Department of Biomedical Engineering, Washington University in St. Louis, St. Louis, Missouri 63130, United States.
Langmuir. 2013 Mar 26;29(12):4128-39. doi: 10.1021/la3051115. Epub 2013 Mar 11.
Clickable nanogel solutions were synthesized by using the copper catalyzed azide/alkyne cycloaddition (CuAAC) to partially polymerize solutions of azide and alkyne functionalized poly(ethylene glycol) (PEG) monomers. Coatings were fabricated using a second click reaction: a UV thiol-yne attachment of the nanogel solutions to mercaptosilanated glass. Because the CuAAC reaction was effectively halted by the addition of a copper-chelator, we were able to prevent bulk gelation and limit the coating thickness to a single monolayer of nanogels in the absence of the solution reaction. This enabled the inclusion of kosmotropic salts, which caused the PEG to phase-separate and nearly double the nanogel packing density, as confirmed by quartz crystal microbalance with dissipation (QCM-D). Protein adsorption was analyzed by single molecule counting with total internal reflection fluorescence (TIRF) microscopy and cell adhesion assays. Coatings formed from the phase-separated clickable nanogel solutions attached with salt adsorbed significantly less fibrinogen than other 100% PEG coatings tested, as well as poly(L-lysine)-g-PEG (PLL-g-PEG) coatings. However, PEG/albumin nanogel coatings still outperformed the best 100% PEG clickable nanogel coatings. Additional surface cross-linking of the clickable nanogel coating in the presence of copper further reduced levels of fibrinogen adsorption closer to those of PEG/albumin nanogel coatings. However, this step negatively impacted long-term resistance to cell adhesion and dramatically altered the morphology of the coating by atomic force microscopy (AFM). The main benefit of the click strategy is that the partially polymerized solutions are stable almost indefinitely, allowing attachment in the phase-separated state without danger of bulk gelation, and thus producing the best performing 100% PEG coating that we have studied to date.
点击纳米凝胶溶液是通过铜催化的叠氮化物/炔烃环加成(CuAAC)反应来合成的,该反应部分聚合了叠氮化物和炔基功能化的聚(乙二醇)(PEG)单体的溶液。通过第二次点击反应来制备涂层:纳米凝胶溶液的紫外硫醇-炔键合到巯基硅烷化玻璃上。由于铜螯合剂的加入有效地阻止了 CuAAC 反应,我们能够防止大量凝胶化,并在没有溶液反应的情况下将涂层厚度限制在单层纳米凝胶。这使得包含亲水性盐成为可能,亲水性盐导致 PEG 相分离并使纳米凝胶的堆积密度几乎增加一倍,这一点通过石英晶体微天平(QCM-D)得到了证实。通过全内反射荧光(TIRF)显微镜和细胞黏附实验分析蛋白质吸附。由相分离的点击纳米凝胶溶液形成的涂层在吸附盐后,与其他测试的 100%PEG 涂层以及聚(L-赖氨酸)-g-PEG(PLL-g-PEG)涂层相比,吸附的纤维蛋白原显著减少。然而,PEG/白蛋白纳米凝胶涂层的性能仍然优于最佳的 100%PEG 点击纳米凝胶涂层。在存在铜的情况下对点击纳米凝胶涂层进行进一步表面交联,将纤维蛋白原吸附水平进一步降低到与 PEG/白蛋白纳米凝胶涂层接近的水平。然而,这一步骤对长期抵抗细胞黏附的能力产生了负面影响,并通过原子力显微镜(AFM)显著改变了涂层的形态。点击策略的主要优点是部分聚合的溶液几乎可以无限期地稳定,允许在相分离状态下进行附着,而不会有发生大量凝胶化的危险,从而产生了我们迄今为止研究过的性能最佳的 100%PEG 涂层。