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Biomedical subjects

P Sandra

Publications and source records attributed to P Sandra.

64 records · Page 4Linked to original sources

Structures and concentrations of fifteen different steroid sulfates in human breast cyst fluids.

By applying capillary gas chromatography (GC) and gas chromatography mass spectrometry (GC-MS), a simultaneous quantitation of all important steroid sulfates present in a number of breast cyst fluids, has been obtained. The fact that prevailing androgen sulfate structures in the cyst fluids are different from those in blood suggests at least intracystic metabolism of blood-born precursors. Particularly greater amounts of 5 alpha-reduced steroids are found in breast cysts. 5 alpha-Androstane-3 alpha,17 beta-diol is a major androgen sulfate of breast cyst fluids, its concentration being some 2000-fold that of blood. After prolonged topical application of progesterone on the breast, an accumulation of the sulfates of several pregnanediol isomers could be observed.

Adult↗

Analysis of mycolic acids from a group of corynebacteria by capillary gas chromatography and mass spectrometry.

The cell wall of leprosy-derived corynebacteria (a group of 'diphtheroids' isolated from human leprosy lesions and patients' blood) was previously shown to contain, in addition to peptidoglycan and arabinogalactan, mycolic acids. These alpha-branched beta-hydroxy fatty acids were attributed to the corynomycolic group, according to their RF in monodimensional thin-layer chromatography. In the present work, mycolic acids from leprosy-derived and reference corynebacteria have been fractionated by monodimensional and bidimensional thin-layer chromatography and by gas chromatography. Pyrolyzed mycolic acids have been analyzed on conventional packed columns, whereas intact methyl esters of mycolic acids with free and silylated beta-hydroxyl group have been analyzed on capillary columns, and their structure has been established by mass spectrometry. In all leprosy-derived corynebacteria, some 20 components containing 24-36 carbon atoms and 0-4 double bonds were obtained. The three major groups had 32, 34 and 36 carbons, and the frequency of unsaturated versus saturated chains increased proportionally to the molecular weight. For comparison, the main components of a reference corynebacterium. Corynebacterium diphtheriae PW8, had 30 and 32 carbons, and their hydrocarbon chains were essentially saturated. This work confirms the relative chemical homogeneity of different leprosy-derived corynebacteria and describes some peculiar traits in the chemical structure of this group of organisms. In addition, it shows the complexity of the mycolic acid fraction of corynebacterial cell wall and suggests that the mycolic acid pattern is a sort of fingerprint of each bacterial strain grown under standard conditions. Finally, the fractionation of intact corynomycolic acid methyl esters with free or silylated beta-hydroxyl group by capillary gas chromatography proved to be the best analytical procedure at present available for resolving this complex mixture of corynomycolate isomers. Structural determination of silylated samples by mass spectrometry is preferred because they have more diagnostic fragments.

Cell Wall↗

Fatty acid chain length combinations in ascitic fluid triglycerides containing lymphatic absorbed medium-chain fatty acids.

Information on the fatty acid chain length combinations in lymph triglycerides containing medium-chain fatty acids was obtained by combining the fatty acid composition and the carbon number composition of triglycerides from ascitic fluid of patients on medium-chain triglyceride-containing diets. In these triglycerides, the major part of the medium-chain fatty acids was present in combination with long-chain fatty acids. These results indicate that part of the lymphatic absorbed medium-chain fatty acids are absorbed as triglycerides which also contain long-chain fatty acids.

Ascites↗

Measurement of 5-fluoro-2'-deoxyuridine serum levels by gas chromatography chemical ionization mass spectrometry.

Serum levels of 5-fluoro-2'-deoxyuridine in cancer treated patients were measured by gas chromatography mass spectrometry under chemical ionization conditions; 1-(2-deoxy-beta-D-lyxofuranosyl)-5-fluorouracil (3'-epi-5-fluoro-2'-deoxyuridine) was used as an internal standard. The drug and internal standard were quantitatively isolated from the serum sample by a mini-column anion exchange method and the extract permethylated using potassium-tert-butoxide in dimethylsulphoxide and methyl iodide. The derivatized nucleosides were then re-extracted from the reaction mixture and analysed on a glass capillary column coated with Superox-4. The column was coupled directly to the chemical ionization source of the mass spectrometer; NH3 was used as the reagent gas. The gas chromatographic effluent was monitored at m/z 289, the [MH]+ ion of the N,O-permethyl derivatives of 5-fluoro-2'-deoxyuridine and the internal standard. Recovery of 5-fluoro-2'-deoxyuridine from serum in the 0-1 microgram ml-1 concentration range averaged 93 +/- 2% (SD); a linear detector response was observed up to 50 ng 5-fluoro-2'-deoxyuridine ml-1. At the 10 ng ml-1 level, a within-run assay precision of 10% (CV) (n = 5) was found, while a detection limit of about 1 ng 5-fluoro-2'-deoxyuridine ml-1 of serum was attained. The method was applied to the measurement of disappearance curves of 5-fluoro-2'-deoxyuridine in the serum of treated patients.

