RESUMEN
A capillary zone electrophoretic method (CZE) was developed using an uncoated fused silica capillary for the separation and determination of the main tropane alkaloids. The applicability of the developed method for analysis of plant samples was examined by analyzing samples of transgenic Egyptian henbane Hyoscyamus muticus (L.) plants. A simple 40 mM phosphate buffer at pH 7.8 using a voltage of 20 kV was found the best for this purpose. The main tropane alkaloids, atropine and scopolamine as well as nor-(-)-scopolamine, and tropic acid, the precursor of tropane alkaloids, could be separated in less than 13 min. The linear concentration range for atropine was 5.00-140 microg ml(-1), for scopolamine 7.50-210 microg ml(-1) and for tropic acid 2.50-70.0 microg ml(-1).
Asunto(s)
Atropina/análisis , Electroforesis Capilar/métodos , Fenilpropionatos/análisis , Plantas Medicinales/química , Derivados de Escopolamina/análisis , Escopolamina/análisis , Atropina/aislamiento & purificación , Concentración de Iones de Hidrógeno , Concentración Osmolar , Fenilpropionatos/aislamiento & purificación , Plantas Modificadas Genéticamente , Escopolamina/aislamiento & purificación , Derivados de Escopolamina/aislamiento & purificación , Sensibilidad y EspecificidadRESUMEN
A stability-indicating high performance thin layer chromatography method for analyzing hydrolyzed tinidazole solutions using silica gel plates was developed and validated. The mobile phase used was methanol-diethyl ether-chloroform (1:9:3, v/v/v) allowing small changes in its composition. Detection was at 314 mm. Rf values being 0.1-0.4, baseline resolution was achieved for tinidazole and the hydrolysis products. The analytes were stable on the sorbent and could be precisely and accurately measured in the range 20-170 ng per band.
Asunto(s)
Antitricomonas/análisis , Tinidazol/análisis , Cromatografía en Capa Delgada/métodos , Densitometría , Estabilidad de Medicamentos , Hidrólisis , Reproducibilidad de los Resultados , Soluciones , Espectrofotometría UltravioletaRESUMEN
In a citrate-borate-phosphate buffer, 5 mM tinidazole solutions exhibited maximum stability stability around pH 4.0-5.0. The hydrolysis of tinidazole was mostly a first-order reaction. At pH 10.0 and 60-80 degrees C, tinidazole had an activation energy of 122 kJ mol-1 for hydrolysis. It was postulated that tinidazole decomposes by different mechanisms under basic and neutral/acidic conditions.
