You are hereANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF IRBESARTAN BY DERIVATIVE SPECTROSCOPY (FIRST ORDER)

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF IRBESARTAN BY DERIVATIVE SPECTROSCOPY (FIRST ORDER)


Materials and Methods

Drug
The standard sample of IBRESARTAN was obtained as gift sample from Dr. Reddy’s Laboratory Pvt. Ltd., Hyderabad, A.P., India. The irbesartan tablets were procured from local market.

Instrument specifications
UV Spectrophotometer, Shimadzu, model 1800.

Chemicals and reagents used
Ethanol obtained from local market, manufactured by Merck Pharmaceuticals.

Preparation of stock solution
The stock solution of candesartan is prepared by dissolving 100 mg of drug in 100 ml methanol in volumetric flask with continuous shaking; 0.08 ml of sample was withdrawn and diluted to 10 ml methanol to get 8 μg/ml of solution. The solution was than scanned in UV range between 200-400 nm UV-VIS Spectrophotometer, Shimadzu, Japan to determine the absorption maxima of the drug against blank as methanol.

Wavelength scanning and determination of absorption maximum
From the stock solution of Irbesartan, known concentration of 8μg/ml is prepared by suitable dilution with 50 % aqueous ethanol. Wavelength scanned for the maximum absorption of drug solution using UV-Visible spectrophotometer within the wavelength region of 200–400 nm against blank solvent. Convert the normal mode obtained spectra to first order derivative. The wavelength that shows the peak with a highest absorbance is considered as absorbance maximum of the drug. The result is presented in fig. 2.


Fig. 2: Wavelength scanning and determination of absorption maximum

Linearity studies
Stock solution was subsequently diluted with methanol to get 4μg/ml, 6μg/ml, 8μg/ml, 10μg/ml, 12μg/ml 14μg/ml, 16μg/ml, 18μg/ml 20μg/ml, 22μg/ml 24μg/ml. Convert the normal mode obtained spectra to first order derivative using software UV probe 2.34. The results are tabulated and the linearity curve was constructed by plotting concentration Vs. D1 value. The result is presented in table 1 and fig. 3.

Fig. 3: standard graph of Irbesartan

Regression equation; y = 0.001x + 0.0012
R2 = 1
X – Axis: Concentration
Y- Axis: D1 value

Precision
The precision of method was ascertained; the percent relative standard deviation were calculated and presented.

Inter day and intraday studies for Irbesartan analytical method
The prepared stock solution was subsequently diluted to get 14 μg/ml. The resulting solution absorbance was measured at detection wavelength of 237 nm using double beam UV spectrophotometer against blank solvent. The findings was made at different time intervals in day times in a day and performed continuously for six days. Convert the normal mode obtained spectra to second order derivative. The results obtained were tabulated and studied for inter day and intraday variation. The results are tabulated in table 2(a) and 2(b).

Accuracy studies
The accuracy/recovery studies were carried out by adding a known amount of drug from the pre-analyzed tablet powder and percentage recoveries were calculated. Convert the normal mode obtained spectra to first order derivative. The reproducibility of estimation was determined by performing the tablet drug content of different samples. The results of accuracy studies were expressed in %. The result is presented in table 3.

Assay studies
The assay studies were carried out with the help of candesartan SMEDDS. The percentage purity was calculated. Convert the normal mode obtained spectra to first order derivative. The reproducibility of estimation was determined by performing the drug content of different samples. The results of assay studies were expressed in %. The result is presented in table 4.

Results and Discussion
Irbesartan is a novel, potent, highly selective non peptide Angiotensin II type 1 (AT1) receptor blocker which is administered orally. It is rapidly and completely hydrolyzed to the active moiety, during absorption from the gastrointestinal tract. The physico-chemical characteristic study of Irbesartan like melting point is 180°C nearer to the literature value 182°C in previous literature. The literature survey ascertains that HPLC analytical method is developed for Irbesartan, which is cost effective. In our laboratory we developed first order derivative spectroscopic method for the analysis of irbesartan. The known concentration of irbesartan is prepared and scanned for absorption maximum. The detection wavelength according to spectra is 237 nm. Different measured D1 values at detection wavelength 237.0 nm is plotted as the curve as D1 value versus concentration. Irbesartan obeys the beer’s law in the concentration range 8-18 μg/ml. Linearity study indicates the curve is linear in the range of 8 to 18 μg/ml. The linear regression equation is Y = 0.001x +0.012 with regression coefficient, R2= 1. The developed method is validated for repeatability, reproducible and the accuracy and precision. In the inter day and intraday study of standard graph, the % RSD is less than 2% indicating the developed method is reproducible. The different levels of standard concentration solutions are measured for D1 value and actual concentration is calculated. The results showed that the amount recovered is 100% indicating the first order derivative spectroscopic method is accurate and precise.

TABLE 1: Linearity of Irbesartan

S.NO.

CONCENTRATION (µg/ml)

D1 VALUE AT DETECTION WAVELENGTH  (237 nm)

1

8

0.012

2

10

0.015

3

12

0.018

4

14

0.021

5

16

0.024

6

18

0.027

TABLE 2 (a) intraday precision

S.NO

CONCENTRATION (µg/ml)

D1 VALUE AT DETECTION WAVELENGTH  (237 nm)



TIME (MINS)

I

II

III

MEAN

1

14

0 min.

0.020

0.020

0.020

0.020

2

14

15 min

0.020

0.020

0.021

0.02033

3

14

30 min

0.020

0.020

0.021

0.02033

4

14

60 min

0.020

0.021

0.020

0.02033

5

14

120 min

0.021

0.020

0.020

0.02033

6

14

180 min

0.021

0.021

0.021

0.021

7

14

240 min

0.020

0.020

0.020

0.020

  Mean =

0.020

    SD =

0.000333

     % RSD =

1.66

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