Search results for "performance liquid chromatography"

Determination of triamterene in urine by HPLC using fluorescence detection and column-switching

1994

A liquid chromatographic method incorporating column-switching and fluorimetric detection for the determination of triamterene in untreated urine, is described. The urine samples (5 μL) were directly introduced onto an Hypersil ODS-C18, 30 μm (20 mm×2.1 mm I.D.) pre-column. Polar urinary compounds were removed by flushing the pre-column with water for 1 min, and the analyte was then switched onto an HP-LiChrospher RP C18,5 μm (125 mm×4mm ID) analytical column using an acetonitrile/phosphate buffer gradient elution. Fluorescence detection was performed at 230 nm excitation and 430 nm emission wavelengths. The recovery of drug was 102±2% in the 0.10–20.0 μg/mL concentration range, the limit o…

The quantitative determination of metabolites of 6-mercaptopurine in biological materials. VII. Chemical synthesis by phosphorylation of 6-thioguanos…

1990

Abstract A fast and reliable two-step method has been established for the chemical synthesis of 6-thioguanosine 5′-monophosphate, 6-thioguanosine 5′-diphosphate and 6-thioguanosine 5′-triphosphate starting from the ribonucleoside. In the first step, 6-thioguanosine dissolved in triethyl phosphate, at high yield reacts with phosphorus oxide trichloride to 6-thioguanosine 5′-monophosphate which is purified by anion-exchange chromatography on DEAE-Sephadex using a step gradient of hydrochloric acid. In the second step, 6-thioguanosine 5′-monophosphate dissolved in water, reacts with phosphoric acid in the presence of pyridine/dicyclohexyl carbodiimide and is converted to 6-thioguanosine 5′-dip…

Chromatographic and mass spectrometric characteristics of 20-dihydroaldosterone.

1992

The 20 alpha-reduced derivative of aldosterone, 20 alpha-dihydroaldosterone, was needed as reference compound in order to continue the studies on 18-hydroxylation in the Y-1 adrenal cell line. It was obtained by reduction of aldosterone with sodium borohydride. Analysis of the products of the reaction as methoxime trimethylsilyl (MO-TMS) derivatives by gas chromatography (GC) and GC-mass spectrometry (GC-MS) showed three possible forms of the compound. Their identification was confirmed by comparison with the products obtained by stereospecific reduction of aldosterone using 3 alpha,20 beta-hydroxysteroid dehydrogenase. Chromatographic behavior and mass spectra are given for the three forms…

An inter-laboratory validation of methods of lipid peroxidation measurement in UVA-treated human plasma samples

2010

Lipid peroxidation products like malondialdehyde, 4-hydroxynonenal and F2-isoprostanes are widely used as markers of oxidative stress in vitro and in vivo. This study reports the results of a multi-laboratory validation study by COST Action B35 to assess inter-laboratory and intra-laboratory variation in the measurement of lipid peroxidation. Human plasma samples were exposed to UVA irradiation at different doses (0, 15 J, 20 J), encoded and shipped to 15 laboratories, where analyses of malondialdehyde, 4-hydroxynonenal and isoprostanes were conducted. The results demonstrate a low within-day-variation and a good correlation of results observed on two different days. However, high coefficie…

Determination of ascorbic acid in plasma and urine by high performance liquid chromatography with ultraviolet detection.

1999

Abstract A reliable simple reversed-phase liquid chromatographic method for the routine determination of ascorbic acid in plasma and urine with ultraviolet detection is described. This method enables the complete separation of the ascorbic acid peak from others with a recovery of above 95 % within 8 minutes. The method can be used for analysing multiple samples within a day. In addition, the storage conditions and stability of ascorbic acid in plasma and urine were investigated. Samples of plasma and urine can be stored on ice in darkness for at least 60 min without reduction of ascorbic acid concentration. Prepared samples can be stored in darkness at 4 °C for at least 120 min and in liqui…

A simple high-performance liquid chromatography (HPLC) method for the measurement of pyridoxal-5-phosphate and 4-pyridoxic acid in human plasma.

2014

Abstract Background Low concentration of plasma pyridoxal-5-phosphate (PLP) is associated with hyperhomocysteinemia and inflammation. Most methods for the measurement of plasma PLP require large specimen volume and involve the use of toxic reagents. Methods We have developed a HPLC method for the measurement of PLP and 4-pyridoxic acid (4-PA) in plasma, which requires small specimen volume. The samples are prepared without adding any toxic reagents. Furthermore, we have examined whether intake of vitamin B 6 affects the concentration of plasma PLP and 4-PA. Results The coefficient of variation of the method was 6% and the recovery of the added vitamin in plasma was about 100%. The concentra…

Retention pharmacokinetic and pharmacodynamic parameter relationships of antihistamine drugs using biopartitioning micellar chromatography

2001

Abstract Antihistamines are drugs which act by competitive inhibition of the H1 or H2 histamine receptors. Little has been known about their clinical pharmacokinetics and biological responses until the last few years. In this paper, we propose quantitative retention–activity relationship, QRAR, models based on the retention data of antihistamines in a biopartitioning micellar chromatography (BMC) system using a Brij35 mobile phase for describing pharmacokinetic parameters such as half-life and volume of distribution, or the pharmacodynamic parameters, therapeutic plasma levels, lethal doses and drug-receptor dissociation constant. The predictive ability of these models is statistically vali…

Determination of 5-nitrofurylacrylic acid in wines by high-performance liquid chromatography

1988

HPLC determination of volatile phenols in wines

1993

An alternative to the traditional solvent extraction method used to extract and rapidly quantify ethyl-and vinylphenol and ethyl-and vinylgaiacol from wine is presented. The method is based on retention of volatile phenols on adsorbants. Among the tested resins, the most efficient, AG 2-X8 (anion exchange resin), worked as well with a synthetic solution as with wines. The percolation of clarified wine adjusted to pH 9 on this resin permits, in particular, the elimination of organic acids. Phenols are not eluted after rinsing the column with 1N HCl, but are eluted with methanol after this treatment. Good recovery (91 %) and good repeatability are observed. The eluate is directly analysed by …

Quantitative determination of sotolon in wines by high-performance liquid chromatography

1993

Sotolon (4,5-dimethyl-3-hydroxy-2(5H)-furanone) is a key flavour compound in the french flor-sherry “Vin jaune”. This compound was determined quantitatively by extraction of 25 ml of wine on a XAD-4 resin, elution with diethyl ether, separation by HPLC on a Lichrospher 100 Diol column, elution with dichloromethane/hexane (60/40) and UV detection at 232 nm. The amount of sotolon in “Vin jaune” (120 to 268 μg/l) was related to the development of the yeast film over a period of 6 years. Only 6 to 51 μg/l were found in the “Vin de paille” which is made with overmaturated grapes of the same Savagnin vine-plant but without development of yeasts, and 80 to 140 μg/l in “Tokai” which are partly grow…