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EN
The popular pharmaceutical base used in pharmacy – vaselinum flavum – was studied by an X-band (9.3 GHz) EPR spectrometer in the range of microwave power of 2.2–70 mW. The samples were sterilized in hot air oven at temperatures: 160°C (120 min), 170°C (60 min), and 180°C (30 min). The aim of this work was to determine properties and free radical concentrations in vaselinum flavum thermally sterilized at different conditions. The changes in free radical system in vaselinum flavum during storage were analyzed. Free radicals were found in all the heated samples. The lowest free radical concentration was obtained for vaselinum flavum heated at 180°C for 30 min; so these parameters are proposed for the thermal sterilization of this pharmaceutical base. Interactions with oxygen decreased free radical concentration in vaselinum flavum during storage. Strong quenching of free radicals in vaselinum flavum was observed after 2 days for the samples sterilized at temperatures 160 and 180°C. Such an effect for vaselinum flavum heated at temperature 170°C was observed later, 13 days after sterilization. Fast spin-lattice relaxation processes exist in thermally sterilized vaselinum flavum. The EPR lines of heated vaselinum flavum were homogeneously broadened. EPR spectroscopy and its use for examining the thermal sterilization process in pharmacy was confirmed.
EN
Free radicals formed during thermal sterilization of eucerinum anhydricum – the pharmaceutical base were examined by an X-band (9.3 GHz) spectrometer. Eucerinum anhydricum was sterilized at different physical conditions according to the Polish Pharmacopeia norms. The samples were heated at temperatures: 160°C (120 min), 170°C (60 min), and 180°C (30 min). The aim of this study is to compare free radical concentration and effect of microwave power on EPR spectra of eucerinum anhydricum base thermally sterilized at different temperatures and periods of time. The effect of time storage on the free radicals in the heated samples was tested. Free radical concentrations in the sample stored 15 min strongly decreased with the increasing of sterilization temperature, probably as the result of recombination. Storage caused strong decrease of free radical concentrations in the samples, probably as the result of interactions with oxygen. It was observed to be independent of sterilization conditions from 2 days of storage and longer. Because of the lowest free radical concentration, for eucerinum anhydricum thermal sterilization at 180°C for 30 min is recommended. The sterilized samples should be stored at inert atmosphere without oxygen molecules. Fast spin-lattice relaxation processes existed in sterilized eucerinum anhydricum. The character of changes of amplitudes and linewidths of EPR lines with increasing of microwave power was the same for different storage times. The parameters of thermal sterilization and storage time influenced free radical concentration in eucerinum anhydricum, but magnetic spin-lattice interactions were unchanged. The usefulness of EPR spectroscopy in optimization of thermal sterilization process of eucerinum anhydricum was confirmed.
EN
Free radicals formation in thermally sterilized famotidine was studied by the use of an X-band (9.3 GHz) electron paramagnetic resonance (EPR) spectroscopy. The influence of temperature and time of sterilization on free radicals generated in famotidine was determined. The best sterilization conditions for the tested drug were found. Sterilization was done according to the pharmaceutical norms at temperatures 160°C (120 min), 170°C (60 min), and 180°C (30 min). It was pointed out that the optimal temperature of thermal sterilization for famotidine was 170°C and time of heating 60 min in this conditions the lowest free radicals concentration was found. The highest free radicals concentration was measured in famotidine heated at 160°C during 120 min, the long time of sterilization is responsible for this effect. Free radicals concentration changes during storage of famotidine after thermal sterilization. Its value increased with storage time for the drug sterilized at both temperatures of 170°C and 180°C. Free radicals concentration decreases from 7 days after sterilization. Complex system of free radicals with the shape of EPR lines, dependent on microwave power exist in thermally sterilized famotidine. Slow spin-lattice relaxation processes, strong dipolar interactions characterize thermally sterilized famotidine. Microwave saturation indicates that EPR lines of famotidine are homogeneously broadened. The usefulness of EPR spectroscopy to examine of the sterilized drugs was evaluated.
