Search results for "Column chromatography"
showing 10 items of 143 documents
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…
Determination of Homovanillic Acid in Human Plasma Using HPLC with Electrochemical Detection and Automated Solid Phase Extraction
1993
Abstract An isocratic HPLC method with electrochemical detection for the quantification of homovanillic acid (HVA) is described. The method included automated solid phase extraction on C-18-reversed phase material, followed by separation on a 3-μm Nucleosil 100 C18 column (250 mm × 4.6 mm I. D.) with a 100 mM citric acid solution (pH 6.6) containing 4% acetonitrile (v/v) as eluent at a flow rate of 0.6 ml/min. Isovanillinic acid served as internal standard. Extractability of both analytes was ca. 80 %. After extraction of 1 ml of plasma, coefficients of variation of replicate analyses were below 10 % in the naturally occuring concentration range.
Über die mikrobiologische Umwandlung N-haltiger Substrate. 3. Mitt.: Über die Konstitutionsaufklärung von Umwandlungsprodukten des 5-Hydroxyindols du…
1968
In Schuttelkulturen von Cordyceps militaris entstehen aus 5-Hydroxyindol zwei neue Substanzen, die nach Chromatographie an Polyamidsaulen und nachfolgender Isolierung auf Grund ihres chemischen Verhaltens gegenuber Diazomethan sowie ihrer Elementaranalysen, IR-, Massen-und NMR-Spektren als ω-N-Acetyl-5-hydroxy-tryptophan und ω-N-Acetyl-serotonin identifiziert wurden. Two new substances are produced in submerged cultures of Cordyceps militaris fed with 5-hydroxyindole. These substances, separated by column chromatography with polyamide and isolated afterwards, have been identified as ω-N-acetyl-5-hydroxytryptophan and ω-N-acetyl-serotonin by their reaction with diazomethane, by elementary an…
Darstellung und eigenschaften von linearen oligourethanen mit phenylendgruppen und von cyclischen oligourethanen aus diäthylenglykol und hexamethylen…
1971
Es wurden lineare Oligourethane mit Phenylendgruppen und cyclische Oligourethane aus Diathylenglykol und Hexamethylendiisocyanat dargestellt. Der groste bisher isolierte Ring enthalt je sieben Grundbausteine und besitzt 119 Ringglieder bei einem Molekulargewicht von 1920. Eine gute Trennung der Oligomeren wurde durch Adsorptionssaulenchromatographie erzielt. Hierbei wurde ein Elutionsmittel mit Losungsmittelgradient verwendet. Schmelzpunkte, Umwandlungserscheinungen, Langperioden und Weitwinkeldiagramme der Oligomeren werden im Hinblick auf ihre Struktur diskutiert. Linear oligourethanes with phenylurethane endgroups and cyclic oligourethanes were prepared from diethylene glycol and hexamet…
Antibakterielle Wirkstoffe, 6. Mitt.1) 2,4-Unsymmetrisch dialkylierte Pyrimido[1,2-a]benzimidazole
1982
Durch Kondensation von 2-Aminobenzimidazol (1) mit 2,4-Hexandion (2a) entsteht das Isomerenpaar 3a/3b, mit 6-Methyl-2,4-heptandion (2b) das Isomerengemisch 3c/3d, wahrend mit 1-Phenyl-2,4-pentandion (2c) die Isomere 3e und 3f gebildet werden. Die Trennung der Isomere ist durch Saulenchromatographie, die Strukturfestlegung auf spektroskopischem Wege, moglich. 2-Imino-2H-s-triazino[2,1-b]benzoxazol weist antibakterielle Wirksamkeit auf. Antibacterial Drugs, VI: 2,4-Unsymmetrically Dialkylated Pyrimido[1,2-α]benzimidazoles Condensation of 2-aminobenzimidazole (1) with 2,4-hexanedione (2a) leads to the pair of isomers 3a/3b. Condensation with 6-methyl-2,4-heptanedione (2b) yields the isomers 3c…
HPLC Method for Cyst(e)ine and Methionine in Infant Formulas
1996
Cyst(e)ine and methionine were converted into cysteic acid and methionine sulfone by oxidizing with performic acid. The oxidized samples were then subjected to acid hydrolysis (6N HCl, 105-110°C/24 hr). After derivatization with phenylisothiocyanate, reverse phase HPLC separation was carried out at 48°C and with UV detection. Different gradients and pH values in the eluent were assayed to determine the best resolution. Analytical parameters, detection and quantification limits, linearity, precision and accuracy, were determined. The method was reliable and accurate for measuring cyst(e)ine and methionine in infant formulae.
Crystal structure of (R)-6-fluoro-2-[(S)-oxiran-2-yl]chroman
2015
The title compound, C11H11FO2, is a building block in the synthesis of the active pharmaceutical ingredient DL-nebivolol. The synthesis starting from the enantiomerically pure (R)-6-fluoro-4-oxo-3,4-dihydro-2H-chromene-2-carboxylic acid resulted in a mixture of two stereoisomers, namely (R)-6-fluoro-2-[(S)-oxiran-2-yl]chroman and (R)-6-fluoro-2-[(R)-oxiran-2-yl]chroman. The mixture was separated by column chromatography but only one stereoisomer crystallized. The X-ray structure analysis revealed that the solid consisted of theR,Sisomer. A similar procedure was repeated for (S)-6-fluoro-4-oxo-3,4-dihydro-2H-chromene-2-carboxylic acid and, in this case, theS,Risomer was produced as a crystal…
Structure and properties ofn-alkyldimethylsilyl bonded silica reversed-phase packings
1978
Summary The effects of the modifier functionality and the chain length ofn-alkylchlorosilanes on the surface structure of packings and on their retention behaviour in reversed-phase chromatography were investigated. Comparative retention studies on three silica packings that had been treated to maximum conversion withn-octyltrichlorosilane (I),n-octylmethyldichlorosilane (II) andn-octyldimethylmonochlorosilane (III) showed that the most pronounced reversed-phase character is obtained by using III as the modifying reagent. A series ofn-alkyldimethylsilyl bonded silica packings were prepared with widely differingn-alkyl chain lengths. Although the packings are very hydrophobic, the maximum su…
N-Cinnamoyltetraketide Derivatives from the Leaves of Toussaintia orientalis
2015
Seven N-cinnamoyltetraketides (1−7), including the new Ztoussaintine E (2), toussaintine F (6), and toussaintine G (7), were isolated from the methanol extract of the leaves of Toussaintia orientalis using column chromatography and HPLC. The configurations of E-toussaintine E (1) and toussaintines A (3) and D (5) are revised based on single-crystal X-ray diffraction data from racemic crystals. Both the crude methanol extract and the isolated constituents exhibit antimycobacterial activities (MIC 83.3−107.7 μM) against the H37Rv strain of Mycobacterium tuberculosis. Compounds 1, 3, 4, and 5 are cytotoxic (ED50 15.3−105.7 μM) against the MDA-MB-231 triple negative aggressive breast cancer cel…