Determination of Imatinib mesylate from Pharmaceutical Dosage Form by extractive ion pair complex colorimetric Method

 

Rele Rajan V.*, Prathamesh P. Tiwatane

Central Research Laboratory, D.G. Ruparel College, Mahim, Mumbai 400 016.

*Corresponding Author E-mail: drvinraj@gmail.com

 

ABSTRACT:

Simple sensitive and accurate extractive colorimetric method was developed for the estimation of Imatinib mesylate in Pharmaceutical dosage forms. The method was based on the formation of colored ion pair complexes by the drugs with thiocynate ions. These ion pair complexes were quantitatively extracted under the experimental condition in chloroform. The absorbance values were measured at 618 respectively. The proposed method was validated statistically. A recovery of method was carried out by standard addition methods. The Beer’s law ranges were found to be 1-12μg/ml, respectively. The low values of standard deviation and percentage RSD indicate high precision of method. Hence the method is useful for routine estimation of Imatinib mesylate in tablets respectively.

 

KEYWORDS: Imatinib Mesylate, Cobalt Nitrate, Ammonium Thiocynate, Chloroform.

 

 

INTRODUCTION:

It is a 4-[(4-methylpiperazin-1-yl)methyl]-N-(4-methyl-3-{[4-(pyridin-3-yl)pyrimidin-2-yl]amino}phenyl) benzamide, imatinib mesylate. It is known for chronic myelogenous leukemia and acute lymphocytic leukemia that are philadephia chromosome positive, certain types of gastrointestinal stromal tumors, hypersinoiphilic syndrome, chronic eosinophilic leukemia, systemic mastocytosis and myelodysplastic syndrome.

 

According to the literature review several methods has been developed for drug, like spectroscopy methods1-6. HPLC7-21, HPTLC22 and miscellaneous23,24. This extractive colorimetric can be used for the routine analysis. In the proposed methods optimization and validation of this method are reported.

 

MATERIALS AND METHODS:

A Shimadzu -160 A double beam UV-Visible recording spectrophotometer with pair of 10mm matched quartz cell was used to measure absorbance of solutions. A Shimadzu analytical balance was used.

 

Cobalt nitrate, Ammonium thiocynate, and chloroform of A.R. grade were used in the study.

 

Preparation of standard solution and reagents:

Stock solution of Imatinib mesylate (100μg/ml) was prepared in distilled water. From this stock solution working standard (10μg/ml) was prepared by diluting 10 ml stock solution to 100ml with distilled water.

 

Structure of Imatinib mesylate:

 

EXPERIMENTAL:

Preparation of solutions:

Stock solutions of Imatinib mesylate (100μg/ml) were prepared in distilled water.

 

From these stock solutions, working standard solutions (10μg/ml) were prepared by diluting 10 ml stock solution to 100μg/ml with distilled water.

 

Preparation of reagents:

Cobalt thiocynate was prepared by dissolving cobalt nitrate and ammonium thiocynate in 1:2 molar proportions in distilled water.

 

Experimental:

Into a series of separating funnels appropriate amount of the working standard drug solutions were pipetted out. To each funnel 2.1ml of cobalt thiocynate complex solution was added along with 10ml of chloroform to each funnel. The solutions were shaken for thorough mixing of the two phases and were allowed to stand for separation of the layers. The absorbance value of the chloroform layers were measured against their respective reagent blank at the wavelength of the maximum absorbance (λ max 61nm).

 

Estimation from tablets:

Twenty tablets of Imatinib mesylate were weighed accurately. Average weight of each tablet of Imatinib mesylate was determined. Tablets were crushed into fine powder. An accurately weighed quantity of powder equivalent to 10mg of Imatinib mesylate was transferred into a beaker and it was shaken with 50ml of distilled water and filtered. The filtrate and the washing were collected in a 100.0ml volumetric flask. This filtrate and the washing were diluted up to the mark with distilled water to obtain final concentration as 100μg/ml. A 10ml. of this solution was further diluted to give 10μg/ml.

 

Such solutions were further used for estimation of Imatinib mesylate respectively.

 

Appropriate aliquots of drug solution were taken. The individual assay procedures were carried out for the estimation of drug contents in tablets. The concentration of the drug in the tablets was calculated using calibration curve. Fig. no.1

 

RESULT:

The extractive spectrophotometric methods are popular due to their sensitivity in assay of the drug and hence ion pair extractive spectrophotometric methods have gain considerable attention for quantitative determination of many pharmaceutical preparations. These proposed methods are extractive spectrophotometric methods for the determination of imatinib mesylate by using chloroform as solvent from its formulations.

The colour ion –pair complexes are formed and are very stable. The working conditions of these methods were established by varying one parameter at time and keeping the other parameters fixed by observing the effect produced on the absorbance of the colour species. The various parameters involved for maximum colour development for these methods were optimized. The proposed methods were validated statistically and by recovery studies. The optical characteristics such as absorption maxima (nm), correlation coefficient (r) and were calculated and are also summarized in table I. Assay results of recovery studies are given in table no. 2.

 

Fig. no: 1. Calibration curve

 

 

The recovery experiment was carried out by standard addition method. The values of optical and regression terms of analysis are given in table no1.

 

 

Table 1: Values of results of optical and regression of drug

Parameter

Values

Detection Wavelength (nm)

618

Beer Law Limits (µg/ml)

1-12

Correlation coefficient(r2)

0.9999

Regression equation (y=b+ac)

 

Slope (a)

0.0005

Intercept (b)

0.006

 

Results are in good in agreement with labelled value. The percent recovery obtained indicates non interference from the common excipients used in the formulation.

 

Table no 2: Results of recovery studies

Amount of Sample Added in (µg/ml)

Amount of Standard Added in (µg/ml)

Total amount recovered

Percentage recovery (%)

Standard deviation

Percentage of relative standard deviation (C.O.V.)

2

0

2.015584

100.7792

0.09346

4.69884

2

2

4.036364

100.9091

0.082234

2.022518

2

4

6.015584

100.2597

0.053082

0.883082

2

6

8.033766

100.4221

0.037535

0.463453

 

 

 

 

Mean= 0.066578

Mean= 2.016973

 

DISCUSSION:

The reproducibility, repeatability and accuracy of these methods were found to be good, which is evidenced by low values of standard deviations. Colorimetric methods suggested in literature were applied in UV region, need costly reagents for development of chromogen and useful in higher concentration. The proposed methods are simple, sensitive, accurate, precise, and reproducible applicable to even very low concentration as compare to previous methods suggested in literature. They are directly applied to drug to form chromogen. Hence they can be successfully applied for the routine estimation of Imatinib mesylate in bulk and pharmaceutical dosage form even at very low concentration in formulation such as tablets. The strong recommendation is made here for the proposed methods for determination of Imatinib mesylate from its formulation.

 

ACKNOWLEDGMENT:

Authors express sincere thanks to the Principal, D. G. Ruparel College for providing necessary facilities and encouragement for research work.

 

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Received on 12.01.2024                    Modified on 17.02.2024

Accepted on 19.03.2024                   ©AJRC All right reserved

Asian J. Research Chem. 2024; 17(2):78-80.

DOI: 10.52711/0974-4150.2024.00015