用红外光谱和薄层色谱法研究聚乙二醇的活化及其表征

R. Bashyal
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摘要

聚乙二醇(PEG)是最常用的用于改变和控制生物分布的聚合物材料。PEG可以增加“药物载体”组装的寿命,这有助于施用较低浓度的“药物载体”复合材料。由于聚乙二醇提供了一种屏蔽特性,避免了体内的肾脏快速清除,因此它已被广泛用于治疗中使用的载体的修饰。本研究于2005年5月至7月在德拉敦海豚生物医学和自然科学研究所和印度鲁尔基印度理工学院(IIT)进行。用干苯、三乙胺、二氯乙烯和4-硝基苯氯甲酸酯对不同分子量(400da、4000da、8000 Da和20000 Da)的聚乙二醇进行活化。用EDC:甲醇(7:3)对反应混合物进行薄层色谱监测。然后在EDC和水之间分配反应混合物。EDC分离漏斗中较低的馏分被收集并浓缩在旋转蒸发器上得到活化的PEG。从上面的反应和结构可以清楚地看出,4-硝基氯甲酸乙酯含有两个高电负性基团,即NO2和Cl。这两组相互作用导致极性中和。然后作为非极性分子,对流动相(甲醇和EDC)表现出高亲和力。因此,4-硝基苯氯甲酸酯的迁移率最高,而PEG的迁移率最低。红外光谱分析发现,聚乙二醇的羟基(OH)峰位于3400 ~ 3450cm-1。C-Cl键的峰值在746 cm-1处。而聚乙二醇与4-硝基苯氯甲酸酯反应后,发现- OH峰没有聚乙二醇那么深。山峰有点短,有点宽。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
A study on activation of polyethylene glycol and its characterization by infrared spectroscopy and thin layer chromatography
Polyethylene Glycol (PEG) is the most popular polymeric material used for alteration and control of biodistribution. PEG may increase the lifetime of “drug carrier” assembly which helps in administering lower concentration of the “drug carrier” composite. It has been used widely for the modification of carriers used in therapeutics because PEG offers a shielding characters that avoids rapid renal clearance from the body. This study was carried out at Dolphin Institute of Biomedical and Natural Sciences, Dehradun and Indian Institute of Technology (IIT), Roorkee, India during May-July 2005. Activation of PEG of different molecular weight (400 Da, 4000 Da, 8000 Da and 20,000 Da) was done using dry benzene, Triethylamine, Ethylene dichloride and 4-nitrophenyl chloroformate. Reaction mixture was monitored on TLC using EDC: Methanol (7:3). Then reaction mixture was portioned between EDC & water. The lower fraction in separating funnel of EDC was collected & concentrated on rota evaporator to get activated PEG. From the above reaction and structure it was clear that 4-Nitrophenyl Chloroformate contains two highly electronegative groups i.e. NO2 and Cl. These two groups interact with each other resulting in neutralization of polarity. It then acts as non-polar molecule and shows high affinity for mobile phase (methanol & EDC). Therefore, 4-Nitrophenylchloroformate has the highest mobility and PEG has lowest mobility. From IR Spectroscopy it was found that the peak of Hydroxyl group- (OH) of PEG was at 3400- 3450cm-1. The peak of C-Cl bond was found at 746 cm-1. But after the reaction between PEG and 4-Nitrophenyl Chloroformate the- OH peak was found not so deep as in PEG. The peak was somewhat short and broad.
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