Amino acid analysis of honey by high-performance liquid chromatography (HPLC) was used first to discriminate different botanical origins and then to combat adulteration. Pure honeys of seven selected floral varieties were examined. A principal component analysis (PCA) was carried out on the results after selection of the most discriminating parameters. Lavender honeys were thus perfectly characterized, but complete satisfaction was not obtained with the six other varieties. This method (analysis by HPLC and statistical processing by PCA) enabled us to detect the addition of sugar syrup to rape and fir honeys.
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.
The beneficial effects of high temperature on separation and detection of basic compounds, the detection being performed by MS via ESI, are investigated. The influence of various parameters on both separation and detection performances is studied. These parameters include the mobile phase pH, the temperature, and the type of stationary phase. Experiments are performed under gradient elution conditions. The results obtained with four different supports, silica-, zirconia-, carbon-, and polymer-based columns, are compared by means of different criteria including the elution composition, the peak asymmetry, and the S/N. High temperature liquid chromatography at high pH with volatile buffers suitable for MS detection was shown to be an interesting choice for solutes with basic sites.
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