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.