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  1. 11 Nukleonika
  2. 5 Engineering of Biomaterials
  3. 4 Bulletin of the Polish Academy of Sciences. Chemistry
  4. 3 Acta Poloniae Pharmaceutica - Drug Research
  5. 3 Annales Academiae Medicae Silesiensis
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  1. 1 2022
  2. 1 2020
  3. 2 2019
  4. 1 2018
  5. 2 2017
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  1. 16 Pilawa B.
  2. 11 Ramos P.
  3. 4 Sadło J.
  4. 3 Sterniczuk M.
  5. 3 Strzelczak G.
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1
Content available EPR examination of free radicals thermally formed in vaselinum flavum
100%
Ramos P. , Pilawa B.
Nukleonika
|
2015
|
tom Vol. 60, No. 3, part 1
443--447
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.
2
Content available Electron paramagnetic resonance studies on silver atoms and clusters in regularly interstratified clay minerals
100%
Yamada H. , Sadlo J. , Tamura K. , Shimomura S. , Turek J. , Michalik J.
Nukleonika
|
2004
|
tom Vol. 49, nr 4
131-136
EN
The formation and stabilization of reduced silver species in the regularly interstratified clay minerals, trioctahedral smectite/chlorite (tri-Sm/Ch) and dioctahedral smectite/mica (di-Sm/M), have been studied by electron paramagnetic resonance (EPR) spectroscopy. Both minerals loaded with Ag+ cations after degassing and dehydration were g-irradiated at 77 K and monitored by EPR as the temperature increased. Some samples were exposed to water or methanol vapor after dehydration. In both hydrated and dehydrated samples only the doublets assigned to Ag0 atoms were observed with no evidence of the formation of Ag clusters. However, the EPR parameters of silver atoms in both matrices are different. In tri-Sm/Ch the narrow anisotropic EPR lines overlap with the broader isotropic lines, whereas in di-Sm/M only broad lines are recorded. The hyperfine splitting - Aiso(Ag0) is larger in tri-Sm/Ch than in di-Sm/M. Also the stability of Ag0 in both clay minerals is distinctly different. Ag0 doublet in di-Sm/M disappears completely above 230 K, whereas in tri-Sm/Ch it is still recorded at 310 K. It is proposed, basing on the EPR results that Ag0 atoms appear at different sites in both matrices: - in tri-Sm/Ch in the middle of smectite interlayer and in hexagonal cavities in the silicate sheets of tetrahedron layer and in di-Sm/M in hexagonal cavities only. When samples had been exposed to methanol before irradiation, the silver clusters become stabilized in the interlayer sites. In tri- Sm/Ch matrix the silver dimer Ag2+ formed by g-irradiation at 77 K is transformed to tetrameric cluster, Ag43+ at 150 K. In di-Sm/M the radiation-induced silver agglomeration proceeds in a similar way, but with a slower rate and Ag tetramer is formed only above 190 K. In both clay minerals, Ag43+ clusters decay above 250 K.
3
Content available remote Spektroskopia EPR w biopomiarach płynności lipidów błonowych
100%
Żakowska I. , Jóźwik K. , Gwoździński K. , Olejniczak J. , Pawlicki L.
Zeszyty Naukowe. Elektryka / Politechnika Łódzka
|
2001
|
tom z. 98
471-475
PL
W referacie przedstawiono metodyką biopomiarów płynności lipidów błonowych metodą spektroskopii elektronowego rezonansu paramagnetycznego (EPR). Zastosowano trzy znaczniki spinowe 5-, 12- oraz kwas 16-doksylostearynowy, które lokują się na różnych głębokościach lipidów błonowych. Wykazano istotny statystycznie (odpowiednio: p < 0,01; p < 0,001) wzrost płynności lipidów błonowych w płytkach krwi pochodzących od osób z chorobą niedokrwienną serca w głębszych regionach łańcucha węglowodorowego kwasu stearynowego.
EN
The methodology of biomeasurements of lipid membrane fluidity using electron paramagnetic resonance (EPR) spectroscopy has been shown. Three spin labelled fatty acids: 5-, 12- and 16-doxylstearic acid, which are located at different depths in the lipid membrane have been used. The blood was taken from ischaemic heart disease (IHD) patients. Results showed a significant increase (p < 0,01; p < 0,001 respectively) in lipid membrane fluidity of human blood platelets in deeper regions of hydrocarbon chains of stearic acid.
