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Separation of polybutylene glycols widely differing in molecular weight on different stationary phase by gradient RP-HPLC and detection by evaporative light scattering

机译:梯度RP-HPLC在不同固定相上分离分子量相差很大的聚丁二醇,并通过蒸发光散射进行检测

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摘要

Polybutylene glycols (PBG's) substantially differing in molecular weight (MW), i.e., PBG 650, PBG 1000, PBG 2000 and PBG 3000 were subjected to separation on monolithic, i.e., Chromolith SpeedRod RP-18 and Chromolith Performance RP-18, polymeric, i.e., Polymer C-18 and silica-based, i.e., Nucleosil 5C(4) chromatographic supports. Different eluent systems each consisting of a ternary gradient built up from acetonitrile, tetrahydrofuran and water were applied and monitoring of signal responses was accomplished by evaporative light scattering detection (ELSD). Fine-tuning of the gradient profiles for the different PBG's yields optimum separation of the individual oligomers of the low MW samples PBG 650 and PBG 1000 and no marked differences seem to occur on the four stationary phases used within the study. However in contrast, pronounced deviations between them were observable when applied for separation of PBG 2000 and PBG 3000. Surprisingly in the latter case the Nucleosil 5C4 support proved to be better suited for separation of sample constituents of higher MW. Although better resolution into individual oligomers, in particular of PBG 2000 and PBG 3000, was achieved on both Chromolith SpeedRod RP-18 and Chromolith Performance RP-18 when compared to the Polymer C-18 support, the good separation efficiency of the latter support is nevertheless quite remarkable making this material an additional valuable alternative for chromatographic fingerprinting at least for PBG 650 and PBG 1000.
机译:将分子量(MW)基本不同的聚丁二醇(PBG)(即PBG 650,PBG 1000,PBG 2000和PBG 3000)在整体式(即Chromolith SpeedRod RP-18和Chromolith Performance RP-18)上分离,即聚合物C-18和二氧化硅基,即Nucleosil 5C(4)色谱载体。应用不同的洗脱液系统,每个系统由乙腈,四氢呋喃和水构成的三元梯度组成,并通过蒸发光散射检测(ELSD)监测信号响应。对不同PBG的梯度曲线进行微调可对低分子量样品PBG 650和PBG 1000的各个低聚物进行最佳分离,并且在研究中使用的四个固定相上似乎没有明显差异。但是,相比之下,当用于分离PBG 2000和PBG 3000时,可以观察到它们之间明显的偏差。令人惊讶的是,在后一种情况下,Nucleosil 5C4载体被证明更适合分离更高分子量的样品成分。尽管与聚合物C-18载体相比,Chromolith SpeedRod RP-18和Chromolith Performance RP-18均能更好地拆分成单个低聚物,尤其是PBG 2000和PBG3000。但后者的良好分离效率是尽管如此,这种材料还是非常引人注目的,至少对于PBG 650和PBG 1000而言,它是色谱指纹图谱的另一种有价值的替代品。

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