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41.
Shah Hussain Cornelia Pezzei Yüksel Güzel Matthias Rainer Christian W. Huck Günther K. Bonn 《Analytica chimica acta》2014
An efficient blood plasma clean-up method was developed, where methanol protein precipitation was applied, followed by zirconium silicate assisted exclusion of residual proteins. A strong binding of zirconium (IV) silicate to the proteins enabled the elimination of remaining proteins after solvent deproteinization through a rapid solid-phase extraction (SPE) procedure. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI/TOF MS) was used for monitoring the proteins during clean-up practice applied to human plasma samples. The proteins were quantified by colorimetric detection using the bicinchoninic acid (BCA) assay. The presented analytical strategy resulted in the depletion of >99.6% proteins from human plasma samples. Furthermore, high-performance liquid chromatography hyphenated to diode-array and electrospray ionization mass spectrometric detection (HPLC–DAD/ESI MS) was applied for qualitative and quantitative analysis of the caffeoylquinic acids (CQAs) and their metabolites in human plasma. The procedure demonstrated high recoveries for the standard compounds spiked at different concentrations. Cynarin and chlorogenic acid were recovered in the range of 81–86% and 78–83%, respectively. Caffeic acid was extracted in the excess of 89–92%, while ferulic acid and dihydroxyhydrocinnamic acid showed a recovery of 87–91% and 92–95%, respectively. The method was partially validated in accordance with FDA-Industry Guidelines for Bioanalytical Method Validation (2001). The presented scheme improves the clean-up efficacy of the methanol deproteinization, significantly reduces the matrix effects and provides a great analytical tool for the isolation of small molecules from human plasma. 相似文献
42.
We report the vibrational and orientational dynamics of water molecules in isotopically diluted NaOH and NaOD solutions using polarization-resolved femtosecond vibrational spectroscopy and terahertz time-domain dielectric relaxation measurements. We observe a speed-up of the vibrational relaxation of the O-D stretching vibration of HDO molecules outside the first hydration shell of OH(-) from 1.7 ± 0.2 ps for neat water to 1.0 ± 0.2 ps for a solution of 5 M NaOH in HDO:H(2)O. For the O-H vibration of HDO molecules outside the first hydration shell of OD(-), we observe a similar speed-up from 750 ± 50 fs to 600 ± 50 fs for a solution of 6 M NaOD in HDO:D(2)O. The acceleration of the decay is assigned to fluctuations in the energy levels of the HDO molecules due to charge transfer events and charge fluctuations. The reorientation dynamics of water molecules outside the first hydration shell are observed to show the same time constant of 2.5 ± 0.2 ps as in bulk liquid water, indicating that there is no long range effect of the hydroxide ion on the hydrogen-bond structure of liquid water. The terahertz dielectric relaxation experiments show that the transfer of the hydroxide ion through liquid water involves the simultaneous motion of ~7 surrounding water molecules, considerably less than previously reported for the proton. 相似文献
43.
Muhammad Nasimullah Qureshi Guenther Stecher Christian Huck Guenther K. Bonn 《Central European Journal of Chemistry》2011,9(2):206-212
This article discusses the preparation of different polymeric sorbents for solid phase extraction. Various monomers like acrylamide,
methacrylic acid and 4-vinylpyridine (VP), cross-linkers such as divinylbenzene (DVB) and ethyleneglycoldimethacrylate (EDMA),
porogens like tetrahydrofuran (THF) and dimethylsulphoxide (DMSO) / acetonitrile (ACN) with different ratios were investigated
in order to optimize recoveries. Resulting polymers were characterized through scanning electron microscope (SEM) and compared
with Oasis HLB (Waters, MA, USA) and Strata-X (Phenomenex, Torrance, USA) on the basis of extraction performance, recovery
efficiency and loading capacity. Sample applied was a mixture of flavonoid standards (rutin, myricetin, luteolin, quercetin,
apigenin and kaempferol). HPLC hyphenated with PDA was used for the analysis of samples. Results showed that among the prepared
SPE materials, 4-VP-co-EDMA produced best results. Comparison of the produced polymers with of Oasis HLB and Strata-X resulted
in comparable efficiencies; especially the polymer 4-VP-co-EDMA gave almost similar results for all analytes to those of commercially
available SPE materials. A general trend of decrease in retention efficiency with increase in polarity has been observed in
both synthesized and already available SPE materials. The newly synthesized polymeric materials can be employed as SPE sorbents
for efficient extraction of polyphenolic compounds especially for flavonoid aglycons. 相似文献
44.
