Thurmann Sebastian, Mauritz Laura, Heck Christian, Belder Detlev
J Chromatogr A. 2014 Nov 28;1370:33-9. doi: 10.1016/j.chroma.2014.10.008.
A stable and permanent integration of miniature packed bed separation columns into microfluidic systems is a major issue in nano liquid chromatography. Various approaches like differently shaped retaining elements or the use of key stone effect have been investigated. We show a flexible integration of miniature packed bed separation columns into microfluidic chips utilising common HPLC material achieved by laser-assisted generation of narrow, photopolymerised frits. The generated retaining elements serve as an in- and outlet frits for the columns. An optimised pre-polymeric solution, consisting of butyl acrylates and a porogen, allows a precise fabrication of frit-type structures with lengths of less than 100 m and the capability to withstand common slurry packing pressures of more than 250 bar. The separation of seven polycyclic aromatic hydrocarbons by pressure-driven, reversed-phase chromatography proves the high quality of the created chromatographic column inside a glass chip. Plate heights down to 2.9 were achieved and extremely fast separations with sub-second peak widths were performed in isocratic and gradient elution modes on very short columns (≤ 25 mm).
将微型填充床分离柱稳定且永久地集成到微流控系统中是纳米液相色谱中的一个主要问题。人们已经研究了各种方法，如不同形状的保留元件或利用拱石效应。我们展示了一种将微型填充床分离柱灵活集成到微流控芯片中的方法，该方法利用常见的高效液相色谱材料，通过激光辅助生成狭窄的光聚合烧结体来实现。所生成的保留元件用作柱的进出口烧结体。一种由丙烯酸丁酯和致孔剂组成的优化预聚合溶液，能够精确制造长度小于100μm的烧结体型结构，并能承受超过250 bar的常见浆料填充压力。通过压力驱动的反相色谱法分离七种多环芳烃，证明了玻璃芯片内所创建色谱柱的高质量。在非常短的柱（≤25 mm）上，采用等度和梯度洗脱模式，实现了低至2.9的塔板高度，并进行了具有亚秒级峰宽的极快速分离。
