Monolithic stationary phases styrene monoliths

Table 1.1 gives a comprehensive, albeit fragmentary, snmmary of investigated organic monolithic polymer systems (based on all different kinds of styrene, acrylate, methacrylate, (meth)acrylam-ide building blocks, as well as mixtnres thereof) together with their preparation conditions and ntilization as stationary phase. 

A monolithic silica-based CIS stationary phase was used under high flow rate condition (2 mL/min) without significant back pressure in IPC analysis of a recently discovered new drug candidate for the treatment of Alzheimer s disease [15]. Nanoscale IPC using a monolithic poly(styrene-divinylbenzene) (PS-DVB) nanocolumn coupled to nanoelectrospray ionization mass spectrometry (nano-ESl-MS) was evaluated to separate and identify isomeric oligonucleotide adducts. Triethylammonium bicarbonate was used as the IPR. Interestingly, the performance of the polymeric monolithic PS-DVB stationary phase significantly surpassed that of columns packed with the microparticulate sorbents CIS or PS-DVB [16]. 

Trojer, L. et al. Monolithic poly(p-methylstyrene-co-l,2-bis(p-vinylphenyl)ethane) capiUary columns as novel styrene stationary phases for biopolymer separation. J. Chromatogr. A. 2006, 1117, 56-66. 

A typical mobile-phase composition is an acetonitrile-water gradient with a fixed concentration of trifluoroacetic acid (TFA), formic, or acetic acid (typically 0.05-0.5%). TFA acts as an ion-pairing agent and masks secondary interactions with the silica-based stationary phase. TFA may significantly suppress the ESI response in positive-ion mode. To avoid this, either formic acid is preferred or a mixture of 0.02% TFA and 0.5% acetic acid can be used. Some silica-based RPLC materials can be used with a lower TFA concentration (PepMap ). Alternatively, poly(styrene-divinylbenzene) polymeric materials (PS-DVB) can be applied. With a monolithic PS-DVB column, only a small decrease in separation efficiency on the monolithic column was observed when the TFA concentration was reduced from 0.2%to0.05%[51]. 

The very good performance of molded polymeric stationary phases in HPLC and CEC at high flow rates is especially important when sensitive biomolecules are separated. Thus, the reversed-phase separation of five proteins was easily achieved in less than 20 s on a styrene—DVB rod with an optimized porous structure [405]. The extensive use of molded polymeric monoliths as stationary phases in HPLC and CEC demonstrated within the last decade their wide applicability and many inherent... 

Xiong, B. etal. Capillary electrochromatography with monolithic poly(styrene-co-divinylbenzene-co-methacrylic acid) as the stationary phase, J. High Resol. Chromatogr., 23, 67, 2000. 

More recently, columns have been developed where the stationary phase is formed of a porous polymer network inside the capillary. These are called monolithic phases, and have emerged as an alternative to traditional packed bed columns for use in micro-HPLC. They hold many advantages over traditional packed bed columns, being easy to manufacture since the monolith is formed in situ, often via a one-step reaction process, and its properties such as porosity, surface area, and functionality can be tailored. Another major advantage is that they eliminate the need for retaining frits. These columns can be manufactured from a variety of materials, but the most common include sol-gel, methacrylate-based, acrylamide-based, and styrene-based polymeric structures. 

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