Isolation and structure elucidation of a novel yellow pigment from the marine bacterium Pseudoalteromonas tunicata

The marine environment is a major source for many novel natural compounds. A new yellow pigment has been isolated from the marine bacterium P. tunicata and identified as a new member of the tambjamine class of compounds. The structural identification was achieved by a combination of 1D and 2D-NMR spectroscopy and high resolution mass spectrometry data.     

Quaternary ammonium substituted agarose as surface coating for capillary electrophoresis

A novel positively charged polymer of quaternary ammonium substituted agarose (Q-agarose) has been synthesized and explored for use as a coating in capillary electrophoresis. The fast and simple coating procedure is based on a multi-site electrostatic interaction between the polycationic agarose polymer and the negatively charged fused-silica surface. By simply flushing fused-silica capillaries with hot polymer solution a positively charged, hydrophilic deactivation layer is achieved. The polymer surface provides an intermediate electroosmotic flow of reversed direction, over a range of pH 2-11, compared to unmodified fused-silica. The coating procedure was highly reproducible with an RSD of 4%, evaluated as the electroosmotic flow mobility for 30 capillaries prepared at 10 different occasions. The application of Q-agarose coated capillaries in separation science was investigated using a set of basic drugs and model proteins and peptides. Due to the intermediate electroosmotic flow generated, the resolution of basic drugs could be increased, compared to using bare fused-silica capillaries. Moreover, the coating enabled separation of proteins and peptides with efficiencies up to 300.000 plates m(-1).     

Selective determination of acidic pharmaceuticals in wastewater using molecularly imprinted solid-phase extraction

The determination of acidic pharmaceuticals, such as non-steroidal anti-inflammatory drugs NSAIDs and clofibric acid (metabolite of clofibrate), at low ng L⁻¹ levels in wastewater requires highly selective and sensitive analytical procedures. The removal of matrix components during sample preparation results in significant benefits towards reducing the matrix effects during LC-MS analysis. Therefore this work describes a simple method to enrich and clean up NSAIDs and clofibric acid from sewage water using molecularly imprinted solid-phase extraction (MISPE). Final analysis was performed by liquid chromatography-tandem mass spectrometry. The performance of this method has been evaluated in fortified tap and sewage water in terms of recovery, precision, linearity, and method quantification limit. Recovery for all compounds ranged in all matrices between 84 and 116% with intra-day R.S.D. values below 11.5%. Matrix effect evaluation demonstrated that even complex sample matrixes, such as pond or sewage water did not showed significant ion suppression/enhancement compared to tap water. The performance of the method was further emphasized by the study of pond water, which receives treated water from a sewage treatment plant in south Sweden. Raw sewage and treated water were also tested. In those samples, all acidic pharmaceuticals were detected in concentration above method quantification limits ranging from 5.1 to 5153.0 ng L⁻¹.     

A Cheap One-Pot Approach to Tetraethyl Methylenediphosphonate

A cheap procedure for the preparation of tetraethyl methylene-diphosphonate is described.     

Development and application of an analytical protocol for evaluation of treatment processes for landfill leachates. I. Development of an analytical protocol for handling organic compounds in complex leachate samples

A strategy is presented for evaluation of treatment procedures for landfill leachate with emphasis on organic pollutants. An analytical scheme, the LAQUA protocol, was developed as a guide for the analytical work. The protocol includes organic as well as metals, inorganic ions, water-quality parameters, and toxicity. The proposed strategy considers the behaviour of both polar and non-polar organic substances at trace levels. For polar substances, phenols were chosen as markers and determined with an automated supported liquid membrane extraction device, coupled on-line to HPLC with a diode-array detector. For non-polar substances, PCBs and 10 unidentified compounds were chosen as markers and analysed by solid-phase extraction combined with supercritical fluid extraction with GC analysis. The chosen measurement strategy, based on the use of marker substances, difference measurements, and versatile data-handling procedures, provided essential information about complex systems at relatively low cost.     

