Visible light initiated polymerization of styrenic monolithic stationary phases using 470 nm light emitting diode arrays.
Visible light initiated polymerization of styrenic monolithic stationary phases using 470 nm light emitting diode arrays.
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DOI：
10.1002/jssc.200900624
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发表时间：
2010-01
影响因子：
3.1
通讯作者：
Macka, Mirek
中科院分区：
文献类型：
--
作者：
Walsh, Zarah;Levkin, Pavel A.;Jain, Vijay;Paull, Brett;Svec, Frantisek;Macka, Mirek
首次通过光引发聚合合成了聚（苯乙烯-二乙烯基苯）整体固定相。使用470 nm发光二极管阵列作为光源，激活由(+)-S-樟脑醌/4-二甲基氨基苯甲酸乙酯/四氟硼酸N-甲氧基-4-苯基吡啶鎓组成的引发剂。苯乙烯整体的空间控制聚合已在 100 µm 内径的特定部分内实现。使用简单的光掩模技术涂覆聚四氟乙烯 (PTFE) 熔融石英毛细管。通过光学显微镜确认边缘的清晰度，同时使用扫描电子显微镜验证典型的多孔、球状形态。流阻数据用于评估整体材料的渗透性，发现它们具有良好的流通性能，在 1 µl min−1（水，20°C）下的流阻为 0.725 MPa cm−1。沿毛细管长度的电导率分布用于评估其横向均匀性。发现在聚合过程中轴向旋转的整料沿着毛细管的整个长度是均匀的。整体固定相应用于蛋白质混合物的反相梯度分离。色谱柱制造具有出色的重现性，批次的保留因子 (k) 的 RSD 值为 2.6%，单个色谱柱的 RSD 值低于 1.73%。
Poly(styrene-co-divinylbenzene) monolithic stationary phases have been synthesised for the first time by photoinitiated polymerisation. An initiator composed of (+)-S-camphorquinone/ethyl-4-dimethylaminobenzoate/N-methoxy-4-phenylpyridinium tetrafluoroborate was activated using a 470 nm light emitting diode array as the light source. Spatially controlled polymerisation of styrenic monoliths has been achieved within specific sections of a 100 µm i.d. polytetrafluoroethylene (PTFE)-coated fused silica capillary using simple photo-masking. The sharpness of the edges was confirmed by optical microscopy, while scanning electron microscopy was used to verify a typical porous, globular morphology. Flow resistance data was used to assess the permeability of the monoliths and they were found to have good flow through properties with a flow resistance of 0.725 MPa cm−1 at 1 µl min−1 (water, 20°C). Conductivity profiling along the length of the capillary was used to assess their lateral homogeneity. Monoliths which were axially rotated during polymerisation were found to be homogeneous along the whole length of the capillary. The monolithic stationary phases were applied to the reversed phase gradient separation of a mixture of proteins. Column fabrication showed excellent reproducibility with the retention factor (k) having a RSD value of 2.6% for the batch and less than 1.73% on individual columns.
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DOI：
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发表时间：
2003-07-14
影响因子：
4.3
作者：
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发表时间：
2003-07-14
影响因子：
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作者：
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通讯作者：
Wrzyszczynski, A
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