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Acta Pharmaceutica

The Journal of Croatian Pharmaceutical Society

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Use of Folin-Ciocalteu phenol reagent and 3-methyl-2-benzothiazolinone hydrazine hydrochloride in the determination of oxcarbazepine in pharmaceuticals

Muruganathan Gandhimathi1 / Thengungal Ravi1

Department of Pharmaceutical Analysis College of Pharmacy, Sri Ramakrishna Institute of Paramedical Sciences, Coimbatore, 641 044, India1

This content is open access.

Citation Information: Acta Pharmaceutica. Volume 58, Issue 1, Pages 111–118, ISSN (Online) 1846-9558, ISSN (Print) 1330-0075, DOI: 10.2478/v10007-007-0049-x, March 2008

Publication History

Published Online:
2008-03-12

Use of Folin-Ciocalteu phenol reagent and 3-methyl-2-benzothiazolinone hydrazine hydrochloride in the determination of oxcarbazepine in pharmaceuticals

Two spectrophotometric methods are proposed for the assay of oxcarbazepine (OXC) in bulk and dosage forms using Folin-Ciocalteu phenol reagent (FCP) and 3-methyl-2-benzothiazolinone hydrazine hydrochloride (MBTH) as reagents. The first method involves addition of FCP reagent to OXC in alkaline medium followed by measurement of absorbance at 760 nm (method A), and the other involves addition of a fixed volume of MBTH after treatment of OXC with ferric chloride and measurement of absorbance at 456 nm (method B). In both methods, the amount of chromogen formed corresponds to the amount of OXC and the measured absorbance was found to increase linearly with the concentration of OXC, which is corroborated by the correlation coefficients of 0.9985 and 0.9984 for method A and B, respectively.

The systems obey Beer's law for 5--30 μg mL-1 and 10--50 μg mL-1 for methods A and B, respectively. The apparent molar absorptivity was calculated to be 8.06 x 103 L mol-1 cm-1 and 3.126 x 103 L mol-1 cm-1 for methods A and B, respectively. The limits of detection (LOD) and limit of quantification (LOQ) were calculated to be 1.6 and 5 μg mL-1 for method A and 3 and 10 μg mL-1 for method B. The inter-day and intra-day imprecision of the methods were found to be in the range of 1.1--1.7 and 0.9--1.1% for method A, and 1.1--1.9 and 0.6--0.9% for method B. The accuracy ranged between 98.9--99.7% and 99.3--100.1 for method A and B, respectively. No interference was observed from common pharmaceutical excipients. The methods were successfully applied to the assay of OXC in tablet preparations.

Upotreba Folin-Ciocalteuovog reagensa i 3-metil-2-benzotiazolinon hidrazin hidroklorida u određivanju okskarbazepina u ljekovitim pripravcima

Predložene su dvije spektrofotometrijske metode za određivanje okskarbazepina (OXC) koje koriste Folin-Ciocalteu fenolni reagens (FCP) i 3-metil-2-benzotiazolinon hidrazin hidroklorid (MBTH). Predložene metode uspješno su primijenjene za analizu ljekovite tvari i ljekovitih pripravaka. Prva metoda uključuje adiciju FCP reagensa na OXC u lužnatom mediju i mjerenje apsorbancije pri 760 nm (metoda A), a druga adiciju istog volumena MBTH nakon obrade OXC sa željezovim(III) kloridom i mjerenje apsorbancije pri 456 nm (metoda B). U obje metode količina stvorenog kromogena proporcionalna je količini OXC, a izmjerena apsorbancija linearno raste s koncentracijom OXC, uz koeficijent korelacije 0,9985 i 0,9984 za metodu A odnosno B. Oba sustava podliježu Beerovom zakonu u koncentracijskom području 530 μg mL-1 i 10-50 μg mL-1 za metodu A odnosno B. Izračunati molni apsorpcijski koeficijent bio je 8,06 x 103 L mol-1 cm-1 za metodu A i 3,126 x 103 L mol-1 cm-1 za metodu B. Granice detekcije (LOD) i granice kvantifikacije (LOQ) bile su 1,6 i 5 μg mL-1 za metodu A i 3 i 10 μg mL-1 za metodu B. Nepreciznost unutar dana i između dana bila je 1,1-1,7 i 0,9-1,1% za metodu A, odnosno 1,1-1,9 i 0,6-0,9% za metodu B. Analitički povrat bio je 98,9-99,7% za metodu A i 99,3-100,1 za metodu B. Nije primijećena interferencija uobičajenih pomoćnih tvari. Metode su uspješno upotrijebljene za određivanje OXC u tabletama.

Keywords: okskarbazepin; spektrofotometrija; Folin-Ciocalteuov reagens; 3-metil-2-benzotiazolinon hidrazin hidroklorid; ljekoviti pripravci; validacija

Keywords: okskarbazepin; spektrofotometrija; Folin-Ciocalteuov reagens; 3-metil-2-benzotiazolinon hidrazin hidroklorid; ljekoviti pripravci; validacija

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