UV Spectrophotometric Method for Estimation of Eprosartan Mesylate in Bulk and in Pharmaceutical Formulation

 

Pandya Dimple Bhupendra1*, Shinkar Dattatraya Manohar2, Saudagar Ravindra Bhanudas3, Bacchav Jyoti Kailas4

1Department of Pharmaceutics, KCT’s R.G.S. College of Pharmacy, Anjaneri, Nashik-422213, Maharashtra.

3Department of Pharmaceutics, KCT’s R.G.S. College of Pharmacy, Anjaneri, Nashik-422213, Maharashtra.

4Department of Pharmaceutical Chemistry, KCT’s R.G.S. College of Pharmacy, Anjaneri, Nashik-422213, Maharashtra.

2Department of Quality Assurance Techniques, KCT’s R.G.S. College of Pharmacy, Anjaneri, Nashik-422213, Maharashtra.

*Corresponding Author E-mail: dimplepandya6293@gmail.com

 

ABSTRACT:

UV Spectrophotometric method provides a simple, efficient, precise and accurate method for development and validation of Eprosartan mesylate in bulk and its tablet formulation. The present study is based on measurement of the absorbance of Eprosartan mesylate solution in methanol: phosphate buffer pH 7.4 (10:90) at 293 nm in wavelength length of 200-400nm. Beers law was observed in the range of 5-25 ppm for this method. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantification which proves the suitability of this method for estimation of EPM in bulk and its tablet formulation. Results of recovery studies shows that the method was not affected by the presence of common excipients in tablets. Thus the method was found to be simple, economical, accurate and reproducible.

 

KEYWORDS: Eprosartan mesylate, UV Spectrophotometry, phosphate buffer ph7.4.

 

 

INTRODUCTION:

Eprosartan mesylate (EPM) is an antihypertensive agent which is chemically mono methane sulfonate of (E)-2- butyl-1-(p-carboxybenzyl)-α-2-thienylmethyl imidazole-5-acrylic acid. EPM is not official in any pharmacopoeia. EPM, a potent vasoconstrictor is the principal pressor agent of renin-angiotensin system. The present work aims to develop a simple, precise, accurate and validated UV Spectrophotometric method for estimation of EPM in pure and in tablet formulation using phosphate buffer pH 7.4.Confirmation of the applicability of the developed method was validated according to the International Conference on Harmonization guidelines for determination of EPM in pure and in tablet dosage form.

 

 

Fig. 1. Structure of Eprosartan mesylate.

 

MATERIALS AND METHODS:

MATERIALS:

Eprosartan mesylate was obtained as a gift sample from Mylan Pharmaceuticals Ltd, Sinnar, Nashik, India. All analytical grade chemicals and solvents were supplied by R.G. Sapkal College of Pharmacy, Nashik, India. Distilled water and phosphate buffer pH 7.4 was used to prepare all solutions.

Equipment:

The UV-Visible spectrophotometer (Jasco-630) with data processing system was used. The sample solution was recorded in 1cm quartz cell against solvent blank over 200-400nm. A citizen electronic analytical balance was used for weighing the sample. An ultrasonicatorbath (PCI Analytics Pvt Ltd) was used for sonicating the tablet powder.

 

Development of method:

Accurately weighed 10mg of Eprosartan mesylate was solubilized in 10ml of methanol in a volumetric flask and phosphate buffer pH 7.4 was added to make up the volume upto 100ml so as to give stock solution of concentration 100µg/ml. The standard solution were diluted with phosphate buffer pH 7.4 to obtain various dilutions (5, 10, 15, 20, 25µg/ml) in standard volumetric flask (10ml). The dilutions were scanned in wavelength range of 200-400 nm. The maximum of EPM was found at 293 nm. The linear relationship was observed over the range of 5-25µg/ml. Absorbance were noted at 293nm against pH 7.4 phosphate buffer as blank. A calibration graph of absorbance versus drug concentration of drug was plotted and represented in figure 2.