4
Content available remote EPR examination of free radicals thermally formed invaselinum flavum
100%
Ramos P. , Pilawa B.
Nukleonika
|
2015
|
tom 60
|
nr 3
443-447
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.
5
Content available THE INFLUENCE OF STORAGE TEMPERATURE AND UV-IRRADIATION ON FREE RADICAL SCAVENGING PROPERTIES OF ETHANOLIC EXTRACTS OF PROPOLIS
88%
Komosińska-Vassev K. , Olczyk P. , Ramos P. , Mencner L. , Derkacz A. , Waluga E. , Krysik K. , Olczyk K. , Pilawa B.
Acta Poloniae Pharmaceutica - Drug Research
|
2018
|
tom 74
|
nr 6
1833-1840
EN
The free radical scavenging activity of ethanolic extracts of propolis (EEP) at the concentrations of 3%, 7%, and 10% was examined. The impact of storage temperature and exposure to ultraviolet (UV) light on the interactions of extracts of propolis with the model DPPH free radicals was also determined. The quenching of an X-band electron paramagnetic resonance spectra of DPPH free radicals by the extracts stored at room temperature, heated at the temperature of 50 oC and exposed to UV-irradiation, were compared. The examined propolis ethanolic extracts revealed an antioxidative character. The storage of the samples at a higher temperature (50 oC) caused a decrease of the scavenging activity equaling to 7% and 10% EEP. UV-irradiation of the 3% EEP increased the quenching of DPPH free radical lines. The reverse effect was observed for the 7% and 10% propolis extracts. The 3% ethanolic extract of propolis is more stable for storage at 50ºC, and less than other analyzed EEP susceptible for UV-irradiation. Alterations of the antioxidative properties of the analyzed EEP and changes in the kinetics of their interactions with free radicals, indicate that 3%, 7%, and 10% propolis extracts should not be exposed to the temperature of 50 oC and UV-irradiation.
6
Content available Effect of UV irradiation on free radicals in synthetic melanin and melanin biopolymer from Sepia offi cinalis : EPR examination
88%
Zdybel M. , Pilawa B.
Nukleonika
|
2015
|
tom Vol. 60, No. 3, part 1
483--488
EN
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.
7
Content available remote Preparation of N-aryl-ketonitrone spin traps
88%
Hassan I. , Lauricella R. , Tuccio B.
Open Chemistry
|
2006
|
tom 4
|
nr 2
338-350
EN
The syntheses of seven N-aryl-C,C-dialkoxycarbonylnitrones 1–7, six of which were original, were achieved from the appropriate aryl-nitroso compounds. These ketonitrones were found to trap efficiently carbon-centred free radicals in aqueous media, yielding stable aminoxyl radicals whose EPR spectra lasted several days. The two penta-deuterated compounds 6 and 7 were also found to be efficient at trapping methoxyl radical. Their various spin adducts showed simple three line signals, very sensitive to the polarity of the environment. This study represents the very first use of linear ketonitrones as spin traps.
8
Content available remote Oxidative stability of the lipid fraction in cookies – the EPR study
88%
Zawada K. , Kozłowska M. , Żbikowska A.
Nukleonika
|
2015
|
tom 60
|
nr 3
469-473
EN
Cookies are a group of convenient food products that are popular among consumers. They may contain high amounts of fats, which can be prone to oxidation. To retard the oxidative deterioration, synthetic and natural antioxidants may be added. Herb and spice extracts can be sources of natural biologically active substances with antioxidant activity. In this work, electron paramagnetic resonance spectroscopy was used to monitor the lipid oxidation in cookies with rosemary and thyme extracts subjected to the storage in elevated temperature. It was shown that thyme extract can be used as a natural antioxidant source for the preparation of bakery products, while the rosemary extract should be used with care in fat-rich products exposed to high temperatures.
9
Content available remote Effect of UV irradiation on free radicals in synthetic melanin and melanin biopolymer fromSepia officinalis– EPR examination
88%
Zdybel M. , Pilawa B.
Nukleonika
|
2015
|
tom 60
|
nr 3
483-488
EN
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.
10
Content available remote Synthesis, characterization and structure of the Bis(methyl-cyclopentadienyl)vanadium(IV) carboxylates
88%
Vinklarek J. , Honzíĉek J. , Císařová I. , Pavliŝta M. , Holubová J.
