RESUMO
Adrenergic amines found in extracts of Citrus aurantium (bitter orange) evoke analytically useful chemiluminescence with acidic potassium permanganate in the presence of polyphosphates. From corrected chemiluminescence spectra, the wavelength of maximum intensity for these reactions was 680+/-5 nm and, using flow injection analysis methodology, limits of detection for synephrine, octopamine, tyramine and hordenine were found to be between 1x10(-9) and 1x10(-8) M. We have applied this method of detection to the rapid determination of synephrine in dietary supplements using monolithic column chromatography.
Assuntos
Fármacos Antiobesidade/análise , Cromatografia Líquida de Alta Pressão/métodos , Permanganato de Potássio/química , Sinefrina/análise , Química Farmacêutica , LuminescênciaRESUMO
This paper describes a procedure for the determination of psilocin and psilocybin in mushroom extracts using high-performance liquid chromatography with postcolumn chemiluminescence detection. A number of extraction methods for psilocin and psilocybin in hallucinogenic mushrooms were investigated, with a simple methanolic extraction being found to be most effective. Psilocin and psilocybin were extracted from a variety of hallucinogenic mushrooms using methanol. The analytes were separated on a C12 column using a (95:5% v/v) methanol:10 mM ammonium formate, pH 3.5 mobile phase with a run time of 5 min. Detection was realized through a dual reagent chemiluminescence detection system of acidic potassium permanganate and tris(2,2'-bipyridyl)ruthenium(II). The chemiluminescence detection system gave improved detectability when compared with UV absorption at 269 nm, with detection limits of 1.2 x 10(-8) and 3.5 x 10(-9) mol/L being obtained for psilocin and psilocybin, respectively. The procedure was applied to the determination of psilocin and psilocybin in three Australian species of hallucinogenic mushroom.
Assuntos
Agaricales/química , Cromatografia Líquida de Alta Pressão , Alucinógenos/análise , Medições Luminescentes/métodos , Psilocibina/análogos & derivados , Psilocibina/análise , Indicadores e Reagentes , Compostos Organometálicos , Permanganato de PotássioRESUMO
A simple and rapid method for the analysis of carbohydrates in heroin samples by capillary electrophoresis utilizing a borate complexation method is described. Separations were performed using an uncoated fused silica capillary, 50 cm x 50 micro I.D. x 360 microm O.D. with an effective separation length of 9 cm. The system was run at 60 degrees C with an applied voltage of -8 kilovolts. Injection of each sample was for 1 sec at -50 mbar. UV detection was employed with the wavelength set at 195 nm. The background electrolyte consisted of 65 mM borate, pH 12.0. Samples and standards were prepared in the run buffer containing 2 mg/mL of mannose as an internal standard. Under these conditions a test mixture containing glucose, sucrose, lactose, mannitol and mannose as an internal standard was resolved within 5 min. The method was used to determine the concentration of carbohydrates in heroin seizure samples and synthetic heroin samples. The results were in good agreement with the reported values.
RESUMO
A simple and rapid method for the analysis of heroin seizures by micellar electrokinetic chromatography with short-end injection is described. Separations were performed using an uncoated fused silica capillary, 50 cm x 50 microm I.D. x 360 microm O.D. with an effective separation length of 8 cm. The system was run at 25 degrees C with an applied negative voltage of -25 kilovolts. Injection of each sample was for 2 s at -50 mbar. UV detection was employed with the wavelength set at 210 nm. The background electrolyte consisted of 85:15 (water:acetonitrile, v/v) containing final concentrations of 25 mM SDS and 15 mM sodium borate, pH 9.5. Samples and standards were prepared in 0.1% v/v acetic acid and diluted in the run buffer containing 1 mg/ml of N,N-dimethyl-5-methoxytryptamine as an internal standard. Under these conditions a text mixture containing caffeine, paracetamol, morphine, codeine, heroin, and acetylcodeine was resolved within 1.5 min. The method was used to determine the concentration of heroin in heroin seizure samples, and the results were in good agreement with those obtained by a validated gas chromatographic method.
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This paper reviews recent applications of capillary electrophoresis to forensic drug analysis and covers the literature since 2001. A brief overview of capillary electrophoresis is followed by a discussion of analytical applications which have been categorized into two sections: (i) drug seizures and non-biological samples, and (ii) forensic toxicology and biological samples.
RESUMO
A simple, rapid and sensitive method for the determination of psilocin and psilocybin is described. This is the first report on the determination of psilocin and psilocybin using flow injection analysis with acidic potassium permanganate and tris(2,2'-bipyridyl)ruthenium(II) chemiluminescence. The limits of detection (signal-to-noise ratio=3) are 9x10(-10)M and 3x10(-10)M for psilocin and psilocybin, respectively. A concise synthetic route for psilocin in three steps from readily available starting materials is also described. The structures were elucidated on the basis of spectroscopic data.
RESUMO
The limits of detection (3s) for ascorbic acid were 5x10(-8)M with acidic potassium permanganate using both flow injection analysis (FIA) and sequential injection analysis (SIA) whereas the soluble manganese(IV) afforded 1x10(-8)M and 5x10(-9)M for FIA and SIA, respectively. Determinations of ascorbic acid in Vitamin C tablets were achieved with minimal sample pretreatment using a standard additions calibration and gave good agreement with those of iodimetric titration.
RESUMO
The postmortem concentrations of citalopram in blood, bile, liver, and vitreous humour were investigated in 14 cases using a specially developed high performance liquid chromatography assay. Concentrations from drug and non-drug related deaths were categorized to determine a postmortem therapeutic and toxic range. Therapeutic citalopram concentrations for blood, bile, liver, and vitreous humour ranged to 0.4 mg/L, 2.1 mg/l, 6.6 mg/kg, and 0.2 mg/L, respectively. In one potentially fatal response to citalopram, concentrations were 0.8 mg/L, 6.0 mg/L, 0.3 mg/L for blood, bile and vitreous humour, respectively.