Summary The present study deals with the isotachophoretic and the ion chromatographic analysis of organic acids found in hydrolysates of lignocellulosic biomass. The samples were pretreated by means of ultrafiltration to increase the reproducibility of the measurements. The qualitative and quantitative analysis of the fractions obtained during hydrothermal and organosolv degradations of wheat straw allowed a comparison of the rate and amount of organic acids formed (formic acid, glycolic acid, lactic acid, acetic acid). Isotachophoresis facilitates research on the reaction mechanisms underlying the hydrolysis of biomass.
Analyse der durch Hydrothermolyse und Organosolv-Aufschluß von lignocellulosehaltiger Biomasse gebildeten organischen Säuren相似文献
45.
E. Arnold J. Bonn W. Neu R. Neugart E. W. Orten The Isolde Collaboration 《Zeitschrift für Physik A Hadrons and Nuclei》1988,331(3):295-298
The quadrupole interaction of nuclear spin polarized8Li (I=2) and9Li (I=3/2) in LiNbO3 has been studied at room temperature. The polarization was achieved by optical pumping of a fast atomic beam with circularly polarized laser light. The atoms were implanted into a hexagonal LiNbO3 single crystal and the quadrupole splitting ofβ-NMR spectra was measured. A ratio of ¦Q(9Li)/Q(8Li)¦=0.88(4) for the nuclear quadrupole moments was deduced, yielding a new value of ¦Q(9Li)¦=25.3 (9) mb for the quadrupole moment of9Li. 相似文献
46.
Combining the effects of electrophoresis and electroendosmosis, flavonoids were separated in less than ten minutes in a fused silica capillary tube with a borate buffer adjusted to pH 10. An increase in the concentration of borate from 0.1 to 0.2 M resulted in longer migration times due to a decrease in electroosmotic flow, but also in improved selectivity and higher resolution of flavonoids. The calibration curve of rutin showed a detection limit of 0.02 mg/mL and linearity over its pharmaceutical concentration range. Using an internal standard of known concentration, the content of rutin in a methanolic extract of Sambuci flos could be determined with a coefficient of variation as small as 3.8% by the molar ratio-peak area ratio method. 相似文献
47.
Molar extinction coefficients of some carbohydrates viz. l-arabinose (C5H10O5), d-glucose (C6H12O6), d-mannose (C6H12O6), d-galactose (C6H12O6), d(-) fructose (C6H12O6) and maltose (C12H24O12) in aqueous solutions have been determined at 81, 356, 511, 662, 1173 and 1332 keV by gamma ray transmission method in a
narrow beam good geometry set-up. These coefficients have been found to depend upon the photon energy following a 4-parameter
polynomial. These extinction coefficients for different sugars having the same molecular formula have same values varying
within experimental uncertainty. Within concentration ranges studied, Beer-Lambert law is obeyed very well. 相似文献
48.
49.
50.
Stasyk T Morandell S Bakry R Feuerstein I Huck CW Stecher G Bonn GK Huber LA 《Electrophoresis》2005,26(14):2850-2854
Here we combine a standard two-dimensional difference gel electrophoresis (DIGE) protocol with subsequent post-staining of gels with phosphospecific fluorescent Pro-Q Diamond dye. The combination of these two methods for fluorescence detection of proteins allows quantitative detection of phosphoproteins in 2-DE-gels. We established this protocol within a functional proteomics experiment. Mammary epithelial cells (EpH4) were stimulated in culture by epidermal growth factor (EGF), endosomal fractions prepared after subcellular fractionation and phosphorylated proteins successfully detected on endosomes. For instance, Endo A cytokeratin, known as phosphoprotein and differentiation marker inducible by MAPK signaling, was identified by matrix-assisted laser desorption/ionization-time of flight-mass spectrometry (MALDI-TOF-MS). With this protocol, all steps of combined proteome and phosphoproteome profiling experiments are significantly simplified and accelerated, taking full advantage of both methods in terms of specificity, sensitivity and accuracy of quantification. 相似文献