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Spektrofluorimetrijsko određivanje ciklopiroks olamina prevođenjem u ternarni kompleks s Tb(III) i EDTA

By MOHAMED IBRAHIM WALASH, MOHAMED SALEM RIZK, MANAL IBRAHIM EID and MONA EL SAYED FATHY

Abstract

A highly sensitive and selective spectrofluorimetric method was developed for the determination of ciclopirox olamine in raw material and in dosage forms. The proposed method is based on the formation of a ternary complex with Tb(III) in the presence of ethylenediaminetetraacetic acid. It was found that this complex manifests intense fluorescence at λem 489 and 545 nm with excitation at 295 nm. Different experimental parameters affecting the fluorescence intensity of the complex were carefully studied and incorporated into the procedure. Under the described conditions, the method is applicable over the concentration range of 30150 and 1070 ng mL-1 with minimum detectability of 6.7 and 0.9 ng mL-1 at λem 489 and 545 nm, respectively. The mean percentage recovery at λem 489 and λem 545 nm ranged between 98.7 and 100.2 for the pure substance, solution, and cream. Relative error of 0.10.4% and RSD up to 0.9% were estimated at λem 489 and 545 nm. A proposal of the reaction pathway is given.Razvijena je vrlo osjetljiva i selektivna spektrofluorimetrijska metoda za određivanje antimikotika ciklopiroks olamina, kao čiste supstancije i u ljekovitim oblicima. Metoda se temelji na stvaranju kompleksa s Tb(III) u prisutnosti etilendiamintetraoctene kiseline. Nakon ekscitacije pri 295 nm taj kompleks intenzivno fluorescira pri λem 489 i 545 nm. Proučavani su različiti eksperimentalni parametri koji utječu na intenzitet fluorescencije kompleksa. Za opisane uvjete metoda se može primijeniti u koncentracijskom području 30150 i 10 70 ng mL-1. Minimalna koncentracija koja se može odrediti je 6,7, odnosno 0,9 ng mL-1 na λem 489, odnosno 545 nm. Analitički povrat pri λem 489 i λem 545 nm iznosio je 98,7100,2% za čistu supstanciju, otopinu i kremu. Relativna pogreška metode je 0,10,4%, a relativna standardna devijacija 0,9%. Predložena je jednažba kemijske reakcije

Topics: ciclopirox olamine; Tb(III); EDTA; spectrofluorimetry; dosage forms, ciklopiroks olamin; Tb(III); EDTA; spektrofluorimetrija; dozirani ljekoviti oblici
Publisher: Croatian Pharmaceutical Society
Year: 2006
OAI identifier: oai:hrcak.srce.hr:4612

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