You are on page 1of 2

M. Madhu Kiran, Prof. C. Ram Babu, Dr. S.V.

M Vardhan / International Journal of Engineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.com Vol. 3, Issue 1, January-February 2013, pp.312-313

Spectro Photometric Determination Of Deferasirox
M. Madhu Kiran*, Prof. C. Ram Babu**, Dr. S.V.M Vardhan***
*(Department of Chemistry, A. N. U Dr. M. R. Apparao Campus, Nuzvidu,) ** (HOD of Chemistry Dept., A. N. U Dr. M. R. Apparao Campus, Nuzvidu.) *** (Department of Bio- Chemistry, A. N. U Dr. M. R. Apparao Campus, Nuzvidu.)

ABSTRACT
A simple, novel and sensitive spectrophotometric method was developed for the determination of Deferasirox1-3 (DFX) in bulk and in pharmaceutical formulations. The method is based on Reduction of the drug in the presence of ferric chloride, followed by reaction under acidic conditions to produce a purple colored complex that exhibited maximum absorbance at λmax of 530 nm. Beer’s law is obeyed in the concentration range of 10 -50 mg / ml. Results of analysis were validated statistically and by recovery studies. This method could be successfully employed for the routine quality control analysis of Deferasirox (DFX) in various pharmaceutical preparations, bulk and dosage forms.

HPLC Coupled with MS-MS4, Magnetic resonance imaging5 , LC-MS6 and fluoroscence7 and no visible spectrophotometric methods This has prompted the author to select this drug for investigation and has succeeded in developing a simple, sensitive, novel and cost effective spectrophotometric method for the routine quality control analysis of DFX in Pharmaceutical formulations

EXPERIMENTAL
Instrumentation: Spectral and absorbance measurements are made with Genesys 10 UV split beam Spectrophotometer procured from Thermo Scientific Company marketed by Merck. Reagents: All the chemicals used were of annular grade. All the solutions were freshly prepared with double distilled water. Aqueous solutions of Ferric chloride (0.5% w/v), and concentrated nitric acid were prepared for the present investigation. Standard and Sample solution of Deferasirox: About 100mg of DFX (bulk dosage form) was dissolved in 100 ml of methanol and the total volume was brought to 100 ml with methanol to give a concentration of 1 mg/ml. 25 ml of the stock solution was diluted to 100 ml with methanol to give a concentration of 250 µg/ml. Assay Procedure: To a series of 10ml volumetric flasks, aliquot samples of reduced DFX ranging from 1.0 to 5.0 ml (1ml = 250 μg/ml) and aqueous solutions of ferric chloride (0.5 % , 2ml) and concentrated nitric acid (0. 5 ml) were added and kept aside for 5 minutes. The solution was made up to mark with methanol and after 5 minutes the absorbance of the purple colored solution was measured at 530 nm against the Corresponding reagent blank. The amount of DFX was computed from the corresponding calibration curve.

KEY

Deferasirox, reduction, validation, Beer’s Law

WORDS:

Spectroscopy,

INTRODUCTION
Deferasirox is 4-[(3Z, 5E)-3,5-bis(6-oxo-1cyclohexa-2,4-dienylidene)-1,2,4-triazolidin-1 yl]benzoic acid. Deferasirox is an oral iron chelator. Its main use is to reduce chronic iron overload in patients who are receiving long term blood transfusions for conditions such as beta-thalassemia and other chronic anemia’s. The structure of the drug with visible and reactive functional groups is as below

Fig: Structure of Deferasirox with reactive groups A very few methods appeared in the literature for the determination of Deferasirox (DFX) in biological fluids and pharmaceutical formulations. Based on the reactive groups and their diversity in the structure, various analytical techniques were proposed, some of which include

RESULTS AND DISCUSSION:
The proposed method was based on the reduction of the drug in the presence of ferric chloride under acidic conditions to produce a purple colored stable complex that exhibited maximum absorption at 530 nm against reagent blank. The optical characteristics

312 | P a g e

M. Madhu Kiran, Prof. C. Ram Babu, Dr. S.V.M Vardhan / International Journal of Engineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.com Vol. 3, Issue 1, January-February 2013, pp.312-313
such as absorption maxima, Beer’s law limits, molar absorptivity and sandell’s sensitivity are presented in Table-1. The regression analysis using the method of least squares was made for the slope (a), intercept (b) and correlation coefficient (γ) obtained from different concentrations was summarized in Table-1. The precision and accuracy were found by analyzing six replicate samples containing known amounts of the drug and the results are summarized in Table-1. The accuracy of the method was ascertained by comparing the results obtained with the proposed and reference methods in the case of formulations and are presented in Table-2. As an additional check on the accuracy of the method, recovery experiments were performed by adding known amounts of pure drug to pre-analyzed formulations and percent recovery values obtained are listed in Table-2. Recovery experiments indicated the absence of interferences from the commonly encountered pharmaceutical additives and excipients. Thus the proposed method is simple and sensitive with reasonable precision and accuracy. This method could be used for the routine determination of Deferasirox in quality control analysis. [6] June 2003, Vol. 101, No. 11, pp. 46324639. V.Kalyana Chakravarthy*, D. Gowri Sankar, LC determination of deferasirox in pharmaceutical Formulation, Journal of Global Trends in Pharmaceutical Sciences, Vol.1, Issue 1, pp 37- 45, Oct –Dec 2010. Jamshid L. Manzoori, Abolghasem Jouyban2, Mohammad Amjadi1, Vahid Panahi-Azar1, Elnaz Tamizi3, Jalil VaezGharamaleki4, Terbium-sensitized fluorescence method for the determination of deferasirox in biological fluids and tablet formulation, The journal of Biological and Chemical Luminiscence, Article first published online: 21 MAY 2010, DOI: 10.1002/bio.1218.

[7]

TABLE-1 Optical characteristics, precision and accuracy of the proposed method

REFERENCES
[1] Choudhry VP, Naithani R (2007). "Current status of iron overload and chelation with deferasirox". Indian J Pediatr 74 (8): 759– 64. Yang LP, Keam SJ, Keating GM (2007). "Deferasirox : a review of its use in the management of transfusional chronic iron overload". Drugs 67 (15): 2211–30. United States Food and Drug Administration (November 9, 2005). "FDA Approves First Oral Drug for Chronic Iron Overload". Press release. Retrieved 200710-31. Chauzit, Emmanuelle PharmD*; Bouchet, Stéphane PharmD*; Micheau, Marguerite MD†; Mahon, François Xavier MD, PhD, Moore, Nicholas MD, PhD*‡¶; Titier, Karine PharmD*; Molimard, Mathieu, A Method to Measure Deferasirox in Plasma Using HPLC Coupled With MS/MS Detection and its Potential Application, Therapeutic Drug Monitoring: August 2010 - Volume 32 - Issue 4 - pp 476-481. Peter D. Jensen, Finn T. Jensen, Thorkil Christensen, Hans Eiskjær, Ulrik Baandrup, and Johan L. Nielsen, Evaluation of myocardial iron by magnetic resonance imaging during iron chelation therapy with deferrioxamine: indication of close relation between myocardial iron content and chelatable iron pool, Blood, 1

[2]

[3]

[4]

* Y= a + bx, where’Y’is the absorbance and x is the concentration of DFX in μg/ml ** For six replicates. TABLE-2 Estimation of formulations

Deferasirox

in

Pharmaceutical

[5]

313 | P a g e