Experimental Investigation of Transitional Flow in Porous Media with Usage of a Pore Doublet Model

The transition from laminar to turbulent flow in porous media is studied with a new method. To mimic interconnected pores, a simplified geometry consisting of a pipe with a relatively large diameter that is split into two parallel pipes with different diameters is studied. This is a pore-doublet setup and the pressure drops over the parallel pipes are recorded by pressure transducers for different flow rates. Results show that the flow in the parallel pipes is redistributed when turbulent slugs pass through one of them. The presence of the slugs is revealed by positive skewness in the pressure signals as well as an increase of the standard deviation of the pressure drops and correlation between the pressure drops of the pipes. A frequency analysis of the pressure drops show that lower band frequency pressure variations in one pipe are communicated to the other pipe while higher band frequencies are filtered out.     

Investigation of Post-Darcy Flow in Thin Porous Media

Transport in Porous Media - We present numerical simulations of post-Darcy flow in thin porous medium: one consisting of staggered arrangements of circular cylinders and one random distribution of...     

Transitional and Turbulent Flow in a Bed of Spheres as Measured with Stereoscopic Particle Image Velocimetry

Stereoscopic particle image velocimetry has been used to investigate inertia dominated, transitional and turbulent flow in a randomly packed bed of monosized PMMA spheres. By using an index-matched fluid, the bed is optically transparent and measurements can be performed in an arbitrary position within the porous bed. The velocity field observations are carried out for particle Reynolds numbers, \({Re}_{{p}}\), between 20 and 3220, and the sampling is done at a frequency of 75 Hz. Results show that, in porous media, the dynamics of the flow can vary significantly from pore to pore. At \({Re}_{{p}}\) around 400 the spatially averaged time fluctuations of total velocity reach a maximum and the spatial variation of the time-averaged total velocity, \(u_\mathrm{tot}\) increases up to about the same \({Re}_{{p}}\) and then it decreases. Also in the studied planes, a considerable amount of the fluid moves in the perpendicular directions to the main flow direction and the time-averaged magnitude of the velocity in the main direction, \(u_{x}\), has an averaged minimum of 40% of the magnitude of \(u_\mathrm{tot}\) at \({Re}_{{p}}\) about 400. For \({Re}_{{p}} > 1600\), this ratio is nearly constant and \(u_{x}\) is on average a little bit less than 50% of \(u_\mathrm{tot}\). The importance of the results for longitudinal and transverse dispersion is discussed.     

Nanoparticle‐based capillary electroseparation of proteins in polymer capillaries under physiological conditions

Totally porous lipid‐based liquid crystalline nanoparticles were used as pseudostationary phase for capillary electroseparation with LIF detection of proteins at physiological conditions using unmodified cyclic olefin copolymer capillaries (Topas^®, 6.7 cm effective length). In the absence of nanoparticles, i.e. in CE mode, the protein samples adsorbed completely to the capillary walls and could not be recovered. In contrast, nanoparticle‐based capillary electroseparation resolved green fluorescent protein from several of its impurities within 1 min. Furthermore, a mixture of native green fluorescent protein and two of its single‐amino‐acid‐substituted variants was separated within 2.5 min with efficiencies of 400 000 plates/m. The nanoparticles prevent adsorption by introducing a large interacting surface and by obstructing the attachment of the protein to the capillary wall. A one‐step procedure based on self‐assembly of lipids was used to prepare the nanoparticles, which benefit from their biocompatibility and suspension stability at high concentrations. An aqueous tricine buffer at pH 7.5 containing lipid‐based nanoparticles (2% w/w) was used as electrolyte, enabling separation at protein friendly conditions. The developed capillary‐based method facilitates future electrochromatography of proteins on polymer‐based microchips under physiological conditions and enables the initial optimization of separation conditions in parallel to the chip development.