Spectrophotometric Estimation of Granisetron in Bulk and Tablet Formulation

 

S. Angayer Kanchana, Ajithadas Aruna^*, V. Niraimathi and A. Jerad Suresh

Department of Pharmaceutical Chemistry, Madras Medical College, Chennai – 600 003. India

*Corresponding Author E-mail: aruna_anantha@yahoo.com; angayer.kanchi@gmail.com

ABSTRACT:

Three simple, precise and economical spectrophotometric methods have been developed for the estimation of granisetron in bulk and pharmaceutical preparations. Method A is based on the reaction of granisetron with Ferric chloride and 2, 2’ Bipyridyl to form blood red chromogen and followed by measuring the absorbance at 522nm. Method B is based on the reaction of granisetron with Ferric chloride and Potassium Ferricyanide to form bluish green chromogen and followed by measuring the absorbance at 820nm. Method C involves the determination of granisetron by absorbance ratio method. In this method the ratio of absorbances at any two wavelengths (301nm and 225nm) is constant for all concentrations were determined. The results of the analysis were validated statistically and found to be satisfactory.

 

 

 

INTRODUCTION:

Granisetron is chemically 1-methyl–N–[(3-endo)-9-methyl-9-azabicyclo[3.3.1]non-3yl]-1H-indazole-3-carboxamide¹ and is used as an antiemetic in chemotherapy induced vomiting. The various other methods for estimation of granisetron by spectrophotometry have been published by the same authors of this paper^2-3 and no method has been reported by RP–HPLC method except estimation of the drug in biological fluids^4-6.

 

EXPERIMENTAL:

Instrumentation:

All spectral measurements were made on Shimadzu UV-VIS spectrophotometer – 1650 with 1cm matched quartz cells.

 

Preparation of standard stock solution:

An accurately weighed amount of 100mg of GSN taken in 100mL volumetric flask and dissolved in 25mL of distilled water and then made up to volume with distilled water.

 

Preparation of sample solution:

The average weight of 20 tablets of GSN was determined and finely powdered. The powder equivalent to 10mg of GSN was taken in 100mL volumetric flask and dissolved in 25mL of distilled water and then made up to volume with the same distilled water.

 

Reagents:

All the reagents used were of analytical reagent grade. All the solutions were freshly prepared with distilled warer. The reagents used in method A were Ferric chloride (0.03M) and 2,2’ Bipyridyl (0.01M) and the reagents used for method B were Ferric chloride (0.5%)  and Potassium ferricyanide (0.15%).

 

ASSAY PROCEDURE:

METHOD A:

Aliquots of the standard stock solution were transferred to a series of 25mL volumetric flasks, and 1mL of 0.03M ferric chloride solution and 2.0 mL of 0.01M 2, 2’ bipyridyl was added. The standard flask were then heated on a water bath for 15 minutes at 60°C, cooled to room temperature and the total volume was made up to 25mL with distilled warer. The absorbance of the blood red colored species was measured at 522nm against reagent blank⁷. The amount of granisetron present in the sample solution was computed from its calibration curve.

 

METHOD B:

Aliquots of the standard stock solution were transferred to a series of 25mL volumetric flasks, and 2mL of 0.5% ferric chloride solution and 2.0 mL of 0.15% potassium ferricyanide⁸ was added. The standard flask were then heated on a water bath for 2 minutes at 100 C, cooled to room temperature and the total volume was made up to 25mL with distilled water. The absorbance of the bluish green chromogen was measured at 820nm against reagent blank. The amount of granisetron present in the sample solution was computed from its calibration curve.

