Rapid titrimetric and spectrophotometric determination of ofloxacin in pharmaceuticals using N-bromosuccinimide

One titrimetric and two spectrophotometric methods have been described for the determination of ofloxacin (OFX) in bulk drug and in tablets, employing N-Bromosuccinimide as an analytical reagent. The proposed methods involve the addition of a known excess of NBS to OFX in acid medium, followed by de...

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Príomhchruthaitheoirí: Kanakapura Basavaiah Vinay, Hosakere Doddarevanna Revanasiddappa, Okram Zenita Devi, Pavagada Jagannathamurthy Ramesh, Kanakapura Basavaiah
Formáid: Alt
Teanga:English
Foilsithe / Cruthaithe: Universidade de São Paulo 2011-06-01
Sraith:Brazilian Journal of Pharmaceutical Sciences
Ábhair:
Rochtain ar líne:http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1984-82502011000200006
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author Kanakapura Basavaiah Vinay
Hosakere Doddarevanna Revanasiddappa
Okram Zenita Devi
Pavagada Jagannathamurthy Ramesh
Kanakapura Basavaiah
author_facet Kanakapura Basavaiah Vinay
Hosakere Doddarevanna Revanasiddappa
Okram Zenita Devi
Pavagada Jagannathamurthy Ramesh
Kanakapura Basavaiah
author_sort Kanakapura Basavaiah Vinay
collection DOAJ
description One titrimetric and two spectrophotometric methods have been described for the determination of ofloxacin (OFX) in bulk drug and in tablets, employing N-Bromosuccinimide as an analytical reagent. The proposed methods involve the addition of a known excess of NBS to OFX in acid medium, followed by determination of unreacted NBS. In titrimetry, the unreacted NBS is determined iodometrically, and in spectrophotometry, unreacted NBS is determined by reacting with a fixed amount of either indigo carmine (Method A) or metanil yellow (Method B). In all the methods, the amount of NBS reacted corresponds to the amount of OFX. Titrimetry allows the determination of 1-8 mg of OFX and the calculations are based on a 1:5 (OFX:NBS) reaction stoichiometry. In spectrophotometry, Beer's law is obeyed in the concentration ranges 0.5-5.0 µg/mL for method A and 0.3-3.0 µg/mL for method B. The molar absorptivities are calculated to be 5.53x10(4) and 9.24x10(4) L/mol/cm for method A and method B, respectively. The methods developed were applied to the assay of OFX in tablets, and results compared statistically with those of a reference method. The accuracy and reliability of the methods were further ascertained by performing recovery tests via the standard-addition method.<br>Descrevem-se métodos, um titulométrico e dois espectrofotométricos, para a determinação de ofloxacino (OFX) na matéria-prima e em comprimidos, empregando a N-bromossuccinimida (NBS) como reagente analítico. Os métodos propostos envolvem a adição de excesso conhecido de NBS ao OFX, em meio ácido, seguida de determinação do NBS que não reagiu. Na titulometria, o NBS que não reagiu é determinado iodometricamente e na espectrofotometria, o NBS que não reagiu é determinado pela reação com quantidade fixa de índigo carmim (Método A) ou amarelo de metanila (Método B). Em todos os métodos, a quantidade de NBS que reagiu corresponde à quantidade de OFX. A titulometria permite a determinação de 1-8 mg de OFX e os cálculos se baseiam na estequiometria de reação de 1:5 (OFX:NBS). Na espectrofotometria, a Lei de Beer é obedecida nas faixas de concentração de 0,5-5,0 µg/mL, para o método A, e de 0,3-3,0 µg/mL, para o método B, respectivamente. Os métodos desenvolvidos foram aplicados para o teste de OFX em comprimidos e os resultados foram comparados estatisticamente com aqueles do método de referência. A precisão e a confiabilidade dos métodos foram, posteriormente, verificadas por meio dos testes de recuperação via método de adição de padrão.