 

Procedure for dosage form:

For analysis of commercial formulations, ten tablets were taken and powdered. Tablet powder equivalent to 10 mg of EPM was dissolved in small quantity of methanol into 100 ml volumetric flask and final volume was made upto 100ml with phosphate buffer pH 7.4 and sonicated for 30min. Then the absorbance of solution (after suitable dilutions) was measured at 293 nm using UV Visible spectrophotometer (Jasco-630)against pH 7.4 buffer as blank. The % drug content was determined by using slope and intercept values from the calibration curve. (n=3).

 

Validation of the proposed method:

The proposed method was validated according to the ICH guidelines:

 

Linearity (calibration curve):

The developed method validates as per ICH guidelines. The plot of absorbance versus concentration is shown in figure 1. It can be seen that plot is linear in the concentration range of 5-25µg/ml with correlation coefficient R2 of 0.9992.

 

Precision (repeatability):

Intraday and interday precision was determined by the measurement of absorbance for three times on same day and on three different days. The relative standard deviation for replicates of sample solution was less than 2% which meet the acceptance criteria for established method. The obtained results are presented in table 1.

 

Table1: Precision study for proposed method:

CONC(µg/ML)

Absorbance mean

Standard deviation

% relative standard deviation

Intraday precision

 

 

 

5

0.2701

0.0059

0.021

10

0.4561

0.0034

0.0074

15

0.6324

0.0027

0.0043

Interday precision

 

 

 

5

0.2703

0.0061

0.0227

10

0.4537

0.0022

0.0049

15

0.6325

0.0024

0.0037

 

Table 2: recovery study:

Sr. no.

Label claim, mg/tablet

Amount of std added, mg

Total amount recovered

% recovery

Standard deviation

% relative SD

1

400

5

405.03

100.01

0.0670

0.0327

2

400

10

409.99

99.99

0.0435

0.0207

3

400

15

415.05

100.02

0.0644

0.0299

 

Accuracy (Recovery Study):

Recovery studies were carried out by adding a known quantity of pure drug to the pre analyzed formulation and the proposed method was followed. From the amount of drug found, percentage recovery was calculated as per ICH guidelines. The data were presented in table 2.

 

LOD and LOQ:

The limit of detection (LOD) and limit of quantification (LOQ) of drug were separately determined based on method of intercept and the average value of slope (i.e. 3.3 for LOD and 10 for LOQ) ratio using the following equations designated by ICH guidelines.

 

LOD=3.3б/S           LOQ=10б/S

 

Where, б=standard deviation of the response, S= slope of calibration curve.

 

RESULTS AND DISCUSSION:

Beer’s law is obeyed over the concentration range of 5-25µ, using regression analysis the linear equation y=0.0354x + 0.0994 with a correlation coefficient of 0.9992. The limit of detection was found to be 0.3169 µg/ml and the limit of quantification was found to be 0.9604 µg/ml. The percentage purity of EPM in formulation was found to be Precision was calculated with intra and inter day variation. Recovery study was performed on formulations and %RSD was found. The optical parameters such as Beers law limit, slope, and intercept values were calculated and given in table 3. Method was validated for accuracy and precision. The accuracy of method was proved by performing recovery studies in commercially available formulations. The results were given in table 2 and relative standard deviation of less than 2% was observed for analysis of three replicate samples, indicating precision and reproducibility. The percentage recovery value indicates that there is no interference from the excipients present in formulation. The applicability of the proposed method for assay of EPM in tablet formulation was examined by analyzing commercial formulations and results are tabulated in table 4. The results of analysis of commercial tablets and the recovery study of drug suggested that there is no interference from any excipient such as starch, lactose, magnesium stearate which are commonly present in tablets.

 

 

Fig 2: calibration curve of EPM at 293nm.

 

 

 

Table 3: Optical Parameters for Determination of EPM:

Sr. no

Parameter

Data

1

ƛ max(nm)

392

2

Beers law limit(µg/ml)

5-25

3

Regression equation

Y= 0.0354x + 0.0994

4

Slope (m)

0.0354

5

Intercept (c)

0.0994

6

Correlation coefficient (r)

0.9992

7

LOD (µg/ml)

0.3169

8

LOQ(µg/ml)

0.9604

 

 

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Received on 14.04.2016       Accepted on 05.04.2016     

© Asian Pharma Press All Right Reserved

Asian J. Pharm. Ana. 2016; 6(2): 119-121.

DOI: 10.5958/2231-5675.2016.00018.1