Acta Pharm. 57 (2007) 87-98

full paper

Original research paper

 

Rapid titrimetric and spectrophotometric methods for salbutamol sulphate in pharmaceuticals using N-bromosuccinimide

 

KANAKAPURA BASAVAIAH1,* BANKAVADI CHIKKASWAMY SOMASHEKAR1

and VEERAIAH RAMAKRISHNA2

basavaiahk@yahoo.co.in

1Department of Chemistry, University of Mysore, Manasagangotri, Mysore-570 006, India

2Department of Pharmaceutical Chemistry, Government College of Pharmacy, Bangalore-27, India

Accepted December 4, 2006

 

One titrimetric and two spectrophotometric methods which are simple, sensitive and rapid are described for the assay of salbutamol sulphate (SBS) in bulk drug and in tablet dosage forms using N-bromosuccinimide (NBS) and two dyes, rhodamine-B and methylene blue, as reagents. In titrimetry, aqueous solution of salbutamol sulphate is treated with a measured excess of NBS in acetic acid medium and after the oxidation of SBS is complete, the unreacted oxidant is determined iodometrically. Spectrophotometric methods entail addition of a known excess of NBS in acid medium followed by the determination of residual oxidant by reacting with a fixed amount of either rhodamine B and measuring the absorbance at 555 nm (method A) or methylene blue and measuring the absorbance at 665 nm (method B). In all methods, the amount of NBS reacting corresponds to the amount of SBS content. Titrimetric method is applicable over 1.74 × 10-4 – 8.68 × 10-4 mol L-1 range and the reaction stoichiometry is found to be 1:6 (SBS:NBS). In spectrophotometric methods, the absorbance is found to increase linearly with the concentration of SBS, which is corroborated by the correlation of coefficients of 0.9993 and 0.9988 for method A and method B, respectively. The systems obey Beer’s law for 0.25-1.75 mg mL-1 (method A) and 0.5-5.0 mg mL-1 (method B). The calculated apparent molar absorptivity values were found to be 2.10 × 105 and 6.16 × 104 L mol-1 cm-1, for method A and method B, respectively. The limits of detection and quantification are also reported for both spectrophotometric methods. Intra-day and inter-day precision and accuracy for the developed methods were evaluated. The methods were successfully applied to the assay of SBS in tablet and capsule formulations and the results were statistically compared with those of a reference method. No interference was observed from common tablet adjuvants. The accuracy and reliability of the methods were further ascertained by recovery experiments via the standard-addition technique.

 

Keywords: salbutamol sulphate, assay, titrimetry, spectrophotometry, N-bromosuccinimide