EN
Electron paramagnetic resonance spectroscopy at X-band (9.3 GHz) is used as the tool of optimalization of storage of thermally sterilized aminoglycoside antibiotic - streptomycin. Thermal sterilization at different conditions was performed according to the norms. Changes in free radicals system of this drug during storage after sterilization were detected. Lineshape analysis and microwave saturation of EPR spectra were done. Free radical concentrations were determined. Microwave saturation EPR analysis is proposed as useful method to determine the best conditions of storage of sterilized drugs.
5
Content available Wolne rodniki w sterylizowanym termicznie verapamilu
PL
Zbadano generowanie wolnych rodników w werapamilu podczas sterylizacji termiczne w temperaturze 180 stopni C. Koncentrację i właściwości wolnych rodników analizowano z zastosowaniem spektroskopii elektronowego rezonansu paramagnetycznego (EPR) na pasmo X (9.3 GHz). Wykazano, że w procesie sterylizacji termicznej powstają w werapamilu stabilne wolne rodniki. Wolne procesy relaksacji spin-sieć oraz silne oddziaływania dipolowe występują w werapamilu. Badania metodą EPR wykazały, że sterylizacja wysokotemperaturowa nie jest zalecana dla werapamilu.
EN
Free radical formation in verapamil during thermal sterilization at temperature 180 degrees of C was studied. Concentration and properties of free radicals were examined by the use of electron paramagnetic resonance (EPR) spectroscopy at X-band (9.3GHz). It was stated that stable free radicals are formed during thermal sterilization of verapamil. Slow spin-lattice relaxation processes and strong dipolar interactions exist in verapamil.EPR studies showed that sterilization at high temperature is not recommended for verapamil.
PL
Sterylność substancji leczniczej jest niezwykle istot-na z punktu widzenia bezpieczeństwa farmakoterapii. Sterylizacja leków może powodować powstawanie wolnych rodników. Porównano właściwości wolnych rodników powstających pod wpływem promieniowania termicznego (180°C/30 minut) i promieniowania gamma (25kGy) w streptomycynie. Badania prze-prowadzono przy użyciu techniki elektronowego rezonansu paramagnetycznego EPR na pasmo X. Zarówno dla próbek sterylizowanych termicznie jak i radiacyjnie zarejestrowano szerokie linie EPR. Obydwie metody sterylizacji prowadzą do powstania wysokich koncentracji wolnych rodników (1016–1018 spin/g). Porównanie parametrów linii EPR dla sterylizacji termicznej i radiacyjnej wskazuje na podobne właściwości wolnych rodników w sterylizowanej próbce – niesparowane elektrony zlokalizowane na atomie tlenu. Więcej wolnych rodników, w przypadku zastosowanych parametrów sterylizacji, powstaje w próbkach sterylizowanych radiacyjnie.
EN
Sterility of medical substances plays significant role from the point of view of pharmacotherapy safety. Drugs sterilization can cause free radicals forming. It was compared free radicals properties forming in streptomycin under the influence thermal radiation (180°C/30 minutes) and gamma radiation (25kGy). Presented studies were performed by use of X band electron paramagnetic spectrometer. Both for thermal sterilized samples as well as for radiosterilized broad EPR lines were recorded. Both methods of sterilization lead to forming of high concentrations of free radicals (1016–1018spin/g). Comparing of EPR lines parameters for thermal sterilization and radiosterilization point at similar free radicals properties in the studied samples – unpaired electrons located on oxygen atoms. More free radicals, in case of used sterilization parameters, create in radiosterilized samples.
