文献:聚乙二醇接枝光反应性聚乙二醇的合成与表征及其在防生物污损应用方面的研究
链接:https://www.mdpi.com/2073-4360/15/1/184
作者:马哈茂德·H·奥斯曼1,2奥西德,伊藤义弘1,2,3,*奥西德和秋元准
节选:
EO、AzPheEO和mPEG-EPO的共聚
首先,将环氧乙烷 (EO) 与 AzPheEO 和 mPEG-EPO 共聚(方案 1)。为此,将 TBAB、AzPheEO 和 mPEG-EPO 在真空下干燥 2 小时,然后暴露于干燥氮气中。将甲苯加入烧瓶中以溶解 mPEG-EPO。随后,将 EO 溶液和 i-Bu 3 Al 加入置于冰浴中的烧瓶中。将溶液在 25 °C 下避光搅拌共聚 18 小时。将甲醇加入溶液中,减压除去溶剂。将粗化合物溶解于丙酮中,并将溶液用水透析三天。然后将所得聚合物冷冻干燥,称为 AzPEGx [y],其中 x 和 y 分别代表 Mn 和 mPEG-EO 的投料比。所得 AzPEGx [y] 聚合物采用1 H-核磁共振 (NMR) 光谱法 (JNM-ECZ400R, 400 MHz, JEOL, 日本东京) 在氯仿中进行表征,以及采用凝胶渗透色谱法 (GPC; JASCO, 日本东京) 进行表征。该系统配备一台折射率检测器 (RI-2032, JASCO, 日本东京) 和两根色谱柱 (SB-803 HQ 和 SB804 HQ; Showa Denko, 日本东京),在含有 10 mM 溴化锂的二甲基甲酰胺 (DMF) 中进行分析。
Copolymerization of EO, AzPheEO, and mPEG-EPO
First, EO was copolymerized with AzPheEO and mPEG-EPO (Scheme 1). For this, TBAB, AzPheEO, and mPEG-EPO were dried under vacuum for 2 h, after which they were exposed to dry nitrogen. Toluene was added to the flask to dissolve mPEG-EPO. Subsequently, the EO solution and i-Bu3Al were added to the flask in an ice bath. The solution was stirred for copolymerization at 25 °C in the dark for 18 h. Methanol was added to the solution, and the solvent was removed under reduced pressure. The crude compound was dissolved in acetone, and the solution was dialyzed against water for three days. The resulting polymer was then freeze-dried and is referred to as AzPEGx [y], where x and y represent the Mn and feed ratio of mPEG-EO, respectively. The obtained AzPEGx [y] polymer was characterized via 1H-nuclear magnetic resonance (NMR) spectroscopy (JNM-ECZ400R, 400 MHz, JEOL, Tokyo, Japan) in chloroform, as well as via gel permeation chromatography (GPC; JASCO, Tokyo, Japan). The system was equipped with a refractive index detector (RI-2032, JASCO, Tokyo, Japan) and two columns (SB-803 HQ and SB804 HQ; Showa Denko, Tokyo, Japan) in dimethylformamide (DMF) containing 10 mM lithium bromide.
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