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Synthesis and chromatographic evaluation of poly(pentabromostyrene)-silica composite: A versatile stationary phase for separating both polar and non-polar aromatic compounds
Microchemical Journal ( IF 4.9 ) Pub Date : 2020-07-01 , DOI: 10.1016/j.microc.2020.104838
Zhanying Chu , Weibing Zhang , Duxin Li , Lingyi Zhang , Manman Zhu , Zhaosong Ge

Abstract Polymer-silica composite materials have been witnessed as one of the most promising chromatographic packing materials. The demands of novel stationary phases are always existing due to the requirements for the separation of special samples. In our present work, the novel poly(pentabromostyrene)-silica composite stationary phases were successfully prepared by surface initial free-radical polymerization. The polymer chains bonding on the surface of the poly(pentabromostyrene) contain plenty of phenyl moiety, which provide hydrophobic and π-π interactions between the stationary phase and analytes. Besides, the bromide atoms, existing in the polymer, provide extra polar interaction with polar or easily polarized analytes. Compared with the typical C18 stationary phase, the novel stationary phase showed special separation selectivity. Samples, including polycyclic aromatic hydrocarbons, phenols, anilines, amino acids, halogenated benzenes, acetophenone derivatives, benzene homologous compounds, were all well separated by the new stationary phase. Also, the great stability (0.13% ≤ RSDs ≤ 0.98%, n = 5) of packed columns and the good synthesis repeatability were demonstrated. Finally, the new columns were applied to the separation of fullerenes. The loading ratio reached 2.67% (36 mg of fullerenes was loaded onto the column packed with 1.35 g stationary phase), with high yield (86.3%) of high pure C60 (>95%). This novel stationary phase has a great potential to be a complementary to traditional C18 column and a special column for fullerenes separation.

中文翻译:

聚(五溴苯乙烯)-二氧化硅复合材料的合成和色谱评价:一种用于分离极性和非极性芳香族化合物的通用固定相

摘要 聚合物-二氧化硅复合材料被认为是最有前途的色谱填料之一。由于特殊样品分离的要求,对新型固定相的需求始终存在。在我们目前的工作中,通过表面初始自由基聚合成功制备了新型聚(五溴苯乙烯)-二氧化硅复合固定相。聚(五溴苯乙烯)表面上键合的聚合物链含有大量苯基部分,它们在固定相和分析物之间提供疏水性和 π-π 相互作用。此外,存在于聚合物中的溴原子提供了与极性或易极化分析物的额外极性相互作用。与典型的C18固定相相比,新型固定相表现出特殊的分离选择性。样品,包括多环芳烃、酚类、苯胺类、氨基酸类、卤代苯类、苯乙酮衍生物、苯类同系物等,均被新型固定相很好地分离。此外,还证明了填充柱的高稳定性(0.13% ≤ RSD ≤ 0.98%,n = 5)和良好的合成重复性。最后,将新色谱柱应用于富勒烯的分离。加载率达到2.67%(36 mg富勒烯加载到填充有1.35 g固定相的柱子上),高纯度C60(>95%)的产率(86.3%)。这种新型固定相具有作为传统 C18 色谱柱的补充和富勒烯分离专用色谱柱的巨大潜力。苯同系物均被新固定相很好地分离。此外,还证明了填充柱的高稳定性(0.13% ≤ RSD ≤ 0.98%,n = 5)和良好的合成重复性。最后,将新色谱柱应用于富勒烯的分离。加载率达到2.67%(36 mg富勒烯加载到填充有1.35 g固定相的柱子上),高纯度C60(>95%)的产率(86.3%)。这种新型固定相具有作为传统 C18 色谱柱的补充和富勒烯分离专用色谱柱的巨大潜力。苯同系物均被新固定相很好地分离。此外,还证明了填充柱的高稳定性(0.13% ≤ RSD ≤ 0.98%,n = 5)和良好的合成重复性。最后,将新色谱柱应用于富勒烯的分离。加载率达到2.67%(36 mg富勒烯加载到填充有1.35 g固定相的柱子上),高纯度C60(>95%)的产率(86.3%)。这种新型固定相具有作为传统 C18 色谱柱的补充和富勒烯分离专用色谱柱的巨大潜力。新色谱柱用于分离富勒烯。加载率达到2.67%(36 mg富勒烯加载到填充有1.35 g固定相的柱子上),高纯度C60(>95%)的产率(86.3%)。这种新型固定相具有作为传统 C18 色谱柱的补充和富勒烯分离专用色谱柱的巨大潜力。新色谱柱用于分离富勒烯。加载率达到2.67%(36 mg富勒烯加载到填充有1.35 g固定相的柱子上),高纯度C60(>95%)的产率(86.3%)。这种新型固定相具有作为传统 C18 色谱柱的补充和富勒烯分离专用色谱柱的巨大潜力。
更新日期:2020-07-01
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