Open Chemistry
|
2005
|
tom 3
|
nr 1
157-168
EN
The 1,1’-dimethylvanadocene dichloride ((C5H4CH3)2VCl2) reacts in aqueous solution with various carboxylic acids giving two different types of complexes. The 1,1’-dimethylvanadocene complexes of monocarboxylic acids (C5H4CH3)2V(OOCR)2 (R=H,CCl3, CF3, C6H5) contain two monodentate carboxylic ligands, whereas oxalic and malonic acids act as chelate compounds of the formula (C5H4CH3)2V(OOC-A-COO) (A=−, CH2). The structure of the (C5H4CH3)2 V(OOCCF3)2 complex was determined by single crystal X-ray diffraction analysis. The isotropic and anisotropic EPR spectra of all the complexes prepared were recorded. The obtained EPR parameter values were found to be in agreement with proposed structures.
11
Content available Oxidative stability of the lipid fraction in cookies : the EPR study
88%
Zawada K. , Kozłowska M. , Żbikowska A.
Nukleonika
|
2015
|
tom Vol. 60, No. 3, part 1
469--473
EN
Cookies are a group of convenient food products that are popular among consumers. They may contain high amounts of fats, which can be prone to oxidation. To retard the oxidative deterioration, synthetic and natural antioxidants may be added. Herb and spice extracts can be sources of natural biologically active substances with antioxidant activity. In this work, electron paramagnetic resonance spectroscopy was used to monitor the lipid oxidation in cookies with rosemary and thyme extracts subjected to the storage in elevated temperature. It was shown that thyme extract can be used as a natural antioxidant source for the preparation of bakery products, while the rosemary extract should be used with care in fat-rich products exposed to high temperatures.
12
Content available remote Continuous microwave saturation of EPR spectra of melanin complexes at different temperatures
88%
Zdybel M. , Pilawa B. , Buszman E. , Wrzesniok D. , Krzyminiewski R. , Kruczynski Z.
Polish Journal of Medical Physics And Engineering
|
2011
|
tom 17
|
nr 2
85-94
EN
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.
13
Structural and Spectroscopic Characterization of Mixed Ligand Complex: Bis(quinoline-2-carboxylato)bis(imidazole)manganese(II)
88%
Dobrzyńska D. , Jerzykiewicz L. , Jezierska J. , Słoniec E.
Polish Journal of Chemistry
|
2006
|
tom Vol. 80, nr 11
1789-1797
EN
A new complex, [Mn(quin-2-c)2(Him)2] (quin-2-c = quinoline-2-carboxylate ion, Him = imidazole), was synthesized by self assembly and its structure was determined by X-ray analysis. The compound crystallizes in the centrosymmetric space group C2/c with the Mn atom on a twofold axis, a = 18.091(6) Alfa; b = 10.125(4) Alfa; c = 13.708(5) Alfa; Beta= 111.73(3)graduate; V = 2332.5(15) Alfa3 and Z = 4 (T = 100 K). Strong hydrogen bonds between imidazole moieties and carboxylate groups connect themolecules of the complex into the 1D chains extending parallel to the c axis. The interchain contacts of the C-HźźźO, C-HźźźN,piźźźpi and C-Hźźźpi type influence the architecture of the crystal. The complex was characterized by thermal analysis, and by EPR and IR spectroscopy.
14
Content available EPR study of free radicals formed in fusidic acid and neomycin under UV irradiation
75%
Pierzchała E. , Ramos P. , Pilawa B.
Acta Poloniae Pharmaceutica - Drug Research
|
2019
|
tom 76
|
nr 2
215-223
EN
Free radicals in UV irradiated antibiotics used in dermatology were examined. Concentrations of free radicals in fusidic acid and neomycin, were determined. EPR spectra of the tested antibiotics were measured by electron paramagnetic resonance spectrometer with magnetic modulation of 100 kHz and numerical acquisition system the Rapid Scan Unit. The influence of microwave powers in the range of 2.2-70 mW on the spectra was obtained. Amplitudes (A) and linewidths (ΔBpp) of the EPR spectra, were analysed. The EPR spectra were homogeneously broadened. Fast spin-lattice relaxation processes existed in UV irradiated fusidic acid and neomycin, which EPR spectra were not saturated up to 70 mW. The influence of the time of UV irradiation on free radicals in the samples was observed. The samples were irradiated by UVA (315-400 nm) in the 30, 60, and 90 minute period. Free radical concentrations in the tested antibiotics exposed to UV were proportional to the amplitudes (A) of the EPR spectra. The highest amplitudes (A) were observed for the UV irradiated antibiotics during 60 minutes. The higher amplitudes (A) characterized fusidic acid than neomycin. Fusidic acid and neomycin used to treat bacterial infection of skin under UV irradiation may produce free radical toxic effects. The stronger photosensitivity characterized fusidic acid relatively to neomycin. EPR spectroscopy is the useful method to examine free radicals formed in antibiotics during photolysis.
