Method development and Validation of UV Spectrophotometric estimation of Remogliflozin Etabonate in bulk and its tablet dosage form

 

Dave Vidhi*, Dr. Paresh Patel

Department of Quality Assurance, S.K. Patel College of Pharmaceutical Education and Research,

Ganpat University, Kherva , Gujarat, India

*Corresponding Author E-mail: vidhidave1988@gmail.com

 

ABSTRACT:

A simple, precise and sensitive UV spectrophotometric method has been developed for the estimation of Remogliflozin etabonate in bulk and pharmaceutical dosage Form. Remogliflozin etabonate shows Maximum Absorbance at 229nm. Beer’s law was obeyed in range of 2-10µg/ml. The correlation coefficient was found to be 0.9990. The result of interday and intraday precision shows standard deviation ranging from 0.050% - 0.254% and 0.058% - 0.258% for three concentration and three replicates. The Percentage recovery was found to be in the range of 98.94% - 99.86%. The LOD and LOQ were found to be 0.037µg/ml and 0.113µg/ml respectively. The purposed method was novel and successfully applied for the determination of Remogliflozin Etabonate in Tablet Dosage Form. The method was successfully validated according to ICH guidelines.

 

KEYWORDS: Remogliflozin Etabonate, UV Spectroscopic method.

 

 


INTRODUCTION:

Remogliflozin etabonate, chemically ethyl [(2R,3S,4S,5R,6S)-3,4,5-trihydroxy-6-[5-methyl-1-propan-2-yl-4-[(4-propan-2-yloxyphenyl)methyl]pyrazol-3-yl]oxyoxan-2-yl]methyl carbonate1-3, is an oral selective Sodium-Glucose co-transporter 2 (SGLT2) inhibitor used for the management of type 2 Diabetes Mellitus.  

 

Figure 1: Structure of Remogliflozin etabonate

 

The literature reveals that there is only One UV Spectrophotometric method and HPTLC method has been developed for Remogliflozin etabonate6.

 

The purpose of this work was to develop and validate simple, specific, sensitive, accurate, precise UV Spectroscopic method for the estimation of Remogliflozin etabonate in bulk and it’s tablet Dosage Form.

 

MATERIALS AND METHODS:

MATERIALS:

Remogliflozin etabonate working standard was procured as a gift sample from K Analytical Laboratory., Ahmedabad. Tablet Formulation of Remogliflozin etabonate (Remozen 10mg) manufactured by Glenmark Pharmaceuticals Ltd. was purchased from local market.

 

Chemicals and reagents:

All chemicals were of analytical grade.

 

INSTRUMENTATION:

A Shimadzu 1800 visible Spectrophotometer was used for spectral measurements. A high precision analytical balance was used for weighing the reagents. Ultrasonication was used for solubilization of drug.

 

PREPARATION OF STOCK SOLUTION:

The standard stock solution of Remogliflozin etabonate was prepared by dissolving 10mg drug in 10ml of methanol which gives 1000µg/ml concentration. From that 100µg/ml solution of Remogliflozin etabonate was prepared by taking 5ml of above µg/ml solution in 50ml of volumetric flasks and was diluted up to the mark with methanol.

 

PREPARATION OF CALIBRATION CURVE4,5,9-18

Different aliquots were taken from the 100µg/ml of Remogliflozin etabonate stock solution in separate 10ml volumetric flask and finally diluted with Methanol solution to prepare a series of concentration ranging from 2-10µg/ml as test solution. UV Spectra was taken at 200-400nm. Calibration curve was plotted taking concentration of drug on X-axis and amplitude on Y-axis. The overlain spectrum of Remogliflozin etabonate is shown in Fig. 2. Calibration curve of Remogliflozin etabonate is shown in Fig.3.

         

Figure 2: Overlain spectra of Remogliflozin etabonate

 

 

Figure 3: Calibration curve of Remogliflozin etabonate

 

ANALYSIS OF COMMERCIAL DOSAGE FORM9-18

Twenty tablets were weighed and powdered finely. A quantity of tablet powder equivalent to 10mg of Remogliflozin etabonate was accurately weighed and transferred to 10ml volumetric flask and sonicated for 10 min. The solution was further filtered by Whatman filter paper. The solution was further diluted with methanol to get required concentration. The amount of drug present in the sample solution was determined using the calibration curve of standard drug.

METHOD VALIDATION6

The developed method was validated for linearity, accuracy, precision, and repeatability, limit of detection and limit of quantification. To check the accuracy of the proposed method recovery studies were carried out by spiking 50%, 100% and 150% of test concentration. The Interday and intraday precision of the method was ascertained by taking three concentrations, three replicates within beer’s range and finding out the %RSD.

 

RESULT AND DISCUSSION:

A simple, precise and accurate spectrophotometric method has been developed for the estimation of Remogliflozin etabonate in API and its formulation. In this method the standard deviation of the slope and intercept were low. The correlation coefficient was 0.9990. The mean percent label claims estimated for the formulation was 98.86%, indicating the accuracy of the proposed method. The mean percent recovery was within the range of 98.94% - 99.86%. Thus it is concluded that the proposed method of analysis is new, simple, accurate and reproducible, successfully applied in the routine analysis of Remogliflozin etabonate in Tablet formulation.

 

CONCLUSION:

A new, simple and sensitive spectroscopic method was developed for the analysis of Remogliflozin etabonate in bulk and in its tablet dosage form. At 229nm Remogliflozin etabonate was analyzed and it was found that method was accurate, precise and reproducible and successfully applied to the pharmaceutical formulation as per ICH guideline.

 

Table 1.  Accuracy of Remogliflozin etabonate

% spiking

Tablet Concentration (µg)

Standard

Concentration (spiked) (µg)

% recovery

%RSD (n=3)

0

          4

0

99.86±0.20

0.1532

50

          4

2

99.56±0.12

0.1157

100

          4

4

99.53±0.16

0.1030

150

          4

6

98.94±0.30

0.2103

 

Table 2. Optical characteristic and validation parameter of Remogliflozin etabonate

Parameter

Value

Wavelength

229nm(maximum)

Linearity

2-10 µg/ml

Correlation coefficient

0.9990

Slope

0.001

Intercept

0.025

LOD

0.037µg/ml

LOQ

0.113µg/ml

Precision

Repeatability

0.158±0.030%

Interday(n=3)

0.050±0.001%

0.151±0.003%

0.254±0.004%

Intraday(n=3)

0.051±0.001%

0.157±0.003%

0.258±0.004%

Accuracy ( n=3)

0%

50%

100%

150%

 

99.86±1.10%

99.56±1.19%

99.53%±1.10%

98.94%±1.59%

 

Table 3. Analysis of Tablet dosage form (3 replicates)

Brand Name

Label claim

Amount estimated

Average

%

RSD

% recovered

Remozen

100mg

99.49

99.10

0.8237

99.10± 0.8237%

 

AKNOWLEDGEMENT:

The authors are thankful to K. B. Raval college of Pharmacy, Kasturinagar, Gandhinagar for providing the research facilities.

 

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Received on 12.05.2020            Modified on 15.06.2020

Accepted on 10.07.2020         © RJPT All right reserved

Research J. Pharm. and Tech. 2021; 14(4):2042-2044.

DOI: 10.52711/0974-360X.2021.00362