Browsing by Author "Naskrent, Marek"
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Item Radiation sterilization of ephedrine in the solid state(Polish Chemical Society and the Committee on Analytical Chemistry of Polish Academy of Sciences with cooperation of the Czech Chemical Society, the Slovak Chemical Society and the Hungarian Chemical Society, 2008) Dettlaff, Katarzyna; Teżyk, Artur; Marciniec, Barbara; Wachowiak, Roman; Naskrent, Marek; Bednarek, BartłomiejThe effects of the e-beam ionising radiation of energy 9.96 MeV in doses 25 800 kGy on the stability of solid ephedrine hydrochloride (1R,2S)-(-)-2-methylamino-1-phenyl-1-propanol hydrochloride) have been studied. These effects have been observed using the following analytical methods: organoleptic (form, colour, smell, clarity of solution), scanning electron microscope SEM, pH measurement, chirality and water content measurement (Karl Fischer method), spectrometric methods (UV, FT IR, EPR), chromatography (TLC), and combined chromatography (TLC UV, GC MS). Even the standard sterilisation dose of 25 kGy has been found to cause a change in colour from white to pale yellow, the appearance of free radicals in the concentration of 3.05×10^15 spin/g, and about 1% loss of the content. The effects of higher doses 50 800 kGy have shown that radiodegradation degree of the compound is proportional to the dose applied. The main product of radiodegradation, formed at a yield of G = 17.17×10^7 mol/J, has been identified as 2-methylamino-1 phenyl-1-propanone (methcathinone, ephedrone), a psychoactive compound of the activity similar to that of amphetamine. For the above reasons ephedrine hydrochloride can not be subjected to radiative sterilisation with a dose of 25 kGy, however, assuming sufficiently low microbiological contamination of the initial substance, lower doses could be probably used for sterilisation purposes. Our results have not confirmed the earlier reports from 1970s on the resistance of ephedrine to ionising radiation in doses up to 60 kGy.Item The effect of ionizing radiation on chloramphenicol(Springer Netherlands, 2006) Marciniec, Barbara; Stawny, Maciej; Kozak, Maciej; Naskrent, MarekThe effect of ionizing radiation on the physicochemical properties of chloramphenicol in solid state has been studied. The compound was e-beam irradiated with doses from the range 25–400 kGy and the possible changes were detected in the organoleptic methods (colour, form, odour, solubility and clarity), by SEM observations, X-ray, chromatography (TLC), spectrophotometry (UV, IR, EPR) and thermal (DSC) methods. No significant changes relative to the unirradiated sample were observed as a result of irradiation with the dose of 25 kGy – a standard dose for radiation sterilization, besides free radicals generation. Higher doses were found to produce a change in colour, increase in absorbance (UV), changes in the XRD spectra and appearance of products of radiolysis. The presence of the radiolysis products was confirmed by the TLC method, indirectly by DSC showing a decrease in the melting point from 0.2 to 4.5°C and enthalpy from 3.8 to 23.3 J g–1, respectively. A linear relationship was obtained between the irradiation dose (25–400 kGy) and the melting point of chloramphenicol, characterised by the correlation coefficient r=0.9968. The EPR signal intensity increased with increasing dose of irradiation and the lifetime of the free radicals was longer than 6 months. No changes were detected in SEM and IR spectra. As follows from our results, the DSC method is most suitable for a fast monitoring of the drugs subjected to sterilization by irradiation as it permits detection of changes occurring even on irradiation with low doses and their quantitative description.Item Thermal study of four irradiated imidazoline derivatives in solid state(Springer Netherlands, 2007) Marciniec, Barbara; Kozak, Maciej; Naskrent, Marek; Dettlaff, Katarzyna; Ogrodowczyk, Magdalena; Stawny, Maciej; Wachowski, LeszekFour imidazoline derivatives: antazoline (AN), naphazoline (NN), tymazoline (TM), xylometazoline (XM), in the form of hydrochlorides in solid phase have been subjected to high energy e-beam irradiation from an accelerator (10 MeV) at a dose varied from 25 to 200 kGy. The effects of the irradiation have been assessed by DSC, X-ray diffraction, FTIR, EPR and TLC. The standard sterilisation dose of 25 kGy has been found to produce changes in the properties of one derivative (XM), two other ones (AN and TM) have been found sensitive to doses >100 kGy, whereas NN has been resistant to irradiation in the whole range studied (25–200 kGy). EPR results indicated that the changes taking place in the therapeutic substances studied are related to radical formation. The irradiation induced changes in colour, a decrease or increase in the melting point, changes in the XRD pattern, small changes in the shape of FTIR peaks and the presence of radiolysis products. The XM compounds cannot be sterilised by irradiation because of the radiation induced changes in its physico-chemical properties.