Fluorometrische Bestimmung einiger 1,4‐Benzodiazepine

Abstract

Einige pharmazeutisch interessante 1.4-Benzodiazepine konnen nach Behandlung mit Zink/Salzsaure durch Umsetzung mit o-Phthalaldehyd in fluoreszierende Produkte iiberfiihrt werden. Dies ermoglicht die fluorometrische Bestimmung von Oxazepam, Lorazepam, Dikaliumchlorazepat, Demoxepam und Chlordiazepoxid wie sie fur Nitrazepam bekannt ist. Die Zuverlassigkeitskriterien des Verfahrens werden am Beispiel Oxazepam demonstriert. Fluorometric Determination of some 1,4-Benzodiazepines Some pharmaceutically interesting 1.4-benzodiazepines can be converted into fluorescent products with o-phthalaldehyde after treatment with zinc/hydrochloric acid. This permits the fluorometric determination of oxazepam, lorazepam, dipotassium chloroazepate, demoxepam and chlorodiazepoxide. The reliability of the method is demonstrated with oxazepam as an example. 0-Phthalaldehyd (OPTA) kann zum fluorornetrischen Nachweis verschiedener Substanzen eingesetzt werden. So bilden z. B. Indolderivate", Aminosauren" und Amine-" unter geeigneten Bedingungen mit O P T A fluoreszierende Produkte, die teilweise zur quantitativen Bestimmung der Stoffe herangezogen werden konnen. Die Struktur d e r fluoreszierenden Verbindungen ist bisher nur in wenigen Fallen geklart4.s.6). Auch 03654233/81/030M204 f UZ.SO/O The N,O-Acylals 5-l5 are obtainable from the chloro compounds 2 and carboxylic acids. Treatment of the electrophilic synthons with nucleophiles under basic conditions leads to products 1619 by way of transamidoalkylation. A mechanism of the reaction is proposed. o w -m 3 / 8 1~) 3 0~0 9 s m.so/o

Applying cloud point extraction technique for the extraction of oxazepam from human urine as a colour or fluorescent derivative prior to spectroscopic analysis methods

“…The recording of absorption spectrum for different agents used showed that the first band is due to oxine and this reagent does not show any significant absorbance at the analytical wavelength. The native fluorescence of BZPs is very low and a suitable signal intensity is only obtained either by cyclization to acridines after hydrolysis to benzophenones, [20] thermal heating in acidic solvent, [37] photochemical degradation, [38] derivatization with phthalaldehyde and fluorescamine, [39] or by reduction of the target compounds with Zn • /HCl to form highly fluorescent derivatives. [40] Native fluorescence of some BZPs in acidic or methanolic KOH solution was also reported.…”