Fast liquid chromatography combined with mass spectrometry for the analysis of metabolites and proteins in human body fluids

In the last decade various analytical strategies have been established to enhance separation speed and efficiency in high performance liquid chromatography applications. Chromatographic supports based on monolithic material, small porous particles, and porous layer beads have been developed and commercialized to improve throughput and separation efficiency. This paper provides an overview of current developments in fast chromatography combined with mass spectrometry for the analysis of metabolites and proteins in clinical applications. Advances and limitations of fast chromatography for the combination with mass spectrometry are discussed. Practical aspects of, recent developments in, and the present status of high-throughput analysis of human body fluids for therapeutic drug monitoring, toxicology, clinical metabolomics, and proteomics are presented.     

Quantitative characterization of individual particle surfaces by fractal analysis of scanning electron microscope images

Morphological characterization of individual particle surfaces was explored by off-line image processing of data obtained by scanning electron microscope — microanalyzer. The fractal geometry was studied by two methods, the power spectrum and the variogram approach. Both methods were evaluated, theoretically by a series of numerically simulated surface profiles and experimentally on a set of pre-recorded secondary electron images of particle surfaces exposing characteristic textures. It was shown that the fractal approach could stand as a base of the methods enlarging the application of electron probe X-ray microanalyzers for individual particle characterization.Dedicated to Professor Dr. Dieter Klockow on the occasion of his 60th birthday On leave from: State Pedagogical Institute, Kirovograd, Ukraine     

Modelling variations in hospital service delivery based on real time locating information

Variations in service delivery have been identified as a major challenge to the success of process improvement studies in service departments of hospital such as radiology. Largely, these variations are due to inherent system level factors, i.e., system variations such as unavailability of resources (nurse, bed, doctors, and equipment). These system variations are largely unnecessary/unwarranted and mostly lead to longer waiting times, delays, and lowered productivity of the service units. There is limited research on identifying system variations and modelling them for service improvements within hospital. Therefore, this paper proposes a modelling methodology to model system variations in radiology based on real time locating system (RTLS) tracking data. The methodology employs concepts from graph theory to identify and represent system variations. In particular, edge coloured directed multi-graphs (ECDMs) are used to model system variations which are reflected in paths adopted by staff, i.e., sequence of rooms/areas traversed while delivering services. The main steps of the methodology are: (i) identifying the most standard path followed by staff for service delivery; (ii) filtering the redundant events in RTLS tracking database for analysis; (iii) identifying rooms/areas of hospital site involved in the service delivery; (iv) determining patterns of paths adopted by staff from filtered tracking database; and, (v) representation of patterns in graph based model called as edge coloured directed multigraphs (ECDMs) of a role. A case study of MR scanning process is utilized to illustrate the implementation of the proposed methodology for modelling system variations reflected in the paths adopted by staff.     

Temperature gradient spectra and temperature dissipation rate in a turbulent convective flow

Determining mixing coefficients in oceanographic flows relies on the form of temperature gradient spectra in turbulent water flows at large wavenumbers. Several recent investigations concluded that these spectra are best described by the functional form proposed by Kraichnan rather than by the Batchelor form, more commonly used in oceanography. In this study, we provide additional support for this conclusion using laboratory measurements of the temperature gradient spectra in a Rayleigh–Bénard convective cell, in order to avoid difficulties inherent in oceanographic field measurements. The range of Rayleigh numbers in experiments is between Ra = 3×10⁷ and Ra = 5×10⁹. In addition to a traditional method of traversing thermistors, a novel optical technique recently introduced for oceanic measurements was used to obtain the spectra; comparison between these two methods serves as a validation test for the new optical technique. The temperature measurements were also augmented by 2D particle image velocimetry (PIV) observations. The measured dependence of the Nusselt number on the Rayleigh number followed Nu ∝ Ra^0.29 at Pr = 6 and was consistent with the literature data. We observed the temperature dissipation rate to vary by an order of magnitude over a horizontal transect at Ra > 10⁹. The temperature dissipation spectra obtained by both methods were in agreement over the Ra interval considered. The location of the temperature dissipation peaks was also consistent with PIV measured energy dissipation rates. Our data suggest increasing importance of top/bottom boundaries for the momentum and the temperature dissipation with increasing Ra number. Applied to oceanic upper ocean convection, our results imply that most of the dissipation occurs close to the air–sea boundary. Thus, attempts to parameterise or measure air–sea turbulent convective fluxes have to reflect the dominant role of near boundary dissipation at large Ra.     