15
Content available remote Action of Some Organomercury Compounds on Photosynthesis in Spinach Chloroplasts
75%
Šeršeň F. , Kráľová K.
Ecological Chemistry and Engineering S
|
2013
|
tom 20
|
nr 3
489-498
EN
The effects of five organomercury compounds (methylmercuric chloride, phenylmercuric acetate, phenylmercuric borate, phenylmercuric citrate and diphenylmercury) on photosynthetic electron transport (PET) in spinach chloroplasts were investigated. The IC50 values of organomercury compounds related to PET inhibition in spinach chloroplasts varied in the range from 468 mmol dm-3 to 942 mmol dm-3 and were approximately by one order higher than the corresponding value determined for HgCl2 applied also in DMSO solution (IC50 = 58 mmol dm-3). Due to extremely low aqueous solubility of diphenylmercury, the corresponding IC50 value could not be determined. Using EPR spectroscopy as probable sites of action of organomercury compounds in photosynthetic apparatus ferredoxin on the acceptor side of PS 1 and the quinone electron acceptors QA or QB on the reducing side of PS 2 were suggested.
PL
Zbadano wpływ pięciu związków rtęcioorganicznych (chlorku metylortęci, octanu fenylortęci, boranu fenylortęci, cytrynianu fenylortęci i difenylortęci) na fotosyntetyczny transport elektronów (PET) w chloroplastach szpinaku. Wartości IC50 dla związków rtęcioorganicznych związanych z inhibicją PET w chloroplastach szpinaku zmieniała się w zakresie od 468 do 942 μmol dm-3 i była w przybliżeniu o rząd większa od odpowiedniej wartości określonej dla HgCl2, stosowanego również w roztworze DMSO (IC50 = 58 μmol dm-3). Ze względu na bardzo małą rozpuszczalność difenylortęci w wodzie odpowiednia wartość IC50 nie może być określona. Wyniki badań za pomocą spektroskopii EPR pozwoliły na zaproponowanie prawdopodobnych miejsc działania związków rtęci w procesie fotosyntezy ferredoksyny po stronie akceptora PS 1 i chinonowego akceptora elektronów QA lub QB po stronie redukującej PS 2.
16
Content available remote Action of Some Organomercury Compounds on Photosynthesis in Spinach Chloroplasts
75%
Šeršeň F. , Kráľová K.
Ecological Chemistry and Engineering. S
|
2013
|
tom Vol. 20, nr 3
489--498
EN
The effects of five organomercury compounds (methylmercuric chloride, phenylmercuric acetate, phenylmercuric borate, phenylmercuric citrate and diphenylmercury) on photosynthetic electron transport (PET) in spinach chloroplasts were investigated. The IC50 values of organomercury compounds related to PET inhibition in spinach chloroplasts varied in the range from 468 mmol dm-3 to 942 mmol dm-3 and were approximately by one order higher than the corresponding value determined for HgCl2 applied also in DMSO solution (IC50 = 58 mmol dm-3). Due to extremely low aqueous solubility of diphenylmercury, the corresponding IC50 value could not be determined. Using EPR spectroscopy as probable sites of action of organomercury compounds in photosynthetic apparatus ferredoxin on the acceptor side of PS 1 and the quinone electron acceptors QA or QB on the reducing side of PS 2 were suggested.
PL
Zbadano wpływ pięciu związków rtęcioorganicznych (chlorku metylortęci, octanu fenylortęci, boranu fenylortęci, cytrynianu fenylortęci i difenylortęci) na fotosyntetyczny transport elektronów (PET) w chloroplastach szpinaku. Wartości IC50 dla związków rtęcioorganicznych związanych z inhibicją PET w chloroplastach szpinaku zmieniała się w zakresie od 468 do 942 μmol dm-3 i była w przybliżeniu o rząd większa od odpowiedniej wartości określonej dla HgCl2, stosowanego również w roztworze DMSO (IC50 = 58 μmol dm-3). Ze względu na bardzo małą rozpuszczalność difenylortęci w wodzie odpowiednia wartość IC50 nie może być określona. Wyniki badań za pomocą spektroskopii EPR pozwoliły na zaproponowanie prawdopodobnych miejsc działania związków rtęci w procesie fotosyntezy ferredoksyny po stronie akceptora PS 1 i chinonowego akceptora elektronów QA lub QB po stronie redukującej PS 2.
