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Hollow-fibre Based Microextraction and Voltammetric Determination of Vanillylmandelic Acid
Hrdlička, Vojtěch ; Barek, J. ; Navrátil, Tomáš
New method of liquid/liquid/liquid hollow fibre based microextraction of vanillylmandelic acid coupled with voltammetric determination is being developed. Selected liquid membranes based on alcohols, aliphatic hydrocarbons and esters were tested. Highest enrichment factor of 2.52 after 30 minutes of extraction was obtained using propyl benzoate, RSD = 18.2 % (n=5). Mechanically and cathodically pretreated (-1000 mV vs. Ag/AgCl/3M KCl, 15 s) boron doped diamond electrode in a miniaturized arrangement was used for DPV determination. LOD = 1.2 micromol/l, RSD = 5.9% (n=10) for a 10 microl extract.
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HPLC-ED/UV with Solid Phase Extraction for the Determination of 5-Hydroxyindole-3-acetic Acid
Němečková-Makrlíková, Anna ; Dejmková, H. ; Navrátil, Tomáš ; Barek, J. ; Vyskočil, V.
Determination of 5-HIAA in human urine was successfully performed using HPLC-ED/UV with SPE. HPLC-ED is a very sensitive technique, presented method does not need any sample pre-treatment apart from SPE procedure, which replaced filtration of samples of human urine to avoid problems with clogging a HPLC column. The found native\nconcentrations of 5-HIAA in human urine using HPLC-ED with SPE fully corresponds with published normal concentrations in urine (17.8 - 58.3 micromol l-1). The found native concentrations of 5-HIAA were 18.4 micromol L-1 (calculated from peak height). The presented method is fast and could be used for simple\nscreening of human urine, because HPLC-ED/UV allows simultaneous determination of 5-HIAA, HVA, and VMA as important tumour biomarkers.
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Electrochemical Measurements in Flow Systems on Silver Amalgam Tubular Detector Combined with Auxiliary Electrode
Josypčuk, Bohdan ; Barek, J. ; Josypčuk, Oksana
A new type of tubular detector (TD+AuxE) was proposed, fabricated, tested and compared\nwith a typical silver amalgam tubular detector developed earlier. Non-stop-flow differential\npulse voltammetric anodic stripping method (AS-DPV) and amperometric method in a\nglucose oxidase biosensor arrangement were tested. Both detectors were applied for AS-DPV\nmeasurements in flow systems for the first time. The proposed combination of tubular\ndetector with auxiliary electrode provides a much greater current response than the classic\narrangement with three individual electrodes. All relevant parameters (potentials of\naccumulation or detection, flow rate, analyte concentrations, shielding sleeve length, etc.)\nwere optimized for the developed TD+AuxE.
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