Two cases of lysergamide intoxication by ingestion of seeds from Hawaiian Baby Woodrose.

We describe two cases of human consumption of seeds from Argyreia nervosa (Hawaiian Baby Woodrose), which resulted in one fatality due to falling from a building and one surviving witness. The principal psychoactive constituent of the seeds, lysergamide (LSA), was recovered from blood and urine samples by mixed-mode cation exchange solid-phase extraction and quantified by ultra performance liquid chromatography-time of flight mass spectrometry (UPLC-ToF/MS). The LSA concentrations were determined by UPLC-ToF/MS to be 4.

Thermospray liquid chromatography-mass spectrometry of corticosteroids.

A high-performance liquid chromatographic method was developed for thermospray mass spectrometric analysis of steroidal hormones. Using a Nova-Pak C18 reversed-phase column and isocratic elution with a solvent comprised of 25 mM ammonium formate in 30% acetonitrile, corticosteroids were separated within 10 min. This solvent also permitted ultraviolet absorbance detection down to 220 nm with low-nanogram sensitivity.

Syntheses and comparison of three reagents for allyldimethylsilylation of prostaglandins and steroids: a gas chromatographic method.

Three reagents used for allyldimethylsilylation of prostaglandins and steroids have been prepared: N,O-bis(allyldimethylsilyl)trifluoroacetamide, N-methylallyl-dimethylsilyltrifluoroacetamide and allyldimethylsilyl-N,N-diphenylamine. The reaction kinetics of the reagents have been studied at room temperature in several solvents, and the optimal conditions for the derivatization of prostaglandins and steroids are discussed.

Analysis of leukotrienes by liquid chromatography/electrochemistry after conversion to dinitrobenzoate derivatives.

A sensitive liquid chromatography method has been developed using electrochemistry for the determination of leukotrienes in biological fluids. Biological specimens are treated with 3,5-dinitrobenzoyl chloride in acetonitrile which undergoes rapid reaction with hydroxyl groups of non-peptidic leukotrienes in the presence of pyridine and with amino groups of peptidic leukotrienes in the presence of potassium tetraborate buffer. The resulting dinitrobenzoate derivatives of leukotrienes are highly electroactive, suitable for reduction or oxidation at moderate potentials by an electrochemical detector.

Reversed-phase ion-interaction chromatography of leukotrienes, lipoxins and related compounds.

A novel mobile phase containing heptafluorobutyric acid has been used for ion-interaction high-performance liquid chromatography of leukotrienes, lipoxins and related compounds on octadecylsilane silica columns. The use of a hydrophobic perfluorinated carboxylic acid as an ion-interaction agent at optimized concentration and pH permitted rapid, isocratic separation of leukotrienes, lipoxins and monohydroxyeicosatetraenoic acids. A completely volatile mobile phase suitable for preparative chromatography was obtained by using triethylamine as the base for pH adjustment.

Mass spectrometric evaluation of the tert.-butyldimethylsilyl derivatives of monohydroxyeicosatetraenoic acids and leukotrienes.

The tert.-butyldimethylsilyl (t-BDMS) derivatives of the hydroxyl and the carboxyl groups on the monohydroxyeicosatetraenoic acids (HETEs) 5-, 12- and 15-hydroxyeicosatetraenoic acid (5-HETE, 12-HETE and 15-HETE, respectively) as well as leukotriene B4 (LTB4), 20-carboxy-LTB4 (20-COOH-LTB4) and 20-hydroxy-LTB4 (20-OH-LTB4) have been prepared. The derivatization reagents N-methyl-N-tert.

A comparative study of methyl ester trimethylsilyl, allyldimethylsilyl and tert-butyldimethylsilyl ethers for electron impact mass spectrometry of leukotrienes.

