Electron magnetic resonance study of gamma-irradiated poly(lactide-co-glycolide) microspheres
Autor: | Helen Gray, Ian J. Purnell, Mike Claybourn, Christopher C. Rowlands, Damien Martin Murphy |
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Rok vydání: | 2003 |
Předmět: |
chemistry.chemical_classification
Electron nuclear double resonance Magnetic Resonance Spectroscopy Chemistry Radical Analytical chemistry Pharmaceutical Science Resonance Spectral line Microspheres law.invention Glycolates Polylactic Acid-Polyglycolic Acid Copolymer law Gamma Rays Polymer chemistry Irradiation Lactic Acid Electron paramagnetic resonance Hyperfine structure Alkyl Polyglycolic Acid |
Zdroj: | Journal of controlled release : official journal of the Controlled Release Society. 91(3) |
ISSN: | 0168-3659 |
Popis: | A series of poly(lactide-co-glycolide) samples of compositions ranging from (75:25) to (65:35) to (50% (65:35):50% (50:50)) were gamma-irradiated under ambient conditions in air. The irradiation doses used were 15, 20, 25, and 30 kGy. The generation of radicals resulting from the gamma-irradiation was confirmed using EPR. Two major radical species were observed and identified as centered at alkyl and alkyl peroxy groups. The indication from the X-band (9 GHz) frequencies showed that alkyl radicals gave rise to a quartet hyperfine pattern. However, measurements performed at higher W-band frequencies (90 GHz) showed that the X-band spectra are actually a composite profile arising from a series of overlapping individual resonances. Using combined EPR and ENDOR (Electron-Nuclear DOuble Resonance) measurements, an alkyl peroxy radical was identified. For increasing glycolide concentration from 75:25 to the 50:50 blend, there was a factor of 7 increase in the concentration of radicals A and B. Furthermore, both radical species were found to be stable for several weeks after storage at ambient temperature conditions. At elevated temperatures and humidities, radical stability decreased--the decay rate was estimated at approximately 3x10(-8) mol K(-1). The stability characteristics of the radicals under different conditions are attributed to changes in the morphology of the polymer. |
Databáze: | OpenAIRE |
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