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Preparative two-dimensional chromatography is gaining interest in the elucidation of complex samples as it allows the recovery of a large number of molecules without the risks inherent to tedious multi-step sample preparation. While the second dimension is often selected to be liquid chromatography, it may be of interest to compare the specificities of two different techniques, namely liquid chromatography and centrifugal partition chromatography, to be used as first dimension. A fair comparison between off-line CPCxLC and prepLCxLC in selective comprehensive mode for preparative purposes is carried out in this study, illustrated by the isolation of five compounds from high-value Edelweiss plant. The method development of each configuration is achieved on laboratory scale instruments. The quality of separation is compared using 2D-contour plots. The prepLCxLC exhibits a large separation space that leads to an overall large peak capacity, which is of great interest for complex samples. But its limited loading capacity involves a large number of 2 D runs increasing the running costs for preparative purposes. On the other hand, CPCxLC provides a low peak capacity due to the poor efficiency provided by CPC. However, this liquid-liquid technique can be finely tuned to generate a high selectivity, decreasing the number of runs necessary to produce a limited number of target solutes., (© 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

This article shows that there is great interest in using an electrochromatographic microchip made of hexyl acrylate (HA) based porous monolith cast within the channel of a cyclic olefin copolymer (COC) device. The monolith is simultaneously in situ synthesized and anchored to the inner walls of the channel in less than 10 min. By appropriate choice of light intensity used during the synthesis, the separation efficiency obtained for nonpolar solutes such as polycyclic aromatic hydrocarbons (PAH) is increased up to 250 000 plates/m. The performance of this HA-filled COC microchip was investigated for a wide range of analytes of varying nature. The reversed-phase separation of four aflatoxins is obtained in less than 2 min. The baseline separation of a mixture of neurotransmitters including six amino acids and two catecholamines is possible thanks to the superimposition of the differences in electrophoretic mobility on the chromatographic process. The durability of the system at pH 13 allows the separation of five biogenic amines and the quantitative determination of two of them in numerous wine samples. The feasibility of on-line preconcentration is also demonstrated. Hydrophilic surface modification of COC channel via UV-photografting with poly(ethylene glycol) methacrylate (PEGMA) before in situ synthesis of HA, is necessary to reduce the adsorption of very hydrophobic solutes such as PAH during enrichment. The detection limit of fluoranthene is decreased down to less than 1 ppb with a preconcentration of 4.5 h on the HA-filled PEGMA functionalized COC microchip., (© 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

LC is one of the most powerful separation techniques as illustrated by its leading role in analytical sciences through both academic and industrial communities. Its implementation in microsystems appears to be crucial in the development of mu-Total Analysis System. If electrophoretic techniques have been widely used in miniaturized devices, LC has faced multiple challenges in the downsizing process. During the past 5 years, significant breakthroughs have been achieved in this research area, in both conception and use of LC on chip. This review emphasizes the development of novel stationary phases and their implementation in microchannels. Recent instrumental advances are also presented, highlighting the various driving forces (pressure, electrical field) that have been selected and their respective ranges of applications.

An acrylate monolith has been synthesized into a cyclic olefin copolymer microdevice for reversed-phase electrochromatography purposes. Microchannels, designed by hot embossing, were filled up with an acrylate monolith to serve as a hydrophobic stationary phase. A lauryl acrylate monolith was formulated to suit the hydrophobic material, by implementing 100% organic porogenic solvent. This new composition was tested in capillary prior to its transfer into the microfluidic device. Surface functionalization of the cyclic olefin copolymer surface was applied using UV-grafting technique to improve the covalent attachment of this monolith to the plastic walls of the microfluidic chip. The on-chip performances of this monolith were evaluated in detail for the reversed-phase electrochromatographic separation of polycyclic aromatic hydrocarbons, with plate heights reaching down to 10 microm when working at optimal velocity.

This paper shows the in situ synthesis of an hexyl acrylate monolith in PDMS microfluidic devices and its subsequent use as stationary phase for electrochromatography on chip. To overcome the ability of PDMS material to absorb organic monomers, surface modification of the enclosed channels was realized by UV-mediated graft polymerization. This grafting procedure is based on the preliminary adsorption of a photoinitiator onto the PDMS surface and polymerization of charged monomers. Next, hexyl acrylate monoliths were cast in situ using photopolymerization process. The chromatographic behavior of the monolithic column was confirmed by the successful separation of derivatized catecholamines in the PDMS device using a 30 mm effective separation length (100 microm x 100 microm section). Efficiencies reached up to 200,000 plates per meter.