17
Content available Zastosowanie spektroskopii EPR do badania deksametazonu sterylizowanego termicznie
75%
Kościelniak M. , Pilawa B. , Wilczyński S.
Engineering of Biomaterials
|
2008
|
tom Vol. 11, no. 81-84
55--56
PL
Spektroskopię elektronowego rezonansu paramagnetycznego (EPR) zastosowano do oceny optymalnych warunków sterylizacji deksametazonu. Sterylizację sproszkowanego leku wykonano w suchym powietrzu w temperaturze 180°C w czasie wynoszącym 30 minut. Celem pracy jest określenie właściwości wolnorodnikowych sterylizowanego deksametazonu. Optymalnym warunkom sterylizacji powinno towarzyszyć powstawanie niewielkiej ilości wolnych rodników w substancji leczniczej, które mogą powodować szereg efektów ubocznych podczas farmakoterapii. Deksametazon jest syntetycznym glikokortykosteroidem z grupy hormonów steroidowych. Wykazuje silne działanie przeciwzapalne i immunosresyjne. Jest silniejszy ok. 20-30 -krotnie przewyższając hydrokortyzon i 4-5 krotnie niż prednizolon. Deksametazon hamuje zapalenie i obrzęk tkanki, dlatego jest używany do leczenia zapaleń o szerokim zakresie chorób auto-immunologicznych takich zapalenie stawów itp. Jest również aplikowany małych ilościach przed lub po zabiegach dentystycznych. W onkologii deksametazon jest podawany w trakcie chemioterapii [1,2]. Strukturę chemiczną deksametazonu przedstawiono na RYSUNKU 1. Pomiary widm wykonano za pomocą spektrometru EPR Firmy RADIOPAN (Poznań) przy modulacji pola magnetycznego wynoszącej 100kHz. Częstotliwość promieniowania mikrofalowego wynosiła 9.3GHz. Widma EPR w postaci pierwszej pochodnej rejestrowano w szerokim zakresie mocy mikrofalowej 0.7- 70mW. Analizowano parametry widm EPR oraz koncentrację wolnych rodników w sterylizowanym leku. Zbadano zmiany koncentracji i parametrów widm EPR wraz ze wzrostem czasu przechowywania leku sterylizowanego w 180°C przez 30 minut. Wyznaczono zależność amplitudy i szerokości linii EPR od mocy mikrofalowej. Analizowano wpływ mocy mikrofalowej na kształt i asymetrię widm EPR. Próbki deksametazonu nie poddane działaniu wysokiej temperatury nie dawały sygnału EPR. Widma EPR deksametazonu sterylizowanego w 180°C przez 30 minut wykazywały złożony charakter (RYS.2). Wskazuje to, że w sterylizowanym deksametazonie występuje kilka rodzajów wolnych rodników. Rejestrowane widma EPR stanowią superpozycję linii składowych pochodzących od poszczególnych typów wolnych rodników. Zbadano wpływ mocy mikrofalowej na amplitudę i szerokość linii EPR termicznie sterylizowanego deksametazonu. Zaobserwowano zmianę kształtu widm EPR wraz z mocą mikrofalową. Wraz ze wzrostem mocy mikrofalowej rośnie amplituda linii EPR deksametazonu. Podobną zależność zarejestrowano dla szerokości linii EPR. Taki charakter zamian wskazuje na jednorodne rozmieszczenie centrów paramagnetycznych w termicznie sterylizowanym deksametazonie (RYS. 3 i 4). Linie EPR różnych grup wolnych rodników nasycają się przy innej mocy mikrofalowej. Wolne rodniki w sterylizowanym deksametazonie są stabilne. Nie obserwowano szybkiego zaniku wolnych rodników z czasem przechowywania próbki. Badania EPR wskazują na niewielką zależność asymetrii linii EPR od mocy mikrofalowej. Moc mikrofalowa nieznacznie wpływa na wszystkie analizowane parametry IA1-A2I, IA1/A2I, IB1-B2I, IB1/B2I wyznaczone w pracy w celu oceny asymetrii linii EPR.