PL
Zbadano zmiany struktury chemicznej oraz generowanie wolnych rodników w ampicylinie podczas sterylizacji w temperaturach 160 stopni C, 170 stopni C i 180 stopni C. Jako metody badawcze zastosowano spektroskopię FT-IR i EPR.. Wykazano, że sterylizacja w temperaturach od 160 stopni C do 180 stopni C powadzi do zmian struktury chemicznej ampicyliny oraz powoduje powstawanie dużej ilości wolnych rodników w próbce. Widma FT-IR uwidaczniają częściową degradację grupy karboksylowej w trakcie ogrzewania leku. Zależność kształtu widm EPR od mocy mikrofalowej wskazuje na złożony charakter układu centrów paramagnetycznych sterylizowanej ampicyliny.
EN
Changes of chemical structure and formation of free radicals in ampicyline during sterilization at temperatures 160 degrees of C, 170 degrees of C, and 180 degrees of C were studied. FT-IR and EPR were applied as experimental methods. It was proved that sterilization at temperatures from 160 degrees of C to 180 degrees of C lead to changes of chemical structure of the ampicyline and causes formation of high amount of free radicals. FT-IR spectra show that carboxyl groups are partly evolved during heating of this drug. Dependence of lineshape of EPR spectra on microwave power indicates complex character of paramagnetic centers system of ampicyline.
9
Content available remote Badanie systemu ręcznego sterowania procesem pasteryzacji przepływowej
PL
Przedstawiono wyniki badań procesu pasteryzacji prowadzonego z wykorzystaniem ręcznego systemu sterowania. Scharakteryzowano przedmiot badań, który stanowił pasteryzator Bełżyce typ "JE". Badania dotyczyły wpływu ręcznego systemu sterowania na poprawność prowadzenia tego procesu. Obejmowały pomiary podczas pasteryzacji takich wielkości, jak: temperatura wina w procesie wyjaławiania i na wyjściu z pasteryzatora, ciśnienie wina w pasteryzatorze. Uzyskane wyniki badań wskazały na nieprawidłowości prowadzenia tego procesu, wynikające z niedokładnego sterowania zaworem przepuszczającym ogrzaną parę wodną do wymiennika. Docelowo mają za zadanie określić rzędy wielkości niezbęnych parametrów w procesie symulacji pracy modelowanego automatycznego systemu sterowania.
EN
Paper presented the results of testing the pasteurization process operated with the use of manual control system. The pasteurizer of Bełżyce JE type used for tests was characterized. The investigations referred to the effect of applied manual control system on the correctness of pasteurization course. Following parameters were measured during pasteurization: wine temperature - during heat treatment and at the outflow from pasteurizer, the pressure of wine in the pasteurizer. Obtained results showed some irregularities in the course of this process arisen from inaccurate control of the volve supplying heated steam to the heat exchanger. The final task of experiments was to determine the magnitudes of parameters necessary to simulate the operation of model automatic control system.
10
Content available remote Modele matematyczne procesu sterylizacji termicznej mediów w przepływie
PL
W pracy dokonano przeglądu opisanych w literaturze modeli matematycznych procesu sterylizacji termicznej mediów. Analiza danych literaturowych wskazuje, że w dalszym ciągu wielu autorów opisuje przebieg procesu destrukcji termicznej drobnoustrojów reakcją I-go rzędu. Takie założenie jest dopuszczalne przy analizie procesu sterylizacji okresowej, ale doprowadza do błędnych wniosków przy analizie procesu ciągłego. W tym przypadku powinno się zastosować jeden z modeli sekwencyjnych tzn. Shull'a czy Sapru. Jednakże istniejące między tymi modelami rozbieżności oraz brak współczynników kinetycznych uzasadniają celowość prowadzenia dalszych badań.
EN
The paper presents a survey of mathematical models of thermal sterilization of media described in the literature. The analysis of literature data shows that still many authors describe the process of thermal destruction of microorganisms by the 1st order reaction. Such an assumption is admissible when batch sterilization is analyzed but leads to erroneous conclusions when analyzing a continuous process. In this case one of the sequential models, i.e. the one proposed by Shull or Sapru should be used. However, discrepancies between these models and lack of kinetic coefficients justify the necessity of further research.
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