 

TABLE–1: OPTICAL CHARACTERESTICS FOR GRANISETRON

Parameters	Method A	Method B	Method C
λmax	522	820	225and301
Beer’s law Limit (µg/mL)	8-56	20-120	5-30
Molar absorptivity (L mol-1 cm-1)	5,233.2	4,048.94	-
Sandell’s sensitivity (µg cm-2/ 0.001 abs unit)	0.0009523	0.003497	-
Slope	0.01495	0.01152	-
Intercept	0.00225	0.0025	-
Regression Equation(y=mx+c)	0.01495x+ 0.00225	0.01152x+ 0.0025	-
Correlation coefficient	0.9999	0.9999	-
%RSD	0.5019	0.7469	-
LOD	1.0634	1.5509	-
LOQ	3.2225	4.6999	-

 

TABLE–2:  ASSAY AND RECOVERY OF GRANISETRON AND ITS FORMULATIONS

Method	Label Claim (mg/tablet)	Amount obtained (mg)*	% Lable claim	**% Recovery by the proposed methods*
				Amount added	Amount Recovered	% recovery
Method A	1.000mg	1.0005	100.05	0.5 1.0 1.5	0.5005 0.9972 1.4958	100.10 99.72 99.72
Method B		0.9968	99.68	0.5 1.0 1.5	0.4993 1.0012 1.4722	99.87 100.12 98.15
Method C		0.9990	99.90	0.5 1.0 1.5	0.5010 0.9953 1.4985	100.21 99.53 99.90

*   Each average of three determinations

** After spiking the sample

 

METHOD C:

Aliquots of the standard stock solution were transferred to a series of 100mL volumetric flask and suitably diluted to give a varying concentrations ranging from 5–30µg/mL and the solutions were scanned in the spectrum mode from 400-200nm using distilled water as blank and the absorbance were measured at 301nm and 225nm. The ratio of absorbance⁹ was calculated. The same procedure was adopted for Pharmaceutical formulations.

 

RESULTS AND DISCUSSION:

The optical characteristics such as %RSD, regression equation, correlation coefficient, slope and intercept for the two methods were calculated and the results are summarized in Table 1. To evaluate the validity and reproducibility of the methods, recovery studies were carried out by adding a known amount of pure drug to previously analyzed tablet powder sample and re-analyzed. The results obtained are presented in Table 2. Recovery studies revealed that the excipients and additives did not interfere. Hence these methods are most economic, simple, sensitive and accurate and can be used for the routine determination of GSN in pharmaceutical preparations.

 

REFERENCES:

1.        The Merck Index, Merck and Co. Inc., Whitehouse Station, NJ, 13th edition, pp808 (2001).

2.        S. Angayer Kanchana, Ajithadas Aruna, V.Niraimathi and A. Jerad Suresh. Spectrophotometric estimation of Granisetron in Bulk and Tablet Formulation. International Journal of Chemical Sciences 2010. 8(2):1169-1173.

3.        Angayer kanchana S, Aruna A, Niraimathi V, Jerad Suresh A. First order and AUC Method for the estimation of Granisetron in Bulk and Tablet Formulation Acta Ciencia Indica 2010. XXXVIC No.1: 29-31.

4.        Wada I, Santoh M, Takeda T, Nakabayashi T, Honma T, Takada M and  Hirano K. A HPLC method developed for the rapid assay of granisetron in biological fluids from cancer patients. Biol pharm Bull 1998. 21(5):535-7.

5.        Pinguet F, Bressolle F, Martel P, Salabert D, Astre C. High-Performance liquid chromatographic determination of granisetron in human plasma. J chromatogr B Biomed Appl 1996. 12;675(1):99-105.

6.        Capacio BR, Byers CE, Jackson TK, Matthews RL. A high-performance liquid chromatographic method for the determination of granisetron in guinea pig plasma. J Anal Toxicol 1993. 17(3):151-5.

7.        Annapurna MM, Bhanoji Rao ME, Ravi Kumar BVV. Spectrophotometric determination of Raloxifene hydrochloride in Pharmaceutical formulations. E-Journal of Chemistry 2007. 4(1):79-82.

8.        Syed AA, Ayesha S. Spectrophotometic determination of certain Benzimidazole Proton Pump Inhibitors. Indian Journal of Pharmaceutical Sciences 2008. 70(4): 507-510.

9.        Beckett AH, Stenlake JB.“Practical Pharmaceutical Chemistry” 4^th edition, Part two, CBS Publishers and distributors, New Delhi 2007.284-286,286-288.

 

 

 

 

Received on 31.08.2010          Modified on 16.09.2010

Accepted on 22.09.2010         © RJPT All right reserved