Separation of polyethylene glycols and maleimide-terminated polyethylene glycols by reversed-phase liquid chromatography under critical conditions.

Separation of polyethylene glycols and maleimide-terminated polyethylene glycols by reversed-phase liquid chromatography under critical conditions.
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在临界条件下通过反相液相色谱分离聚乙二醇和马来酰亚胺封端的聚乙二醇。

DOI:
10.1002/jssc.201600904
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发表时间:
2016-11
期刊:
J Sep Sci
影响因子:
--
通讯作者:
Jiang Xulin
Jiang Xulin
中科院分区:
其他
文献类型:
--
作者:
Wei Yanzhen;Zhuo Renxi;Jiang Xulin

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在反相色谱柱上,研究了基于马来酰亚胺端基数目的聚乙二醇和马来酰亚胺取代的聚乙二醇衍生物在临界液相色谱条件下的分离。非官能聚乙二醇和双官能马来酰亚胺取代的聚乙二醇的关键溶剂组成在反相十八烷基碳链键合硅胶柱上测定为相同,约为40%乙腈水溶液,使用不同组成的乙腈和水的混合物作为移动的相,25°C。在临界等度洗脱条件下,马来酰亚胺官能化的聚乙二醇根据马来酰亚胺官能度(分别具有零个、一个、两个或三个马来酰亚胺端基)成功分离,摩尔质量没有明显影响。分离主要是由于马来酰亚胺端基与柱填料之间的疏水相互作用。离线基质辅助激光解吸/电离飞行时间质谱被用来识别的重复单元,特别是,端基的马来酰亚胺取代的聚乙二醇。临界条件下的液相色谱分析可以为优化功能化聚乙二醇的合成提供有用的信息。据我们所知,这是第一次报告的基线分离马来酰亚胺官能化的聚乙二醇的基础上的功能独立的摩尔质量,而无需衍生化等度洗脱。
The separation of polyethylene glycols and maleimide-substituted polyethylene glycol derivatives based on the number of maleimide end-groups under critical liquid chromatography conditions has been investigated on a reversed-phase column. The critical solvent compositions for nonfunctional polyethylene glycols and bifunctional maleimide-substituted polyethylene glycols were determined to be identical at about 40% acetonitrile in water on a reversed-phase octadecyl carbon chain-bonded silica column using mixtures of acetonitrile and water of varying composition as the mobile phase at 25°C. The maleimide-functionalized polyethylene glycols were successfully separated according to maleimide functionality (with zero, one, two, or three maleimide end-groups, respectively) under the critical isocratic elution conditions without obvious effect of molar mass. The separation was mainly due to the hydrophobic interaction between the maleimide end-groups and the column packing. Off-line matrix-assisted laser desorption/ionization time of flight mass spectrometry was used to identify the repeating units and, especially, the end-groups of the maleimide-substituted polyethylene glycols. Liquid chromatography analysis at critical conditions could provide useful information to optimize the synthesis of functional polyethylene glycols. To our knowledge, this is the first report of the baseline separation of maleimide-functionalized polyethylene glycols based on the functionality independent of the molar mass without derivatization by isocratic elution.
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