RESUMEN
A simple controlled chemical reduction of 1,3,5-trinitro-1,3,5-triazacyclohexane (RDX) and related nitramine compounds with zinc amalgam generates species that elicit intense chemiluminescence with tris(2,2'-bipyridine)ruthenium(III), which extends this widely utilised chemiluminescence reagent to a new class of analyte and presents a sound chemical basis for a screening test for nitramine high explosives. Examination of the chemiluminescence profiles under stopped-flow conditions revealed contributions from multiple transient species formed in the initial reduction step.
Asunto(s)
2,2'-Dipiridil/análogos & derivados , Compuestos de Anilina/análisis , Sustancias Explosivas/análisis , Nitrobencenos/análisis , Compuestos Organometálicos/química , Triazinas/análisis , 2,2'-Dipiridil/química , Análisis de Inyección de Flujo , Mediciones Luminiscentes , Cloruro de Mercurio/química , Zinc/químicaRESUMEN
We have combined the generation of solvent gradients using milliGAT pumps, chromatographic separations with monolithic columns and chemiluminescence detection in an instrument manifold that approaches the automation and separation efficiency of HPLC, whilst maintaining the positive attributes of flow injection analysis (FIA), such as manifold versatility, speed of analysis and portability. As preliminary demonstrations of this hybrid FIA/HPLC system, we have determined six opiate alkaloids (morphine, pseudomorphine, codeine, oripavine, ethylmorphine and thebaine) and four biogenic amines (vanilmandelic acid, serotonin, 5-hydroxyindole-3-acetic acid and homovanillic acid) in human urine, using tris(2,2'-bipyridyl)ruthenium(III) and acidic potassium permanganate chemiluminescence detection.
Asunto(s)
Cromatografía Líquida de Alta Presión/instrumentación , Cromatografía Líquida de Alta Presión/métodos , Análisis de Inyección de Flujo/instrumentación , Análisis de Inyección de Flujo/métodos , Alcaloides/análisis , Alcaloides/química , Aminas/química , Aminas/metabolismo , Humanos , Estructura Molecular , Neurotransmisores/metabolismoRESUMEN
The use of tris(2,2'-bipyridyl) ruthenium (III) as a chemiluminescent spray reagent spot-test for heroin is discussed. Two forms of the reagent are investigated an aqueous and an anhydrous where both were found to give vastly different results. The aqueous reagent giving slow, low intensity chemiluminescence whilst the anhydrous reagent gave a fast, bright response in the presence of 3,6-diacetylmorphine. The anhydrous reagent is less sensitive the slow, intensity response is characteristic of only two opiates tested 3,6-diacetylmorphine and 3-monoacetylmorphine.
RESUMEN
Time-resolved fluorescence microscopy has rapidly emerged as the technique of choice for many researchers aiming to gain specific insights into the dynamics of intricate biological systems. Although the unique advantages the technique provides over other methods have proven to be particularly useful in the biosciences, to date they have been largely unexploited by other research disciplines. In this paper, we demonstrate the capacity of time-resolved fluorescence microscopy as a practical analytical tool in the forensic sciences via the imaging of gunshot residues that are expelled when a firearm is discharged. This information may prove to be useful for determination of the true sequence of events that took place in a firearm related crime.
RESUMEN
A rapid method for screening drug seizure samples for 3,6-diacetylmorphine (heroin), which consists of a simple hydrolysis procedure and flow-injection analysis with two chemiluminescence reagents, is described. Before hydrolysis, 3,6-diacetylmorphine evokes an intense response with a tris(2,2'-bipyridyl)ruthenium(III) reagent (prepared by dissolving the perchlorate salt in acetonitrile), and a relatively weak chemiluminescence response with a second reagent: potassium permanganate in an aqueous acidic polyphosphate solution. However, the permanganate reagent is extremely sensitive toward the hydrolysis products of 3,6-diacetylmorphine (i.e., 6-monoacetylmorphine and morphine). Some compounds commonly found in drug laboratories may cause false positives with tris(2,2'-bipyridyl)ruthenium(III), but do not produce the markedly increased response with the permanganate reagent after the hydrolysis procedure. The combination of these two tests therefore provides an effective presumptive test for the presence of 3,6-diacetylmorphine, which we have verified with 14 samples obtained from a forensic science laboratory.