Floxuridine↗

Critical aspects for the reliable headspace analysis of plants cultivated in vitro.

Various factors controlling the recoveries of volatile organic compounds in vitro headspace analysis of tomato plants (Lycopersicon esculentum Mill. 'Moneymaker'), sampled using solid phase micro-extraction, were evaluated and optimised. The variations in composition of the headspaces were determined as a function of time, and following in vitro wounding of the plant.

Chromatography, Gas↗

On-flow gas chromatographic method for the determination of the enantiomer interconversion energy barrier.

A novel on-flow gas chromatographic (GC) method is developed for the determination of the kinetic rate constants and interconversion energy barrier of thermally labile enantiomers. The validity of the developed method is approved by the study of interconversion of 1-chloro-2,2-dimethylaziridine enantiomers on an achiral column. The overall experiments are performed in a series of three columns placed in two independently heated GC ovens. The racemate of the 1-chloro-2,2-dimethylaziridine is injected and separated in the first chiral column at 60 degrees C in which the interconversion of enantiomers is suppressed. Separated enantiomers are then transferred into the achiral column, where the enantiomers are interconverted at a selected temperature under the current carrier gas flow. Effluent from this column is transferred into the second chiral column, where the native enantiomers and those originated by the on-flow interconversion on an achiral column are again separated at 60 degrees C. Chromatograms obtained by monitoring the effluents from the second chiral column are used to determine the peak areas of the original and the newly interconverted enantiomers. The corresponding peak areas and the interconversion times are used to calculate the interconversion rate constants and energy barriers of the 1-chloro-2,2-dimethylaziridine enantiomers. The apparent energy barriers of the enantiomers of 1-chloro-2,2-dimethylaziridine are equal for both enantiomers within a 95% confidence interval and independent of the polarity of the stationary phase of the column in which the interconversion of enantiomers occur.

Journal Article↗

Quantitative determination of selected tricyclic biological active compounds by using capillary electrophoresis.

Five tricyclic antidepressants: imipramine hydrochloride, noxiptilin hydrochloride, hydroxyzine dihydrochloride, diethiazine hydrochloride and amitryptyline hydrochloride were determined by the capillary electrophoresis method. The determinations were performed by using a fused sillica capillary (60 cm x 50 microns i.d., effective length 53 cm). Acetate buffer (25 mM ammonium acetate and 1 mM acetic acid) in (1:1) methanol:water solution was used as an electrolyte. The determination voltage was 20 kV. The UV-detector at 214 nm was applied.

Antidepressive Agents, Tricyclic↗

Identification and quantitation of 5-fluorouridine in rat urine after administration of 5-fluorouracil or 5-fluoro-2'-deoxyuridine.

The ribonucleoside 5-fluorouridine was identified in 24-hr urine samples from rats after ip administration of 5-fluorouracil (200 mg/kg) or 5-fluoro-2'-deoxyuridine (380 mg/kg) by means of thin-layer chromatography, high-pressure liquid chromatography, capillary gas-liquid chromatography and gas-liquid chromatography-mass spectrometry techniques, and by comparison with the synthetic compound. By use of a specific extraction procedure, 5-fluorouridine was then quantitatively determined by capillary gas-liquid chromatography with a nitrogen-selective detector. These measurements indicate that not more than 0.2% of the administered dose was excreted as 5-fluorouridine; lower urinary metabolite levels were found after treatment with 5-fluorouracil than after 5-fluoro-2'-deoxyuridine administration. Following an ip dose of either drug, variable amounts of 2'-deoxyuridine and thymidine were detected in the urine samples.

Animals↗