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E-Journal of Chemistry
Extractive Spectrophotometric Methods for the Determination of Rosuvastatin Calcium in Pure Form and in Pharmaceutical Formulations by Using Safranin O and Methylene blue
MAROTHU VAMSI KRISHNA and DANNANA GOWRI SANKAR* Pharmaceutical Analysis and Quality Assurance Division, Department of Pharmaceutical Sciences, Andhra University, Visakhapatnam, India. E-mail:marothu_vamsi@rediffmail.com Received 1 August 2006; Accepted 9 September 2006
Abstract: Two simple extractive Spectrophotometric methods are described for the determination of rosuvastatin calcium (RST) in pure form and in pharmaceutical formulations. These methods are based on the formation of ion association complexes of the RST with basic dyes safranin O (Method A) and methylene blue (Method B) in basic buffer of pH 9.8 followed by their extraction in chloroform. The absorbance of the chloroform layer for each method was measured at its appropriate max against the reagent blank. These methods have been statistically evaluated and are found to be precise and accurate. Keywords: Rosuvastatin Determination. calcium, Extractive Spectrophotometry,
Introduction
Rosuvastatin calcium (RST) is an anti hyperlipidimic agent and is chemically known as 6heptenoic acid, 7-[4-((4-fluorophenyl)-6-(1-methylethyl)-2-[methyl (methylsulphonyl) amino]-5-pyrimidinyl]-3, 5-dihydroxy-, calcium salt (2:1), (3R, 5S, 6E). It acts by inhibiting the enzyme 3-hydroxy-3-methyl glutaryl- coenzyme A (HMG-coA) reductase.To the best of our knowledge, there is no work in the literature reported about the visible spectrophotometric methods for the quantification of RST in pure drug and in pharmaceutical formulations, however one HPTLC 1 and few LC-MS 2-4 methods have been reported for the estimation of RST in pharmaceutical preparations and in biological fluids. The proposed methods are based on the formation of ion association complexes of the RST
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with basic dyes safranin O (SFN O) and methylene blue (MTB) in basic buffer of pH 9.8 followed by their extraction in chloroform.
Experimental
All spectral and absorbance measurements were made on a systronic model 106 digital spectrophotometer with 10mm matched quartz cells.
Apparatus
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proposed and reference methods are presented in Table 2. To evaluate the validity and reproducibility of the methods, known amounts of pure drug were added to the previously analyzed samples and the mixtures were analyzed by the proposed methods. The ingredients present in the formulations of RST did not interfere with the proposed analytical methods. In conclusion the proposed extractive spectrohotometric methods for the estimation of RST are simple, sensitive, accurate and useful for routine quality control analysis. Table1. Optical and regression characteristics, precision and accuracy of the proposed methods for RST Parameter max (nm) Beers law limits (g ml-1) Detection limits (g ml-1) Molar absorptivity (L mole-1 cm-1) Sandells sensitivity (g cm-2 / 0.001 absorbance unit) Optimum photometric range (g ml-1) Regression equation (Y = a + bC) Slope (b) Standard deviation of slope (Sb) Intercept (a) Standard deviation of intercept (Sa) Standard error of estimation (Se) Correlation coefficient (r) Relative standard deviation (%)* % Range of error (Confidence limits)* 0.05 level 0.01 level % Error in bulk samples**
*Average of eight determinations ** Average of three determinations In Y =a + bC, Y is absorbance and C is concentration.
Method A 530 5.0 25.0 0.099 3.60 x 104 0.027 6.0 23.0 3.61 x 10-2 0.70 x 10-4 - 3.00 x 10-4 1.20 x 10-3 1.14 x 10-3 0.9999 0.172 0.144 0.213 -0.260
Method B 655 2.5 12.5 0.076 6.54 x 104 0.015 3.5 10.5 6.52 x 10-2 2.00 x 10-4 1.40 x 10-3 1.67 x 10-3 1.59 x 10-3 0.9999 0.108 0.090 0.134 0.038
Table2. Results of analysis of tablet formulations containing RST Method A Formulations Fortius Rostar Novostat Fortius Rostar Novostat
b
B
a
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References
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