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At least 901 records · Page 50Linked to original sources
PubMed1985

Determination of polysaccharide linkage and branching by reductive depolymerization. Gas-liquid chromatography and gas-liquid chromatography-mass spectrometry reference data.

A series of partially methylated anhydro-D-alditol acetates has been prepared and analyzed by g.l.c. and g.l.c.-m.s. The reference compounds were obtained by reductive cleavage of permethylated and partially methylated standard methyl glycosides, and standard di-, tri-, and tetra-saccharides of known composition and linkage. Structural characterization included retention times on g.l.c. using DB-225 capillary columns and mass spectrometry in both the chemical- and electronionization modes. This compiled library allows further evaluation of the applicability of the reductive cleavage procedure for determining linkage or branching (or both) of new and more complex oligosaccharides. The technique has been applied to microgram amounts of a bacterial-membrane oligosaccharide and to a saccharide obtained from the urine of a mannosidosis patient. The procedures are simple, reliable, and applicable to small amounts of isolated biological materials.

Acetylation↗
PubMed2000

Efficiency through combining high-performance liquid chromatography and high resolution gas chromatography: progress 1995-1999.

Progress during the last 5 years in on-line LC-GC and related techniques is reviewed. In normal-phase LC-GC, the wire interface proved to have advantages over the loop type interface. Further investigations on the solvent evaporation process in an uncoated precolumn under conditions of an early vapour exit revealed that the rules for the transfer by the retention gap techniques must be modified. For reversed-phase LC-GC, approaches with a phase transfer compete with direct evaporation. Eluents were extracted into a bed of Tenax located in a programmed-temperature vaporiser and thermally desorbed. Direct evaporation is possible when a hot vaporising chamber is used and solvent/solute separation occurs in a separate compartment, a coated precolumn possibly in combination with packed beds. As a future strategy, LC-GC transfer techniques should be adjusted to those of large volume injection and involve a single device. It is believed that on-column injection/transfer is the choice. This requires that concurrent evaporation in LC-GC is performed by the on-column interface.

Chromatography, Gas↗
PubMed2000

Comparative study on camphor enantiomers behavior under the conditions of gas-liquid chromatography and reversed-phase high-performance liquid chromatography systems modified with alpha- and beta-cyclodextrins.

The dependence of retention and selectivity parameters of camphor enantiomers on the concentration of alpha- and beta-cyclodextrins were studied under conditions of GLC (matrix solvent: Glycerol, 95 degrees C) and RP-HPLC (matrix solvent: Aqueous methanolic, 20 degrees C). It has been found that beta-cyclodextrin forms complex of 1:1 stoichiometry and does not recognize enantiomers of camphor. In contrast alpha-CD forming complexes of 1:2 stoichiometry appeared to be very efficient chiral selector of (+) and (-)-camphor. Relatively considerable differences have been observed between stability constants determined by GLC and RP-HPLC, what may be explained by the various natures of the matrix solvents and the various temperatures of the measurements. On the contrary, the enantioseparation factor alpha observed at higher concentrations of alpha-cyclodextrin stabilizes on the very similar value alpha+/-(GLC) approximately = alpha-/+(HPLC) approximately = 1.6. Simple theoretical considerations focusing on the differences in the mechanisms of the studied processes have been performed. According to them the enantiomer forming the more stable complex with the cyclodextrin should be eluted from the RP-HPLC column first and GLC column last. This fact has been confirmed experimentally.

Antipruritics↗
PubMed2000

Analysis of tetramethylpyrazine in Ephedrae herba by gas chromatography-mass spectrometry and high-performance liquid chromatography.

A simple and reliable HPLC method was developed for the determination of 2,3,5,6-tetramethylpyrazine (TMP) in Ephedrae herba. Further identification of TMP was achieved using GC-MS. The mobile phase used was methanol-water-35% acetic acid (35:65:0.5, v/v/v) at a flow-rate of 0.8 ml/min. The detection wavelength was set at 290 nm. The linear range of the peak area calibration curve of TMP was 2.64-264 mg/l (r=0.9987) and the recovery for TMP in Ephedrae herba extracts was 101.1-106.9%. The relative standard deviations of retention time and peak area were 0.18 and 1.5% (n=6), respectively. The detection limit of TMP was 0.03 mg/l. The contents of TMP in Ephedrae herba could easily be determined within 10 min.

