Bromatometric assay of simvastatin in pharmaceuticals

Tharpa, K. and Basavaiah, K. (2009) Bromatometric assay of simvastatin in pharmaceuticals. JOURNAL OF ANALYTICAL CHEMISTRY, 64 (11). pp. 1193-1198. ISSN 1061-9348

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Titrimetric and spectrophotometric methods are proposed for the determination of simvastatin (SMT) in bulk drug and in tablets. The methods employ bromate-bromide mixture in acid medium as the brominating agent and iron (III) and thiocyanate as auxiliary regents. In titrimetry, SMT is treated with a measured excess of bromate-bromide mixture in HCl medium, and after a definite time, the unreacted bromine is determined iodometrically. In spectrophotometric method, the residual bromine is reduced by iron (II) and the resulting iron (III) is complexed with thiocyanate, and the absorbance is measured at 470 nm. In both methods, the amount of in situ generated bromine corresponds to the SMT content. The experimental conditions are optimized. Titrimetry is applicable over 1-10 mg range and the calculations are based on the molar ratio of 1: 0.666 (SMT: KBrO3). In spectrophotometric method, Beer's law is obeyed over the concentration range 1-10 A mu g/mL. The calculated molar absorptivity is 3.02 x 10(4) L/mol cm and the corresponding sandel sensitivity being 0.0081 A mu g/cm(2). The limit of detection (LOD) and limit of quantification (LOQ) are calculated to be 0.10 and 0.31 A mu g/mL, respectively. The intra-day and inter-day precision calculated from the analysis of pure SMT were less than 2 and 2.7%, respectively. The methods were satisfactorily applied to the determination of SMT in tablets, and no interferences from common tablet excipients were observed. The validity of the methods was further ascertained by parallel assay by an established technique and by recovery studies.

Item Type: Article
Subjects: C Chemical Science > Chemistry
Divisions: Department of > Chemistry
Depositing User: Users 19 not found.
Date Deposited: 14 Aug 2019 07:52
Last Modified: 14 Aug 2019 07:52

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