The gas chromatographic and mass spectrometric properties of leukotriene B4, 20-hydroxy-leukotriene B4 and 20-carboxy-leukotriene-B4 were investigated as their methyl ester trimethylsilyl, methyl ester allyldimethylsilyl and methyl ester tert-butyldimethylsilyl ethers. The gas chromatographic properties of the trimethylsilyl and tert-butyldimethylsilyl ether derivatives were good with respect to peak shape and sensitivity, whereas the allyldimethylsilyl ether derivative gave a lower sensitivity. The sensitivity defined as the quantity that could be passed through the gas chromatographic column.

Gas chromatography-mass spectrometry of monohydroxyeicosatetraenoic acids as their methyl esters trimethylsilyl, allyldimethylsilyl and tert.-butyldimethylsilyl ethers.

The gas chromatographic and mass spectrometric properties of the monohydroxy acids 5-hydroxyeicosatetraenoic acid (5-HETE), 12-hydroxyeicosatetraenoic acid (12-HETE) and 15-hydroxyeicosatetraenoic acid (15-HETE) as their methyl ester trimethylsilyl, methyl ester allyldimethylsilyl and methyl ester tert.-butyldimethylsilyl ethers were investigated. The gas chromatographic properties of the trimethylsilyl and tert.

Mass spectrometry of prostaglandins, leukotrienes and steroids as their allyldimethylsilyl ether derivatives.

Allyldimethylsilyl ethers of prostaglandin E2 and F2 alpha, leukotriene B4 and 5 beta-pregnane-3 alpha, 20 alpha-diol were prepared at room temperature in good yields with the novel reagent N,O-bis(allyldimethylsilyl)-trifluoroacetamide. The gas chromatographic properties of the derivatives of prostaglandins and the steroid were found to be excellent whereas those of leukotriene B4 were found to be less than satisfactory. The mass spectra of the allyldimethylsilyl ether derivatives of the compounds studied show intense ions in their upper mass region derived from the elimination of an allyl radical.

Comparative study of solid phase extraction techniques for isolation of leukotrienes from plasma.

We have compared five commercially available absorbent materials (i.e. C18 Sep-Pak, C18 J.

Immunological and non-immunological release of leukotrienes and histamine from human nasal polyps.

Nasal polyps were obtained from 22 patients undergoing polyp surgery. They were chopped into fragments of approximately 2 mm2, washed free of blood, and passively sensitized with serum from timothy allergen sensitive patients (RAST 30-40%), then, challenged with timothy allergen. Analysis of the incubation medium after a 30 min challenge as assessed by reversed phase high performance liquid chromatography and bioassay revealed the presence of leukotriene (LT) LTB4, LTC4, LTD4 and LTE4 (29 +/- 9, 6.

Metabolism of prostaglandin E analogs in guinea pig and rat liver microsomes.

Tritium-labelled 16,16-dimethyl-PGE2, 9-methylene-PGE2 (9-deoxo-16,16-dimethyl-9-methylene-prostaglandin E2) and tetranor-9-methylene-PGE2 were incubated with guinea pig liver microsomes. All three compounds were converted to omega-oxidized products in yields of a few per cent. In addition, from incubations with 9-methylene-PGE2 and tetranor-9-methylene-PGE2 were also obtained metabolites with the methylene group transformed into a dihydrodiol.

Metabolism of prostaglandin E analogs in the guinea pig liver mitochondrial fraction.

Tritium-labeled 16,16-dimethyl-PGE2 and 9-methylene-PGE2 were incubated with the guinea pig liver mitochondrial fraction. The tetranor and dinor metabolites were obtained, a large portion of the latter contained a saturated carboxyl side chain. Also the beta-hydroxydinor metabolites, analogous to the beta oxidation of fatty acids, were identified.

Metabolism of 9-deoxo-16,16-dimethyl-9-methylene prostaglandin E2 in humans.

Tritium-labeled 9-deoxo-16,16-dimethyl-9-methylene prostaglandin E2 was administered by intravenous injection into humans. The initial half-life in plasma was determined to be about 3 min. About 35% of the injected radioactivity was excreted in the urine and about 55% in the feces.