Untersuchung von Kaffee und Kaffee-Ersatzstoffen

Ohne Zusammenfassung     

GC-MS and HPLC analyses of lignin degradation products in biomass hydrolyzates

Summary The gas-chromatographic separation of lignin degradation products of hydrolytically degraded biomass (e. g. poplar wood) and their mass spectrometric identification are described. For routine analysis of lignin degradation products of biomass hydrolyzates, a time saving HPLC gradient method using a UV-detection system (280 nm), is described. In addition to reference samples, solutions of hydrothermally degraded biomass were analyzed.

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GC-MS- und HPLC-Analytik von Ligninabbauprodukten in Biomassehydrolysaten

Zusammenfassung Die gas-chromatographische Trennung von Ligninabbauprodukten nach hydrolytischer Spaltung von Biomasse (z.B. Pappelholz) sowie die massenspektrometrische Identifizierung werden beschrieben. Für eine routinemäßige Analytik der Ligninabbauprodukte in Biomassehydrolysaten wird weiterhin die Trennung mittels einer Gradienten-HPLC-Methode aufgezeigt. Die Detektion erfolgte bei 280 nm. Neben Referenzproben wurden hydrothermale Abbaulösungen untersucht.

     

The quadrupole moment of the neutron-halo nucleus11Li

The quadrupole moment ratio of⁹Li and¹¹Li was measured by a combination of in-beam laser induced nuclear polarization and Β-NMR in LiNbO₃. The result ¦Q(¹¹Li)/Q(⁹Li)¦=1.14(16) is consistent with cluster models describing¹¹Li as composed of a⁹Li core and a far extended halo of two loosely bound neutrons.     

Gels and glasses in a single system: evidence for an intricate free-energy landscape of glassy materials

In the free-energy landscape picture of glassy systems, their slow dynamics is due to a complicated free-energy landscape with many local minima. We show that for a colloidal glassy material multiple paths can be taken through the free-energy landscape. The evolution of the nonergodicity parameter shows two distinct master curves that we identify as gels and glasses. We show that for a range of colloid concentrations, the transition to nonergodicity can occur in either direction (gel or glass), accompanied by "hesitations" between the two. Thus, colloidal gels and glasses are merely global free-energy minima in the same free-energy landscape, and the paths leading to these minima can be complicated.     

Poly(N-vinylimidazole/ethylene glycol dimethacrylate) for the purification and isolation of phenolic acids

In this study we report the novel polymeric resin poly(N-vinyl imidazole/ethylene glycol dimethacrylate) for the purification and isolation of phenolic acids. The monomer to crosslinker ratio and the porogen composition were optimized for isolating phenolic acids diluted in acetonitrile at normal phase chromatography conditions, first. Acetonitrile serves as polar, aprotic solvent, dissolving phenolic acids but not interrupting interactions with the stationary phase due to the approved Hansen solubility parameters. The optimized resin demonstrated high loading capacities and adsorption abilities particularly for phenolic acids in both, acetonitrile and aqueous solutions. The adsorption behavior of aqueous standards can be attributed to ion exchange effects due to electrostatic interactions between protonated imidazole residues and deprotonated phenolic acids. Furthermore, adsorption experiments and subsequent curve fittings provide information of maximum loading capacities of single standards according to the Langmuir adsorption model. Recovery studies of the optimized polymer in the normal-phase and ion-exchange mode illustrate the powerful isolation properties for phenolic acids and are comparable or even better than typical, commercially available solid phase extraction materials. In order to prove the applicability, a highly complex extract of rosemary leaves was purified by poly(N-vinyl imidazole/ethylene glycol dimethacrylate) and the isolated compounds were identified using UHPLC–qTOF-MS.     

Zirconium silicate assisted removal of residual proteins after organic solvent deproteinization of human plasma,enhancing the stability of the LC–ESI-MS response for the bioanalysis of small molecules

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.