Biomedical subjects

H Händel

Publications and source records attributed to H Händel.

4 recordsLinked to original sources

PubMed2001

Study on the chiral recognition of the enantiomers of ephedrine derivatives with neutral and sulfated heptakis(2,3-O-diacetyl)-beta-cyclodextrins using capillary electrophoresis, UV, nuclear magnetic resonance spectroscopy and mass spectrometry.

The enantiomers of methylephedrine, pseudoephedrine and ephedrine showed a different migration behavior in capillary electrophoresis in the presence of beta-cyclodextrin (beta-CD), heptakis(2,3-O-diacetyl)-beta-cyclodextrin and heptakis(2,3-O-diacetyl-6-sulfato)-beta-cyclodextrin (HDAS). Utilizing UV, MS and NMR spectroscopy, in particular rotating frame Overhauser experiments, an attempt was made to elucidate the chiral recognition mechanism. In the case of the neutral CDs 1:1 complexes were formed with ephedrine and methylephedrine characterized by the inclusion of the phenyl ring in the cavity and the side chain pointing out of the wider rim. In contrast, manifold complexes were formed with HDAS, which on average are characterized by an upside down inclusion of the phenyl ring in the cavity and the side chain pointing out of the narrow rim. This complex geometry is likely be stabilized by an ion-ion interaction between the positively charged nitrogens of the ephedrine derivatives and the negative charges of HDAS. In addition, an attachment of the ligand to the outside of HDAS and other complex stoichiometries are also possible.

Cyclodextrins↗

PubMed2000

New stationary phase for liquid chromatography with chemically bonded pinane ligand: synthesis and characterization by nuclear magnetic resonance and high-performance liquid chromatographic investigations.

A new bicyclic phase for liquid chromatography was prepared by solution polymerization approaches. To introduce a C4 spacer the starting molecule 3-formylpinane was reduced to the alcohol followed by a substitution of the hydroxy group through a bromide. The obtained halide reacted with magnesium and allyl bromide to the 3-(but-3'-enyl)pinane which was hydrosilylated with trichlorosilane and finally immobilized to silica gels with different pore sizes using the technique of solution polymerization. To elucidate the structure of 3-(but-3'-enyl)pinane high-resolution two-dimensional nuclear magnetic resonance (NMR) spectra were carried out. The new phases were characterized, on the one hand by employing 13C and 29Si solid-state NMR spectroscopy and on the other hand, by separating a standard test mixture consisting of mainly monosubstituted aromatic compounds. The results achieved in chromatography were correlated with the information gained from 29Si CP/MAS NMR measurements.

Bicyclic Monoterpenes↗

PubMed2000

Characterization of polyalkylvinyl ether phases by solid-state and suspended-state nuclear magnetic resonance investigations.

Pure organic polyalkvlvinyl ether phases were synthesized by suspension polymerization using different ratios and compositions of n-butylvinyl ether (C4VE) and n-octadecylvinyl ether (C18VE) with triethylene glycol divinyl ether or divinylbenzene as crosslinkers, respectively. These phases were investigated by means of solid-state 13C cross-polarization magic angle spinning nuclear magnetic resonance (NMR) spectroscopy and 1H high-resolution magic angle spinning (HR MAS) NMR spectroscopy in suspended-state. A comparison of these two methods showed the substantial advantages of 1H HR MAS NMR measurements. Structure elucidation was achieved using a 2D H,H-COSY NMR experiment performed under MAS conditions enabling full peak assignment of the 1H NMR spectra of these phases. The dynamic behavior of the polyalkylvinyl ether phases was determined by employing temperature-dependent measurements of spin-lattice relaxation times (T1) as well as accumulation of a 2D wide line separation NMR spectrum.

Magnetic Resonance Spectroscopy↗

PubMed1997

Stationary interphases with extended alkyl chains: a comparative study on chain order by solid-state NMR spectroscopy.

Stationary interphases with long n-alkyl chains (n = 18, 22, 30, 34) have been examined by solid-state NMR spectroscopy. The determination of the silane functionality and the degree of cross-linking of silane ligands on the silica surface was performed by 29Si CP/MAS NMR spectroscopy. High-speed 1H MAS and 13C CP/MAS NMR spectroscopy were utilized to assess alkyl chain order and mobility of the different bonded phases. For this purpose, 1H NMR line widths and 13C chemical shifts have been evaluated. It is shown that stationary phase order and rigidity increase with alkyl chain length. In addition, the temperature-dependent trans/gauche conformational change occurs at higher temperatures for a polymeric C34 phase compared with a C30 sorbent. This behaviour is discussed in the context of previously reported chromatographic (HPLC) shape selectivity differences.

Carbon Isotopes↗