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Open access

Magdalena Zdybel and Barbara Pilawa

Abstract

Free radicals in synthetic melanin and melanin from Sepia officinalis were studied by electron paramagnetic resonance (EPR) spectroscopy. The effect of time of ultraviolet (UV) irradiation on free radicals in these melanins was tested. The samples were exposed to UV during 15, 30, and 60 minutes. EPR spectra were measured with microwaves from an X-band (9.3 GHz) in the range of microwave power of 2.2–70 mW. The performed EPR examinations indicate that high concentrations (~1021–1022 spin/g) of o-semiquinone free radicals with g factors of 2.0039–2.0045 exist in all the tested samples. For nonirradiated samples, free radical concentration was higher in natural melanin than in synthetic melanin. UV irradiation caused the increase of free radical concentrations in synthetic melanin samples and this effect depends on the time of irradiation. The largest free radical formation in the both melanins was obtained for 60 min of UV irradiation. Free radical concentrations after the UV irradiation of melanins during 30 min were lower than during irradiation by 15 min, and probably this effect was the result of recombination of the radiatively formed free radicals. EPR lines of the tested samples broadened with increasing microwave power, so these lines were homogeneously broadened. The two types of melanins differed in the time of spin-lattice relaxation processes. Slower spin-lattice relaxation processes exist in melanin from Sepia officinalis than in synthetic melanin. UV irradiation did not change the time of spin-lattice relaxation processes in the tested melanins. The performed studies confirmed the usefulness of EPR spectroscopy in cosmetology and medicine.

Open access

Anna Rzepecka-Stojko, Barbara Pilawa, Paweł Ramos and Jerzy Stojko

Antioxidative Properties of Bee Pollen Extracts Examined by EPR Spectroscopy

Bee pollen is a valuable and highly recognized source of exogenous antioxidants. The aim of these studies was to determine the antioxidant capacity of three types of bee pollen extracts: ethanol extracts of bee pollen, pepsin extracts of bee pollen and ethanol extracts of pepsin-digested bee pollen. Their antioxidant properties were determined with the use of electron paramagnetic resonance (EPR) and their ability to quench DPPH free radicals was estimated. The EPR results showed that ethanol extracts of pepsin-digested bee pollen (EEPP) had the highest antioxidative effect and the highest free radical DPPH scavenging potential. The pepsin extracts of bee pollen (PEP) had the weakest antioxidant capacity. The ability to quench DPPH free radicals was also the weakest one for this extract. An average antioxidative effect was recorded for ethanol extracts of bee pollen (EEP).

Open access

Jakub Adamczyk, Paweł Ramos and Barbara Pilawa

Abstract

Paramagnetic centers in the two exemplary synthetic and natural dental biocompatible materials applied in implantology were examined by the use of an X-band (9.3 GHz) electron paramagnetic resonance (EPR) spectroscopy. The EPR spectra were measured in the range of microwave power 2.2–70 mW. The aims of this work were to compare paramagnetic centers concentrations in different dental biocompatible materials and to determine the effect of microwave power on parameters of their EPR spectra. It is the very first and innovatory examination of paramagnetic centers in these materials. It was pointed out that paramagnetic centers existed in both natural (~1018 spin/g) and synthetic (~1019 spin/g) dental biocompatible materials, but the lower free radical concentration characterized the natural sample. Continuous microwave saturation of EPR spectra indicated that faster spin-lattice relaxation processes existed in synthetic dental biocompatible materials than in natural material. Linewidths (ΔB pp) of the EPR spectra of the natural dental material slightly increased for the higher microwave powers. Such effect was not observed for the synthetic material. The broad EPR lines (ΔB pp): 2.4 mT, 3.9 mT, were measured for the natural and synthetic dental materials, respectively. Probably strong dipolar interactions between paramagnetic centers in the studied samples may be responsible for their line broadening. EPR spectroscopy is the useful experimental method in the examination of paramagnetic centers in dental biocompatible materials.

Open access

Paweł Ramos, Piotr Pepliński and Barbara Pilawa

Abstract

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.

Open access

Paweł Ramos and Barbara Pilawa

Abstract

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.

Open access

Magdalena Zdybel, Barbara Pilawa, Ewa Buszman, Dorota Wrzesniok, Ryszard Krzyminiewski and Zdzislaw Kruczynski

Continuous microwave saturation of EPR spectra of melanin complexes at different temperatures

Paramagnetic centers in DOPA-melanin and complexes of DOPA-melanin with netilmicin and Cu(II) were studied by the use of an X-band (9.3 GHz) electron paramagnetic resonance (EPR) spectroscopy. Measurements of continuous microwave saturation of EPR spectra at temperatures: 125 K, 175 K, 225 K, 275 K, were performed. Homogeneous broadening of all the examined EPR spectra was observed. EPR spectra of DOPA-melanin-Cu(II) complexes saturated at higher microwave powers than the others tested melanin samples. Fast spin-lattice relaxation exists in DOPA-melanin-Cu(II) complexes. Slow spin-lattice relaxation processes exist in melanin's paramagnetic centers of DOPA-melanin and its complexes with netilmicin, and its complexes with both netilimicin and Cu(II). EPR spectra of all the tested samples saturated at higher microwave powers with increasing of the measuring temperature. Faster spin-lattice relaxation processes occurs in DOPA-melanin and its complexes with netilmicin and Cu(II) at higher temperature.