Search results for "COLUMN"
showing 10 items of 1301 documents
Capillary column gas chromatographic identification of sugars in honey as trimethylsilyl derivatives.
1987
A method for identifying carbohydrates (mono-, di- and trisaccharides) in honey is presented. It is based on the separate preparation of both trimethylsilyl ethers and oxime trimethylsilyl ethers of the sugars followed by their gas chromatographic separation on a fused-silica capillary column coated with OV-101 using temperature programming. From the two chromatograms, the number of peaks given by each derivatized sugar, their relative retention times and peak-area ratios are used for identification. The identities of two unidentified trisaccharide peaks are considered. Quantitative applications to honey sugar analysis are discussed.
Structures, properties and miscibility behaviour of liquid crystalline polycatenar tetrone derivatives
1995
Abstract The tetrones represent an interesting new mesogenic building block. The results of this study show that they can be incorporated into a variety of mesophases. A smectic phase was observed in the polycatenar compound with four terminal chains as expected. The phase exhibits a tilted structure (Sc phase) to prevent void formation. The compound with six pendant chains forms a columnar phase. In spite of their structural similarity, the tetrones studied tended not to be completely miscible. However, complete miscibility with a semi-discoid phenylhydrazone was observed. When this hydrazone, which forms a columnar ‘Dho phase’, was mixed with tetrone which forms a columnar ‘Dhd phase’ a c…
Simultaneous Automated Determination of Catecholamines, Serotonin, and Their Metabolites in Brain Tissue by HPLC and Electrochemical Detection
1993
Abstract A robust procedure with minimal tissue sample pretreatment, based on reversed-phase, ion-pair high performance liquid chromatography (HPLC) combined with electrochemical detection has been developed for the automated and simultaneous determination of the biogenic amines norepinephrine (NE), epinephrine (E), dopamine (DA), 5-hydroxytryptamine (5-HT) and their metabolites 3-methoxy-4-hydroxyphenylethyleneglycol (MHPG), 3,4-dihydroxyacetic acid (DOPAC), homovanillic acid (HVA) and 5-hydroxyindolacetic acid (H I A A) in as little as 0.5 mg brain tissue. The chromatographic conditions remain stable for at least 8 weeks. In particular small amounts of samples which do not allow reexamina…
Sensitive and selective determination of metabolically formed trans -dihydrodiols and phenols of benzo[ a ]pyrene in water and urine samples by HPLC …
1998
A method has been developed to separate hydroxylated metabolites of the carcinogenic polycyclic aromatic hydrocarbon benzo[a]pyrene, i. e. trans-4,5-, 7,8-, 9,10-dihydrodiol and 1-, 3-, 7-, and 9-phenol, by HPLC with amperometric detection employing an isocratic methanol/water eluent (70:30, v/v) containing 0.5 g/L sulfuric acid and 1 g/L lithium perchlorate. Compared with the usually applied fluorescence (λex = 265 nm, λem = 460 nm) and ultraviolet (λ = 265 nm) detection, the amperometric technique is about 2–12 times more sensitive for the determination of all metabolites investigated. The method was applied to the determination of the seven metabolites of benzo[a]pyrene in different wate…
Die zweifache unterdrückung der polymerisation einiger bis(methacrylsäureester) mittels radikalischer additionsreaktionen
1973
Aus Hydrochinon, Resorcin, Dihydroxydiphenylen und Dihydroxynaphthalinen wurden mit Methacrylsaurechlorid Bis(methacrylsaureester) hergestellt. Setzte man diese in siedendem Benzol mit groser Verdunnung gelosten Ester dem Angriff von Radikalen aus α.α′-Azoisobuttersauredinitril (Primarradikale) aus, dessen Uberschus in Beziehung zum Ester mindestens zwanzigfach molar war, so erhielt man mittels saulenchromatographischer Trennung Verbindungen, bei denen je olefinische Doppelbindung zwei Primarradikale addiert waren (unterdruckte Polymerisation). Die Struktur dieser Produkte wurde mittels Elementaranalyse, Molekulargewichtsbestimmung, IR- und 1H-NMR-Spektren bewiesen. Demnach kann die Polymer…
Water residence time and the dynamics of toxic cyanobacteria
2012
SUMMARY 1. Climate change affects aquatic ecosystems differently depending on local conditions. In the Mediterranean region, predicted drier seasons could especially affect lake water residence time and in consequence cyanobacteria and cyanotoxin dynamics. 2. We carried out a 3-year study of a shallow, Mediterranean lake (Lake Albufera, Spain), to study the effects of water residence time and other drivers on the dynamics of harmful cyanobacteria and microcystin concentrations (MCYST). 3. Longer water residence time in dry years and dry seasons increased total cyanobacteria biomass, Microcystis aeruginosa populations and MCYST concentrations in the lake water and seston. Droughts increased …
Reliable and simple analytical methods for determination of citrulline and metabolically related amino acids by liquid chromatography after derivatiz…
2014
We describe the development of a high-performance liquid chromatography (HPLC) method for the determination of citrulline and other amino acids relevant to intestinal diseases. The amino acids were derivatized with 9-fluorenylmethylchloroformate (FMOC-Cl) and their derivatives were separated on two different columns, a core-shell column (Halo C18) and a silica-based monolith (Chromolith Performance RP-18). The derivatization reaction was optimized with respect to pH, buffer concentration and reproducibility. The optimal derivatization conditions were achieved with 0.4 M borate buffer at pH 9.20, a constant ratio of FMOC-Cl/total amino acids (10 : 1) and 75 mM tyramine after 1 min (quenching…
Fast Response Heating Module for Temperature Programmed GC Analysis in Microreaction Systems
2000
For monitoring the reactant and product concentrations of a gas phase microreactor for ethylene oxide synthesis the development of a miniaturised device for fast GC analysis suitable for operation in conjunction with the microreactor is advantageous. Therefore, a method employing short (0.2 – 0.4 m) packed capillary columns was developed. Highly crosslinked polystyrene microspheres proved to be the most suitable adsorbent enabling a high separation efficiency. For fast temperature programming design concepts for an efficient heating module capable to be used with short capillary columns were developed. In principle, planar as well as cylindrical designs are suitable for integration of a res…
Gas chromatographic study of acetyl derivates of chlorinated guaiacols
1982
The gas chromatography of acetyl derivatives of guaiacol and all chlorinated guaiacols has been studied on SE-30, OV-351 and Carbowax 20M capillary columns. The retention order and relative retention times under isotermal and temperature-programmed conditions are discussed. Different retention times for all mono- and dichloro compounds have been observed on the SE-30 column. However, all trichloroguaiacol isomers were separated only on polar columns. The best overall temperature-programmed separations have been achieved on an SE-30 capillary column.
New Glass Capillary Gas-Chromatographic Methods for Metabolites in Urine and Serum
1981
The analytical system suggested in this paper is a further development of pre-chromatographic methods and of column switching techniques described in previous papers1,2,3.In order to use modern gas-chromatographic techniques for the determination of metabolites in urine and serum quick and reliable pre-chromatographic methods for extraction, concentration and derivatization must be developed which give final (dosage) volumes of 5 to 10 μl with starting sample volumes of 0.1 ml of urine or 5 ml of serum as described by Dunges4.