Department of Chemical and Biomolecular Engineering, Rice University, Houston, Texas, USA.
Nat Protoc. 2012 May 31;7(6):1219-27. doi: 10.1038/nprot.2012.055.
This protocol describes the synthesis of oligo(poly(ethylene glycol) fumarate) (OPF; 1-35 kDa; a polymer useful for tissue engineering applications) by a one-pot reaction of poly(ethylene glycol) (PEG) and fumaryl chloride. The procedure involves three parts: dichloromethane and PEG are first dried; the reaction step follows, in which fumaryl chloride and triethylamine are added dropwise to a solution of PEG in dichloromethane; and finally, the product solution is filtered to remove by-product salt, and the OPF product is twice crystallized, washed and dried under vacuum. The reaction is affected by the molecular weight of PEG and reactant molar ratio. The OPF product is cross-linked by radical polymerization by either a thermally induced or ultraviolet-induced radical initiator, and the physical properties of the OPF oligomer and resulting cross-linked hydrogel are easily tailored by varying PEG molecular weight. OPF hydrogels are injectable, they polymerize in situ and they undergo biodegradation by hydrolysis of ester bonds. The expected time required to complete this protocol is 6 d.
本方案描述了通过聚乙二醇（PEG）和富马酰氯的一锅反应合成聚（聚乙二醇）琥珀酸酯（OPF；1-35 kDa；一种用于组织工程应用的聚合物）。该程序包括三个部分：首先干燥二氯甲烷和 PEG；反应步骤，富马酰氯和三乙胺逐滴加入到二氯甲烷中的 PEG 溶液中；最后，过滤产物溶液以除去副产物盐，并将 OPF 产物两次结晶、洗涤并在真空中干燥。该反应受 PEG 的分子量和反应物摩尔比的影响。OPF 产物通过热诱导或紫外光诱导自由基引发剂进行自由基聚合交联，并且可以通过改变 PEG 分子量轻松调整 OPF 低聚物和所得交联水凝胶的物理性质。OPF 水凝胶可注射，可原位聚合，并通过酯键的水解进行生物降解。完成本方案所需的预期时间为 6 天。