Calibration↗
PubMed2000

Separation of coumarins from Archangelica officinalis in high-performance liquid chromatography and thin-layer chromatography systems.

Complex, multicomponent mixtures are difficult to separate in a single chromatographic run. Therefore, the possibility to separate twelve coumarins from Archangelica officinalis was studied by combining a HPLC and a TLC system. HPLC optimized by the use of DryLab for Windows software was performed on RP-18 column and TLC was performed on silica plates. Fractions from the RP column were evaporated, applied on silica plate and developed in non-aqueous solvent. Possibilities of complete separation of investigated coumarins were discussed in RP and NP systems. The result of their complete separation was presented by HPLC chromatograms, DryLab simulated chromatograms and a video scan of TLC plate.

Chromatography, High Pressure Liquid↗
PubMed2000

Analysis of olive and hazelnut oil mixtures by high-performance liquid chromatography-atmospheric pressure chemical ionisation mass spectrometry of triacylglycerols and gas-liquid chromatography of non-saponifiable compounds (tocopherols and sterols).

We analysed the triacylglycerol, tocopherol and sterol composition of hazelnut oil, olive oil and their mixtures (90% olive oil with 10% hazelnut oil, 70% olive with 30% hazelnut oil and 50% olive oil with 50% hazelnut oil). The main triacylglycerols were 1,2,3-trioleylglycerol, 2,3-dioleyl-1-palmitoylglycerol, 2,3-dioleyl-1-linoleylglycerol and 2,3-dioleyl-1-stearoylglycerol. Non-saponfiable compounds (tocopherols and sterols) were derivatised as O-trimethylsilyl ethers. Alpha-tocopherol was the main vitamin E isomer in all samples; however, small amounts of beta-tocopherol and gamma-tocopherol were also found. Beta-sitosterol and delta5-avenasterol were the principal sterols in all samples; campesterol and stigmasterol were minor sterol compounds in all samples. Obtusifoliol, which was a major sterol in olive oil and oil mixtures, was not found in hazelnut oil. The discriminant analysis showed that hazelnut oil, olive oil and oil mixtures were clearly separated according to their triacylglycerol composition.

Atmospheric Pressure↗
PubMed2000

Quantitative determination of alpha-, beta-, gamma- and delta-tocopherols in human serum by high-performance liquid chromatography and gas chromatography-mass spectrometry as trimethylsilyl derivatives with a two-step sample preparation.

Using a two-step sample preparation with Extrelut and silica gel extraction in Pasteur pipettes it is possible to quantify all tocopherols in human serum samples by means of normal-phase HPLC with fluorescence detection (lambda(ex) 295 nm, lambda(em) 330 nm) or by GC-MS of their trimethylsilyl (TMS) derivatives. The method has been used in pharmacoepidemiological studies concerning the exposition with vitamin E-containing drugs in Germany. The recovery for all tocopherols is 98% and the limit of detection is 50 pg for alpha-tocopherol in the HPLC and 40 pg for all TMS-tocopherols in the GC-MS method using the selected ion monitoring mode with a well-tuned GCQ system. Linearity of calibration is excellent for both methods over the full physiological relevant range. Due to the low sample amount needed, the method is suitable for epidemiological and paediatric research.

Chromatography, High Pressure Liquid↗
PubMed2001

Fractionation and characterization of phenolic resins by high-performance liquid chromatography and gel-permeation chromatography combined with ultraviolet, refractive index, mass spectrometry and light-scattering detection.

HPLC and gel permeation chromatographic (GPC) characterization of complex phenol-formaldehyde resins is described. Reversed-phase HPLC fingerprints the phenolic monomers, dimers and some oligomers. The molecular masses of these phenolic compounds were determined using an ion trap mass spectrometer. GPC analyzes tetrahydrofuran-soluble phenolic polymers beyond HPLC capability. The molecular mass distribution and structural information of the phenolics was determined by both conventional and laser light-scattering calibration methods. GPC with both UV and refractive index detection provides weight concentration of phenolic resin and the molar concentration of the phenol unit in the oligomers or polymers.

Chromatography, Gel↗