You are hereMETHOD DEVELOPMENT AND ITS VALIDATION FOR ESTIMATION OF DEFLAZACORT IN TABLET DOSAGE FORM BY UV SPECTROPHOTOMETRY

METHOD DEVELOPMENT AND ITS VALIDATION FOR ESTIMATION OF DEFLAZACORT IN TABLET DOSAGE FORM BY UV SPECTROPHOTOMETRY


About Authors:
Kapil Sharma*1, Subhash Gupta2, Priyanka Sharma1
1Yaresun Pharmaceutical Pvt. Ltd.,India.
2Oasis test house ltd.
jaipur-302006,rajasthan,india.
*pharma_kapil@rediffmail.com

ABSTRACT
This paper describe a simple, precise and economical spectrophotometric method for the quantitative determination of Deflazacort(DFCT) in tablet dosage form. Method is based on the estimation of DFCT in aqueous acetonitrileat 246 nm. Beer’s law was obeyed in the concentration range of 4-14 µg/ml. The accuracy of the method was assessed by recovery studies and was found to be 99.38±0.15 for DFCT. Results of the analysis were validated statistically so that it can be used for routine analysis of DFCT in tablet dosage form.

Reference Id: PHARMATUTOR-ART-1416

INTRODUCTION
The deflazacort is (11b, 21-Dihydroxy-2'-methyl-5'bH-pregna-1, 4-dieno [17,16-d] oxazole-3,20 dione 21-acetate) is an oxazoline derivative of prednisolone of anti-inflammatory and immunosuppressive activity. It acts by blocking the secretion producing immune and allergic conditions, as a result of  inflammation. It also lowers white blood cells of the blood. So, can block the rejection of organ transplants, as it prevents the body from attacking foreign tissue. It is useful in Nephrotic syndrome,Uveitis, Pemphigus, leukemia, andAsthma1.It is not official in any pharmacopoeia. Literature survey reveals that there is no any simple spectroscopic method for determination of deflazacort in aqueous acetonitrile at 246 nm2-6. Hence the objective of the work is to develop new spectrophotometric method for its estimation in tablet dosage form with good accuracy, simplicity, precision and economy. The result of analysis using the spectrometric method for quantitative determination was found to be satisfactory such that the developed method can be used for routine analysis of drug from tablet dosage form.

MATERIAL AND METHOD
Instrument
, reagents and chemicals
A dual-beam shimadzu UV-visible spectrophotometer 1601 was used. Aqueous Acetonitrile (LR, Merck, mumbai) was used as solvent. Gift sample of DFCT was procured from Zydus Cadila Healthcare India. Tablets of 6 mg strength were procured from local pharmacy.

Stock solution
Stock solution of containing 500 µg/ml of deflazacort was prepared by dissolving 25 mg deflazacort in 50 ml Aqueous Acetonitrile.

Standard solution
Standard solution of containing 10 µg/ml was prepared by dissolving 5 ml deflazacort stock solution in 50 ml Aqueous Acetonitrile. Standard solution was analyzed by UV-spectrophotometer. Maximum absorbance for deflazacort was found to be at 246 nm. The spectrum was shown in figure 1.

Linearity and accuracy
Linearity and accuracy in the concentration range of 1-14 µg/ml were examined employing intraday and interday studies for the determination of DFCT. The results for intraday and interday experiments with a good correlation were obtained and evaluated statistically as demonstrated in table 1 and 2.calibration curve is shown in figure 2.

Application of proposed procedure for the determination of deflazacortin tablet dosage form
Twenty tablets were taken, and accurately weighed. The tablets were crushed to a fine powder. The powder sample equivalent to 6 mg of deflazacort was transferred to a 100 ml volumetric flask and about 80 ml of Aqueous Acetonitrile was added and sonicated to dissolve. The volume was made up to the mark with Aqueous Acetonitrile. This solution was filtered through whatman filter paper 42. 10 ml of this solution was diluted to 100 ml with Aqueous Acetonitrile. The solutions were analyzed by UV-spectrophotometer. Aqueous Acetonitrile  was used as blank.

RESULTS AND DISCUSSIONS
A UV-spectrophotometric method was developed for the estimation of deflazacort in tablet dosage form were found to be simple, accurate, precise and reproducible.Method is based on the estimation of deflazacort in Aqueous Acetonitrileat 246 nm. Beer’s law was obeyed in the concentration range of 4-14µg/ml. The value of standard deviation was satisfactory and the recovery studies were close to 100%.Hence this method can be used in the routine analysis of deflazacort in tablet dosage form7.

ACKNOWLEDGEMENTS
The authors are thankful to Yaresun pharmaceutical Pvt. Ltd for providing the facilities to carry out the work. The authors are also thankful to Zydus Cadila Healthcare Indiaproviding working standard of deflazacort.

REFERENCES
1.    Markham A., Bryson H. Deflazacort: A review of its pharmacological properties and therapeutic efficacy. Drugs. 1995; 50: 317-33.
2.    Santos-Montes A., Gonzalo-Lumbreras R.,Gasco-Lopez A.I.,Extraction and high-performance liquid chromatographic separation of deflazacort and its metabolite from urine samples. J. Chrom. B B.med. 1994; 657: 248-253.
3.    Method development for the determination of deflazacort in pharmaceutical dosage forms. Chromatographia. 2007; 65:591-594.
4.    Santos-Montes A., Izquierdo-Hornillos R.Optimization of separation of a complex mixture of natural and synthetic corticoids by micellar l.c. using sod. dodecyl sulphate: from urine samples. J. Chromatogr. B Biomed. Sci. Appl.1999; 724: 53-63.
5.      Ozkan Y., Savaser A., Tas C., Uslu B.,Ozkan S. Drug dissolution studies and determination of deflazacort in pharmaceutical formulations and human serum samples by RP-HPLC. J. Liq. Chromatogr.2003; 26: 2141-2156 .
6.    Ifa D., Moraes M., Moraes M., Santagada V., Caliendo G., Determination of 21-hydroxydeflazacort in human plasma hplc Asian Journal of Pharmacy and Life Science ISSN 2231 – 4423 Vol. 1 (3), July-Sept, 2011
7.    ICH, Q2 (R1) Validation of Analytical Procedure: Text and Methodology, International Conference on Harmonization,2005.

Table 1: Recovery study of deflazacort

S.No

Drug

Conc.  before

spiking

(mg/ml)

Reference Std.

added

(mg/ml)

Conc. after

spiking

(mg/ml)

percent

Recovery

Mean

percent

Recovery

1

deflazacort

8.00

4.00

12.08

99.33

99.38

±

0.15

8.00

6.00

14.10

99.29

8.00

8.00

16.07

99.56

Table 2: Summary of validation parameters7

PARAMETER

OBSERVATION

Specificity

No interference was found w.r.t. excipients

Linearity
(Correlation coefficient r2)

0.999

Accuracy

(% Recovery)

99.38

Precision RSD

Repeatability (n= 6)

Intra-day (n=3)

Inter-day (days=3)

0.62

0.74

0.82

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