EN
Electron paramagnetic resonance (EPR) spectroscopy was applied to examine optimal sterilization conditions of dexamethasone. Sterilization of powdered dexamethasone was done in dry air at temperature 180°C during the time of 30 minutes. The aim of this work was to determine free radical properties of sterilized dexamethasone. It is expected that optima conditions of sterilization is accompanied by formation of low amount of free radicals in drug which can cause many side effects during pharmacotherapy. Dexamethasone is a potent synthetic member of the glucocorticoid class of steroid hormones. It acts as an anti-inflammatory and immunosuppressant. Its potency is about 20-30 times that of hydrocortisone and 4-5 times of prednisone. Dexamethasone inhibit the inflammatory and the edema of the tissue, so its making useful for the treatment of a wide range of inflammatory and auto-immune conditions such as rheumatoid arthritis ect. It is also given in small amounts before and/or after some forms of dental surgery. In oncology dexamethasone, it is given to cancer patients undergoing chemotherapy [1,2]. Chemical structure of dexamethasone is presented in FIGURE 1. Measurements of spectra were done by the use of EPR spectrometer produced by RADIOPAN Firm (Poznań) with modulation of magnetic field of 100 kHz. Microwave frequency of 9.3GHz was applied. The first-derivative EPR spectra were recorded with microwave power of the wide range of 0.7-70mW. Parameters of EPR spectra and free radical concentration in the sterilized drug were analyzed. Changes of free radical concentration and EPR parameters with increasing of storage time after heating of the drug at 180°C were evaluated. Changes of amplitud es and linewidths of EPR spectra with microwave power were determined. The influence of microwave power on lineshape of EPR spectra and line asymmetry was analyzed. Samples of dexamethasone not heated with high temperature gave no EPR signals. EPR spectra of dexamethasone sterilized in 180°C during 30 minutes reveal complex structure (FIG. 2). It was stated that several types of free radicals exist in the sterilized drug. Its EPR spectra reveal multi-component structure. The recorded EPR spectra are superposition of component lines of the individual types of free radicals. Influence of microwave power on amplitude and linewidths thermally sterilized dexamethasone was tested. Changes of EPR lineshapes with microwave power were observed. Amplitude of EPR line increase with microwave power increasing. Similar relationship for linewidths of EPR lines was recorded. This kind of relationship evidence on homogenous location of paramagnetic centers in thermally sterilized dexam-ethasone (FIG. 3 and 4). EPR lines of the individual groups of free radicals saturate at different microwave powers. Free radicals in sterilized dexamethasone are stabile. EPR studies indicate on small influence of microwave power on line asymmetry. Microwave power only slightly affects on all analyzed parameters IA1-A2I, IA1/A2I, IB1-B2I, IB1/B2I determined to evaluate line asymmetry.
18
Content available Multifrequency EPR study on radiation induced centers in calcium carbonates labeled with 13C
75%
Sadło J. , Bugaj A. , Strzelczak G. , Sterniczuk M. , Jaegermann Z.
Nukleonika
|
2015
|
tom Vol. 60, No. 3, part 1
429--434
EN
In calcite and aragonite, γ-irradiated at 77 K, several paramagnetic centers were generated and detected by EPR spectroscopy; in calcite, CO3 – (orthorhombic symmetry, bulk and bonded to surface), CO3 3–, NO3 2–, O3 –, and in aragonite CO2 – (isotropic and orthorhombic symmetry) depending on the type of calcium carbonate used. For calcium carbonates enriched with 13C more detailed information about the formed radicals was possible to be obtained. In both natural (white coral) and synthetic aragonite the same radicals were identifi ed with main differences in the properties of CO2 – radicals. An application of Q-band EPR allowed to avoid the signals overlap giving the characteristics of radical anisotropy.
19
Content available Free radical formation in salicylic acid and heating parameters – application of EPR, UV-Vis, TGA and colorimetry examination to optimize thermal sterilization
75%
Ramos P. , Pilawa B.