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spelling doaj.art-2769d50e4ce44399aa2b51a22f5c3b922022-12-22T02:38:45ZengUniversidade de São PauloBrazilian Journal of Pharmaceutical Sciences1984-82502175-97902011-06-0147225126010.1590/S1984-82502011000200006Rapid titrimetric and spectrophotometric determination of ofloxacin in pharmaceuticals using N-bromosuccinimideKanakapura Basavaiah VinayHosakere Doddarevanna RevanasiddappaOkram Zenita DeviPavagada Jagannathamurthy RameshKanakapura BasavaiahOne titrimetric and two spectrophotometric methods have been described for the determination of ofloxacin (OFX) in bulk drug and in tablets, employing N-Bromosuccinimide as an analytical reagent. The proposed methods involve the addition of a known excess of NBS to OFX in acid medium, followed by determination of unreacted NBS. In titrimetry, the unreacted NBS is determined iodometrically, and in spectrophotometry, unreacted NBS is determined by reacting with a fixed amount of either indigo carmine (Method A) or metanil yellow (Method B). In all the methods, the amount of NBS reacted corresponds to the amount of OFX. Titrimetry allows the determination of 1-8 mg of OFX and the calculations are based on a 1:5 (OFX:NBS) reaction stoichiometry. In spectrophotometry, Beer's law is obeyed in the concentration ranges 0.5-5.0 µg/mL for method A and 0.3-3.0 µg/mL for method B. The molar absorptivities are calculated to be 5.53x10(4) and 9.24x10(4) L/mol/cm for method A and method B, respectively. The methods developed were applied to the assay of OFX in tablets, and results compared statistically with those of a reference method. The accuracy and reliability of the methods were further ascertained by performing recovery tests via the standard-addition method.<br>Descrevem-se métodos, um titulométrico e dois espectrofotométricos, para a determinação de ofloxacino (OFX) na matéria-prima e em comprimidos, empregando a N-bromossuccinimida (NBS) como reagente analítico. Os métodos propostos envolvem a adição de excesso conhecido de NBS ao OFX, em meio ácido, seguida de determinação do NBS que não reagiu. Na titulometria, o NBS que não reagiu é determinado iodometricamente e na espectrofotometria, o NBS que não reagiu é determinado pela reação com quantidade fixa de índigo carmim (Método A) ou amarelo de metanila (Método B). Em todos os métodos, a quantidade de NBS que reagiu corresponde à quantidade de OFX. A titulometria permite a determinação de 1-8 mg de OFX e os cálculos se baseiam na estequiometria de reação de 1:5 (OFX:NBS). Na espectrofotometria, a Lei de Beer é obedecida nas faixas de concentração de 0,5-5,0 µg/mL, para o método A, e de 0,3-3,0 µg/mL, para o método B, respectivamente. Os métodos desenvolvidos foram aplicados para o teste de OFX em comprimidos e os resultados foram comparados estatisticamente com aqueles do método de referência. A precisão e a confiabilidade dos métodos foram, posteriormente, verificadas por meio dos testes de recuperação via método de adição de padrão.http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1984-82502011000200006OfloxacinoTitulometriaEspectrofotometriaN-BromossuccinimidaComprimidosOfloxacinTitrimetrySpectrophotometryN-BromosuccinimideTablets
spellingShingle Kanakapura Basavaiah Vinay
Hosakere Doddarevanna Revanasiddappa
Okram Zenita Devi
Pavagada Jagannathamurthy Ramesh
Kanakapura Basavaiah
Rapid titrimetric and spectrophotometric determination of ofloxacin in pharmaceuticals using N-bromosuccinimide
Brazilian Journal of Pharmaceutical Sciences
Ofloxacino
Titulometria
Espectrofotometria
N-Bromossuccinimida
Comprimidos
Ofloxacin
Titrimetry
Spectrophotometry
N-Bromosuccinimide
Tablets
title Rapid titrimetric and spectrophotometric determination of ofloxacin in pharmaceuticals using N-bromosuccinimide
title_full Rapid titrimetric and spectrophotometric determination of ofloxacin in pharmaceuticals using N-bromosuccinimide
title_fullStr Rapid titrimetric and spectrophotometric determination of ofloxacin in pharmaceuticals using N-bromosuccinimide
title_full_unstemmed Rapid titrimetric and spectrophotometric determination of ofloxacin in pharmaceuticals using N-bromosuccinimide
title_short Rapid titrimetric and spectrophotometric determination of ofloxacin in pharmaceuticals using N-bromosuccinimide
title_sort rapid titrimetric and spectrophotometric determination of ofloxacin in pharmaceuticals using n bromosuccinimide
topic Ofloxacino
Titulometria
Espectrofotometria
N-Bromossuccinimida
Comprimidos
Ofloxacin
Titrimetry
Spectrophotometry
N-Bromosuccinimide
Tablets
url http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1984-82502011000200006
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