Luef Klaus P, Petit Charlotte, Ottersböck Bettina, Oreski Gernot, Ehrenfeld Francis, Grassl Bruno, Reynaud Stéphanie, Wiesbrock Frank
Polymer Competence Center Leoben, Roseggerstrasse 12, 8700 Leoben, Austria; Institute for Chemistry and Technology of Materials, Graz University of Technology, NAWI Graz, Stremayrgasse 9, 8010 Graz, Austria.
IPREM, UMR 5254 UPPA/CNRS, Hélioparc, 2 Avenue Du Président Angot, 64053 Pau CEDEX 09, France.
Eur Polym J. 2017 Apr;88:701-712. doi: 10.1016/j.eurpolymj.2016.08.012. Epub 2016 Aug 20.
An 80-membered library of gels composed of monofunctional 2-ethyl-2-oxazoline and 2-nonyl-2-oxazoline and one of four selected difunctional 2-oxazolines (containing either ether or ester bonds) were synthesized by microwave-assisted ring-opening polymerizations. The difunctional 2-oxazolines were prepared from the thiol-ene reaction of glycol dimercaptoacetate or 2,2'-(ethylenedioxy)diethanethiol and 2-but-3'-enyl-2-oxazoline or 2-dec-9'-enyl-2-oxazoline. 53 of the gels exhibited glass-transition temperatures, which ranged from -5.9 to 45.3 °C. 13 Derivatives exhibited glass-transition temperatures in the range from 20 to 30 °C, which renders them stiff at room temperature and flexible at body temperature. The gels that did not contain any 2-ethyl-2-oxazoline acted as lipogels, whereas the gels that did not contain any 2-nonyl-2-oxazoline acted as hydrogels; all other gels may be classified as amphigels. The swelling degrees were measured by gravimetry and maximum swelling degrees of 6 (in water) were observed for the gels with the lowest degrees of crosslinking. In a second approach, the synthesis of crosslinked networks had been achieved by performing the polymeranalogous thiol-ene reaction of copoly(2-oxazoline)s containing olefinic side-chains and glycol dimercaptoacetate. This soft strategy enabled the straightforward loading of such gels with active pharmaceutical ingredients without altering them. This method delivered gels with selected composition exhibiting a targeted disc-shape and loaded with active pharmaceutical ingredients from one-step syntheses. The maximum swelling degrees of these specimens were found to be in accordance with the ones from the first route investigated. Preliminary degradation studies were performed at 25 °C; these types of gels were found to be degraded in alkaline media as well as by esterases.
通过微波辅助开环聚合反应合成了一个由单官能团2-乙基-2-恶唑啉和2-壬基-2-恶唑啉以及四种选定的双官能团2-恶唑啉(含有醚键或酯键)之一组成的80种凝胶的文库。双官能团2-恶唑啉是由乙二醇二巯基乙酸酯或2,2'-(乙二氧基)二乙硫醇与2-丁-3'-烯基-2-恶唑啉或2-癸-9'-烯基-2-恶唑啉的硫醇-烯反应制备的。其中53种凝胶表现出玻璃化转变温度,范围为-5.9至45.3℃。13种衍生物的玻璃化转变温度在20至30℃范围内,这使得它们在室温下坚硬而在体温下柔韧。不含任何2-乙基-2-恶唑啉的凝胶用作脂凝胶,而不含任何2-壬基-2-恶唑啉的凝胶用作水凝胶;所有其他凝胶可归类为两性凝胶。通过重量法测量溶胀度,对于交联度最低的凝胶,观察到最大溶胀度为6(在水中)。在第二种方法中,通过对含有烯属侧链的共聚(2-恶唑啉)和乙二醇二巯基乙酸酯进行聚合物类似的硫醇-烯反应,实现了交联网络的合成。这种温和的策略能够在不改变活性药物成分的情况下直接将其负载到此类凝胶中。该方法通过一步合成得到了具有选定组成、呈目标圆盘形状且负载有活性药物成分的凝胶。发现这些样品的最大溶胀度与所研究的第一条路线的溶胀度一致。在25℃下进行了初步降解研究;发现这类凝胶在碱性介质以及酯酶作用下会降解。