH* 8.2 (adjusted with barium hydroxide). The background electrolyte in the electrophoretic step contained 25 mM beta-hydroxy-4-morpholinopropanesulfonic acid (MOPSO), 50 mM Tris, 15 mM boric acid and 5 mM beta-cyclodextrin of pH* 8.5. The content of methanol in all electrolytes was 20% (v/v). For exact timing of the transfer of isotachophoretically stacked analyte zones into the CZE column and for the control of the residual amount of leading and terminating ITP electrolytes picric acid was used as coloured marker. The R.S.D. values (n = 6) ranged between approximately 0.1% (for 0.25 microg ml(-1) rutin) and approximately 11% (for 0.25 microg ml(-1) of quercitrin). Detection limits were 30 ng mi(-1) for phenolic acids, quercitrin and rutin, 100 ng ml(-1) for quercetin, kaempferol and epicatechin and 250 ng ml(-1) for catechin. A single analysis took 45 min.
Závěrečná zpráva o řešení grantu Interní grantové agentury MZ ČR
61 l. : tab. ; 32 cm
Development and validation of original analytical methods based on electrophoretic phenomana /ITP,CZE,tandem ITP-CZE technique/. Intendent for separation,identification and determination of oharmaceutically important compounds in various dosage forms andin herbal drugs.
Vypracování a validace původních metod na elektroforetickém principu /ITP, CZE, tandem ITP-CZE/ pro separaci, inentifikaci a stanovení farmaceuticky důležitých látek chemického a rostlinného původu.
- Konspekt
- Lékařské vědy. Lékařství
- NLK Obory
- farmacie a farmakologie
- chemie, klinická chemie
- NLK Publikační typ
- závěrečné zprávy o řešení grantu IGA MZ ČR
