Simple method for the chromatographic separation and determination of mono-, di- and tricyclic aromatic hydrocarbons in heavier petroleum fractions

Summary The method described is a simple procedure for separating gas oil boiling range petroleum fraction into its aromatic hydrocarbons of the mono-, di- and trinucleartype. This is accomplished by gradient elution through an alumina adsorption column under established/standardised conditions. Characterisation is performed by UV-absorption. The method can be used also for investigating aromatic hydrocarbon structures from other petroleum fractions.

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Einfaches Verfahren zur chromatographischen Trennung und Bestimmung von mono-, di- und tricyclischen aromatischen Kohlenwasserstoffen in schwereren Erdölfraktionen

Zusammenfassung Zur Trennung der Erdölfraktion vom Siedebereich des Gasöls in die ein-, zwei- und dreikernigen aromatischen Bestandteile wird eine Gradientenelution an einer Aluminiumoxidsäule unter standardisierten Bedingungen angewendet. Zur Charakterisierung dienen UV-spektrometrische Messungen. Das Verfahren kann auch zur Untersuchung von Aromaten aus anderen Erdölfraktionen eingesetzt werden.

     

Studies on digitalis. IV. A method for thin-layer chromatographic separation and determination of digitoxin and cardioactive metabolites in human blood and urine.

A thin-layer chromatographic method for the separation of digitoxin and its cardioactive metabolites in one system is described. Pre-coated silica gel plates impregnated with 15% formamide solution in acetone were developed twice in the same direction (running distance 18cm) with ethyl methyl ketone-xylene (50:50) as solvent. The system showed no border-zone effects, and the reproducibility was good. Samples (5 ml) of serum or urine were extracted with dichloromethane, the extracts were evaporated, the residues were dissolved in 70% ethanol, the ethanol solutions were washed twice with light petroleum and then evaporated, and the residues were dissolved in chloroform-methanol for application to the thin-layer plates. After development, the metabolites were scraped from the plates and analyzed by means of a modified rubidium-86 method. The recovery for the whole procedure was 59%, and the sensitivity of the method permitted the determination of down to 0.5 ng per spot. The method will facilitate the study of digitoxin metabolism in patients undergoing treatment with the drug.     

Reversed-phase liquid chromatographic separation and simultaneous fluorimetric detection of polyamines and their monoacetyl derivatives in human and animal urine, serum and tissue samples: an improved, rapid and sensitive method for routine application

A highly sensitive and precise method for the determination of the polyamines putrescine, cadaverine, spermidine and spermine and all their monoacetyl derivatives in a single analysis in human and animal urine, serum and tissue samples is described. For polyamine separation, an ion-pairing reversed-phase high-performance liquid chromatographic (HPLC) method is used, followed by post-column derivatization with o-phthalaldehyde and consecutive fluorescence detection. Urine and serum samples are purified with a Bond Elut silica cartridge. The detection limit for polyamines is 0.5-1.0 pmol and excellent linearity is achieved in the range from 3 pmol up to more than 10 nmol. The influence of some modifications of different analytical steps such as the temperature of the HPLC column and the derivatization reaction coil and the o-phthalaldehyde flow-rate is described. Quality control data and measurements of the reproducibility of the method are presented. In order to establish a rapid analytical method for easy routine use, all steps for preparation and quantitative analysis are minimized. This method was applied to the determination of total polyamines in human urine and serum hydrolysate and of free and acetylated polyamines in human urine and pancreatic tissue of the rat. Values for normal polyamine concentrations in the urine and serum of fifteen male and fifteen female healthy volunteers and in the pancreas of ten normal rats are presented.     

A rapid gas chromatographic method for the determination of chlorophenoxyisobutyric acid in plasma and urine.

A rapid gas chromatographic method is described for the determination of chlorophenoxyisobutyric acid (the active metabolite of clofibrate) in plasma and urine. The assay involves an extraction into toluene and back-extraction of the chlorophenoxyisobutyric acid and the internal standard (2-naphthoic acid) into the methylating reagent (trimethylanilinium hydroxide). Concentrations of 1 mug/ml in plasma and urine can easily be measured; the precision of the method is 3.3 +/- 0.7% for plasma and 2.7 +/- 0.4% for urine. There is no interference from endogenous compounds or from drugs commonly prescribed together with clofibrate.     

A gas-liquid chromatographic method for the analysis of diphenoxylic acid in urine

Summary A gas-liquid chromatographic method has been developed and evaluated for the measurement of diphenoxylic acid in urine. This method uses base hydrolysis to liberate diphenoxylic acid from compounds conjugated in urine, followed by removal of interfering substances in urine by column chromatography on alumina. Quantitation was carried out using p-chlorodiphenoxylic acid as an internal standard.     

Aliphatic monoamines,diamines, polyamines: An HPLC method for their identification and separation by a dansylation reaction; The study of separation factors in homologous series

Summary An analytical method is presented for the identification and separation of aliphatic monoamines, diamines and polyamines. Dansyl chloride as the derivatizing agent and fluorimetric detection were employed. The behaviour of different column packings and eluent compositions was tested and compared. The interaction mechanisms of the dansylated compounds with stationary and mobile phases are discussed on the basis of the analysis of the capacity factors evaluated in the homologous series of monoamines CH₃(CH₂)_nNH₂, with n varying up to 9 and diamines NH₂(CH₂)_nNH₂, with n varying up to 12. An application of this method to a real sample is presented.     

Gas chromatographic assay for N,N-dimethylglycine in urine.

A gas chromatographic method for the determination of N,N-dimethylglycine in urine has been developed. After clean-up by cation-exchange, N,N-dimethylglycine was derivatized with ethanol and hydrochloric acid to form the corresponding ethyl ester. After evaporation of solvent, N,N-dimethylglycine ethyl ester was extracted into methylene chloride and chromatographed on a gas chromatograph equipped with a packed column containing 10% Carbowax 20 M. The detection limit of the method is 0.01 mM N,N-dimethylglycine in urine. This method has been used to detect N,N-dimethylglycine in urine from healthy subjects as well as in urine from patients with metabolic disorders. These findings were verified by gas chromatography-mass spectrometry.     

Gas-liquid chromatographic method for the measurement of methyl urea in blood and urine.

A technique for the measurement of methyl urea in biological fluids is described based upon gas-liquid chromatography of its trifluoroacetyl derivative. The method requires 10 ml of either blood or urine and is capable of measuring methyl urea at concentrations of less than 5 mg/l.     

Chromatographic separation and identification of human urine components

Summary Ultraviolet-absorbing components of human urine were separated by HPLC with a large scale column (250 × 28 mm I.D. stainless-steel) containing a macroreticular type strongly basic anion-exchange resin. The sample was eluted with a linear gradient of 0.006 M to 6.0 M ammonium acetate buffer (pH 4.40) and different fractions were collected. The identification of one compound using ultraviolet, infrared and mass spectral data is illustrated; it was found to be uric acid.     

High-performance liquid chromatographic method for the analysis of Oltipraz in human serum and urine.

A rapid, sensitive procedure for the analysis of Oltipraz in serum and urine using high-performance liquid chromatography was developed. The proposed method illustrates recovery of Oltipraz from biological fluids was greater than 80%. Detection and separation of Oltipraz required as little as 1 ml of serum or urine. Oltipraz was detectable when 2 ng or more of drug was present in 1 ml of serum or urine; the method is highly reproducible when 5 ng/ml or more Oltipraz is present in the biological fluid.