Microwave-assisted synthesis of substituted hexahydro-pyrrolo[3,2-c]quinolines

New compounds with the ethyl hexahydro-1H-pyrrolo[3,2-c]quinoline-2-carboxylate skeleton were prepared by microwave-assisted intramolecular 1,3-dipolar cycloaddition reactions. The reactions were carried out under solvent-free conditions and compared with the same reaction in the presence of a solvent and a catalyst. Steric effects on the selectivity of the reaction were noted and evaluated.     

Peculiarities of luminescent properties of cerium doped YAG transparent nanoceramics

Optical and luminescence properties of transparent nanosized cerium doped Y₃Al₅O₁₂ (YAG:Ce) ceramics have been studied. YAG:Ce nanoceramics were obtained by means of low temperature and high pressure (LTHP) sintering method. Nanoceramic samples were sintered in the 2–8 GPa pressure range, whereas Ce³⁺ concentration was varied in the 0.5–5 at. % range. It is shown that, in contrast to the single crystal, a strong rise of absorption coefficient was detected already at wavelength shorter than 400 nm in all nanoceramic samples studied. Furthermore, in nanoceramic samples unusual UV emission band near 3.1 eV was observed, which is not observed in the YAG:Ce single crystal. High pressure applied during nanoceramics sintering leads to significant changes in their optical and luminescence properties.     

Determination of linear alkylbenzenesulfonates in communal wastewater by means of solid phase microextraction coupled with API-MS and HPLC-FLD

The use of Solid Phase Microextraction (SPME) for the qualitative and quantitative determination of Linear Alkylbenzenesulfonates (LAS) in waste water samples was investigated. A Carbowax/Templated Resin (CW/?TPR) coated fiber was directly immersed into influent and effluent samples of a sewage treatment plant (STP). Extraction conditions such as time, pH, ion strength were investigated. The extracted LAS were desorbed with a solvent in a specially designed SPME-LC interface for analysis with HPLC-FLD and Electrospray Ionization Mass Spectrometry (ESI-MS). The combination of SPME with ESI-MS proved to be an alternative technique for the LAS determination in waste water. Linear ranges of the external calibration were found from 0.5–100 ng/mL, with detection limits of 0.5 ng/mL for each individual LAS homologue. The reproducibility of the method is 15% (relative standard deviation). Received: 3 May 1999 / Revised: 22 July 1999 / Accepted: 24 July 1999     

Determination of linear alkylbenzenesulfonates in communal wastewater by means of solid phase microextraction coupled with API-MS and HPLC-FLD

The use of Solid Phase Microextraction (SPME) for the qualitative and quantitative determination of Linear Alkylbenzenesulfonates (LAS) in waste water samples was investigated. A Carbowax/Templated Resin (CW/¶TPR) coated fiber was directly immersed into influent and effluent samples of a sewage treatment plant (STP). Extraction conditions such as time, pH, ion strength were investigated. The extracted LAS were desorbed with a solvent in a specially designed SPME-LC interface for analysis with HPLC-FLD and Electrospray Ionization Mass Spectrometry (ESI-MS). The combination of SPME with ESI-MS proved to be an alternative technique for the LAS determination in waste water. Linear ranges of the external calibration were found from 0.5–100 ng/mL, with detection limits of 0.5 ng/mL for each individual LAS homologue. The reproducibility of the method is 15% (relative standard deviation).