Limits...
Titrimetric and spectrophotometric assay of oxcarbazepine in pharmaceuticals using N-bromosuccinimide and bromopyrogallol red.

Rajendraprasad N, Basavaiah K, Vinay KB - Int J Anal Chem (2011)

Bottom Line: No interference was observed from common pharmaceutical adjuvants.Statistical comparison of the results with a reference method shows an excellent agreement and indicates no significant difference in accuracy and precision.The reliability of the methods was further ascertained by recovery studies in standard addition procedure.

View Article: PubMed Central - PubMed

Affiliation: Department of Chemistry, University of Mysore, Manasagangothri, Mysore-570 006, Karnataka, India.

ABSTRACT
Titrimetric and spectrophotometric methods are described for the determination of oxcarbazepine (OXC) in bulk drug and in tablets. The methods use N-bromosuccinimide (NBS) and bromopyrogallol red (BPR) as reagents. In titrimetry (method A), an acidified solution of OXC is titrated directly with NBS using methyl orange as indicator. Spectrophotometry (method B) involves the addition of known excess of NBS to an acidified solution of OXC followed by the determination of the unreacted NBS by reacting with BPR and measuring the absorbance of the unreacted dye at 460 nm. Titrimetry allows the determination of 6-18 mg of OXC and follows a reaction stoichiometry of 1 : 1 (OXC : NBS), whereas spectrophotometry is applicable over the concentration range of 0.8-8.0 μg mL(-1). Method B with a calculated molar absorptivity of 2.52 × 10(4) L mol(-1) cm(-1) is the most sensitive spectrophotometric method ever developed for OXC. The optical characteristics such as limits of detection (LOD), quantification (LOQ), and Sandell's sensitivity values are also reported for the spectrophotometric method. The accuracy and precision of the methods were studied on intraday and interday basis. The methods described could usefully be applied to routine quality control of tablets containing OXC. No interference was observed from common pharmaceutical adjuvants. Statistical comparison of the results with a reference method shows an excellent agreement and indicates no significant difference in accuracy and precision. The reliability of the methods was further ascertained by recovery studies in standard addition procedure.

No MeSH data available.


Study of reaction time between NBS and OXC in sulphuric acid medium and stability of the coloured species by measuring the absorbance of the unreacted BPR after reacting with NBS.
© Copyright Policy - open-access
Related In: Results  -  Collection


getmorefigures.php?uid=PMC3139870&req=5

fig2: Study of reaction time between NBS and OXC in sulphuric acid medium and stability of the coloured species by measuring the absorbance of the unreacted BPR after reacting with NBS.

Mentions: Under the described experimental conditions, the reaction between OXC and NBS was complete within 30 min (Figure 2) at room temperature (28 ± 2°C). After the addition of BPR, the reaction between NBS and dye was instantaneous and the absorbance of the unreacted dye was stable for at least 45 min, thereafter.


Titrimetric and spectrophotometric assay of oxcarbazepine in pharmaceuticals using N-bromosuccinimide and bromopyrogallol red.

Rajendraprasad N, Basavaiah K, Vinay KB - Int J Anal Chem (2011)

Study of reaction time between NBS and OXC in sulphuric acid medium and stability of the coloured species by measuring the absorbance of the unreacted BPR after reacting with NBS.
© Copyright Policy - open-access
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC3139870&req=5

fig2: Study of reaction time between NBS and OXC in sulphuric acid medium and stability of the coloured species by measuring the absorbance of the unreacted BPR after reacting with NBS.
Mentions: Under the described experimental conditions, the reaction between OXC and NBS was complete within 30 min (Figure 2) at room temperature (28 ± 2°C). After the addition of BPR, the reaction between NBS and dye was instantaneous and the absorbance of the unreacted dye was stable for at least 45 min, thereafter.

Bottom Line: No interference was observed from common pharmaceutical adjuvants.Statistical comparison of the results with a reference method shows an excellent agreement and indicates no significant difference in accuracy and precision.The reliability of the methods was further ascertained by recovery studies in standard addition procedure.

View Article: PubMed Central - PubMed

Affiliation: Department of Chemistry, University of Mysore, Manasagangothri, Mysore-570 006, Karnataka, India.

ABSTRACT
Titrimetric and spectrophotometric methods are described for the determination of oxcarbazepine (OXC) in bulk drug and in tablets. The methods use N-bromosuccinimide (NBS) and bromopyrogallol red (BPR) as reagents. In titrimetry (method A), an acidified solution of OXC is titrated directly with NBS using methyl orange as indicator. Spectrophotometry (method B) involves the addition of known excess of NBS to an acidified solution of OXC followed by the determination of the unreacted NBS by reacting with BPR and measuring the absorbance of the unreacted dye at 460 nm. Titrimetry allows the determination of 6-18 mg of OXC and follows a reaction stoichiometry of 1 : 1 (OXC : NBS), whereas spectrophotometry is applicable over the concentration range of 0.8-8.0 μg mL(-1). Method B with a calculated molar absorptivity of 2.52 × 10(4) L mol(-1) cm(-1) is the most sensitive spectrophotometric method ever developed for OXC. The optical characteristics such as limits of detection (LOD), quantification (LOQ), and Sandell's sensitivity values are also reported for the spectrophotometric method. The accuracy and precision of the methods were studied on intraday and interday basis. The methods described could usefully be applied to routine quality control of tablets containing OXC. No interference was observed from common pharmaceutical adjuvants. Statistical comparison of the results with a reference method shows an excellent agreement and indicates no significant difference in accuracy and precision. The reliability of the methods was further ascertained by recovery studies in standard addition procedure.

No MeSH data available.