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Determination of pindolol by sequential injection analysis with chemiluminescence detection
Havelková, Jana ; Polášek, Miroslav (advisor) ; Pospíšilová, Marie (referee)
The oxidation of the drug pindolol, [1-(indol-4-yloxy)-3-(isopropylamino)-2-propanol (I)] by permanganate in the medium of aqueous H2SO4 is accompanied by the emission of chemiluminescence (CL) radiation. The CL signal is enhanced by hexametaphosphate. This CL reaction was used for devising automated sequential injection analysis (SIA) assay of I in pharmaceutical preparations. The PC-controlled SIA setup consisted of a Cavro XL 3000 2.5- ml syringe pump, Vici-Valco 10-port selection valve and Spectra-Physics FS970 flow- through fluorescence detector equipped with a lab-made CL detection module. The net CL signal of I increased by a factor of 4.4 (compared to purely aqueous test solution of I injected) if the test solution contained 80% (v/v) of methanol. Optimal order, concentrations and volumes of aspirated zones of reactants were: 43l of 80mM Na hexametaphosphate, 30 l of I in 80% (v/v) methanol, 28 l of 2M H2SO4 and 1 l of 5mM KMnO4. Calibration curve relating the intensity of CL (peak height) to the concentration of I was linear in the range 1 - 10 M I; the limit of detection (S/N = 3) was 0.15 M I. The sample throughput was 90 h-1 . The repeatability of the peak heights was characterized by RSD 1.8% for 30 replicate injections of 8 M I. The SIA-CL method was used for the assay of I in...

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