The thermogravimetric analysis (TG) of two series
of tri-block copolymers based on poly(L,L-lactide) (PLLA) and poly(ethyleneglycol) (PEG)
segments, having molar mass of 4000 or 600 g mol–1,
respectively, is reported. The prepared block copolymers presented wide range
of molecular masses (800 to 47500 g mol–1)
and compositions (16 to 80 mass% PEG). The thermal stability increased with
the PLLA and/or PEG segment size and the tri-block copolymers prepared from
PEG 4000 started to decompose at higher temperatures compared to those copolymers
from PEG 600. The copolymers compositions were determined by thermogravimetric
analysis and the results were compared to other traditional quantitative spectroscopic
methods, hydrogen nuclear magnetic resonance spectrometry (1HNMR)
and Fourier transform infrared spectrometry (FTIR). The PEG 4000 copolymer
compositions calculated by TG and by 1HNMR, presented
differences of 1%, demonstrating feasibility of using thermogravimetric analysis
for quantitative purposes.
Authors:C. Mothé, A. Azevedo, W. Drumond, and S. Wang
Samples of poly(l,l-lactide)-block-poly(ethylene glycol)-block-poly(l,l-lactide) (PLLA-PEG-PLLA) were synthesized from l,l-lactide polymerization using stannous 2-ethylhexanoate, Sn(Oct)2 as initiator and di-hydroxy-terminated poly(ethylene glycol) (PEG) (Mn = 4000 g mol−1) as co-initiator. The chemical linkage between the PEG segment and the PLA segments was characterized by Fourier transform
infrared spectroscopy (FTIR). Thermogravimetry analysis (TG) revealed the copolymers composition and was capable to show the
deleterious effect of an excess of Sn(Oct)2 in the polymer thermal stability, while Differential Scanning Calorimetry (DSC) allowed the observation of the miscibility
between the PLLA and PEG segments in the different copolymers.
Authors:C. G. Mothé, A. D. Azevedo, W. S. Drumond, S. H. Wang, and R. D. Sinisterra
Amphiphilic triblock copolymers, based on hydrophilic poly(ethylene glycol) (PEG) blocks and hydrophobic poly(l,l-lactide) (PLLA) blocks, were used as the matrix material for the preparation of tetracycline-loaded microspheres. The morphology and thermal properties of the biodegradable microspheres were evaluated. SEM showed the predominance of the spherical shape, however, it was possible to distinguish three patterns: rough or smooth surface or uneven collapsed volume. The FTIR analysis indicated good mechanical stability and structural integrity of the PLLA-PEG-PLLA copolymer’s microspheres enclosing tetracycline. By thermal analysis it was possible to see the marginal influence of tetracycline on the glass transition and melting temperatures of the PLLA-PEG-PLLA triblock copolymer, while the results by TG indicated the presence of tetracycline in the inner structure of the microspheres, which thermal decomposition leading to char formation was triggered by the drug’s presence.