Acta Poloniae Pharmaceutica - Drug Research
|
2020
|
tom 77
|
nr 3
431-441
EN
Salicylic acid heated at different temperatures and times was examined by an X-band (9.3 GHz) EPR spectroscopy, UV-Vis spectrophotometry, TGA and colorimetry test to optimize its thermal sterilization process. Free radical formation (~1018 spin/g) during thermal sterilization of salicylic acid according to the pharmaceutical norms at temperature 120oC and time of 120 minutes was compared with those for heating at the new tested temperatures and times: 130oC and 60 minutes, and 140oC and 30 minutes. It was obtained that the relatively lower free radical concentrations characterized salicylic acid heated at temperatures (times): 120oC (120 minutes), and 130oC (60 minutes), than at temperature (time) 140oC (30 minutes). So treatment at temperature 120oC during 120 minutes, and temperature 130oC during 60 minutes, were recommended as the optimal for thermal sterilization of salicylic acid. Salicylic acid should not be sterilized at temperature 140oC during 30 minutes, because of the highest free radical formation. Free radical systems of thermally treated salicylic acid revealed complex character. Fast spin-lattice relaxation processes existed in heated salicylic acid. Strong dipolar interactions characterized all the heated salicylic acid samples. EPR spectroscopy, UV-Vis spectrophotometry, thermogravimetry, and color measurement may be helpful besides microbiological analysis to optimize thermal sterilization conditions of salicylic acid.
20
Content available Effects of storage conditions on formation of free radicals in soybean extract – an EPR spectroscopy study
75%
Jarco S.
Annales Academiae Medicae Silesiensis
|
2017
|
tom 71
217-224
EN
OBJECTIVE: Soybean extract is a valuable food supplement used for the prevention of cancer and other purposes. The role of free radicals in carcinogenesis has been proven. Studies have also confirmed the effect of storage conditions on the formation of free radicals in natural medicinal products. The study presents an attempt to optimize the storage conditions of soybean extract to prevent the formation of free radicals. AIM OF THE STUDY: The aim of the study was to determine the effect of temperature and UV radiation on the formation of free radicals in soybean extract during storage. MATERIAL AND METHODS: Samples of soybean extract were heated to temperatures of 30, 40 and 50°C. Subsequent samples were exposed to UV radiation (wavelengths 315–400 nm) for 30 and 60 minutes. EPR (electron paramagnetic resonance) spectroscopy was used to analyse the amplitude and linewidth of the EPR signal and to calculate the concentration of free radicals in the samples. RESULTS: At a room temperature of 25°C and in the absence of light, no EPR signal was recorded for the tested samples. Heating and exposure to UV light caused the formation of free radicals in the samples. The highest concentration of free radicals was found in the sample exposed to UV light for 60 minutes, while the lowest was in the sample heated to 30°C. CONCLUSIONS: The use of EPR spectroscopy enabled the identification of optimal storage conditions for soybean extract, i.e. 25°C and darkness.
PL
WSTĘP: Cennym uzupełnieniem diety jest wyciąg z nasion soi, wykorzystywany między innymi w profilaktyce nowotworów. Udział wolnych rodników w procesach karcynogenezy został udowodniony. Badania potwierdzają wpływ warunków przechowywania naturalnych środków leczniczych na zachodzące w nich zjawiska wolnorodnikowe. W pracy podjęto próbę optymalizacji warunków przechowywania wyciągu z nasion soi, aby zapobiec powstawaniu w nim wolnych rodników. CEL PRACY: Celem pracy było określenie wpływu temperatury i promieniowania UV na generowanie wolnych rodników w wyciągu z nasion soi w trakcie przechowywania. MATERIAŁ I METODY: Próbki z wyciągiem z nasion soi ogrzewano w temperaturach 30, 40 i 50°C. Kolejne próbki naświetlano promieniowaniem UV (długość fali 315–400 nm) przez 30 i 60 minut. Wykorzystano spektroskopię EPR (elektron paramagnetic resonance), analizując amplitudę i szerokość linii EPR oraz obliczając koncentrację wolnych rodników w próbkach. WYNIKI: W temperaturze pokojowej 25°C oraz przy braku dostępu światła nie rejestrowano sygnału EPR dla testowanych próbek. Ogrzewanie próbek oraz ekspozycja na promieniowanie UV powodowały pojawienie się w nich wolnych rodników. Największą koncentrację wolnych rodników stwierdzono w próbce naświetlanej UV przez 60 minut, najniższe zaś w próbce ogrzanej do 30°C. WNIOSKI: Wykorzystanie spektroskopii EPR pozwoliło na ustalenie optymalnych warunków przechowywania wyciągu z nasion soi, którymi są temperatura 25°C oraz brak dostępu światła.
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