DIFFERENCE SPECTROPHOTOMETRIC ESTIMATION OF CAPECITABINE FROM TABLET DOSAGE FORM

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Recovery studies:
Accuracy and sensitivity of analysis was determined by performing recovery studies by spiking different concentrations of pure drug in the preanalyzed tablet sample. Results of recovery studies indicated that the method is rapid, accurate and reproducible. The recovery obtained after replicate determinations (n=5) is shown in Table No.4

Table No.4: Results of Recovery Study:

Analyte

Label claim

(mg)

%Label claim estimated*

(Mean ± S. D.)

R.S.D.

CAP

500

99.22 ± 1.0792

1.09

* Average of nine determinations; S.D.: standard deviation

Method validation:
The proposed method was validated according to ICHQ1A (R2)guidelines for validation of analytical procedures in order to determine accuracy, precision, repeatability, robustness, linearity, range, sensitivity, limit of detection and quantitation17.and results are shown in Table No. 5 to 10.

Table No.5: Results of Repeatability:

Analyte

Label claim

(mg)

Tablet Analysis %Label claim estimated*

(Mean ± S.D.)

R.S.D.

CAP

500

100.56 ± 0.6482

0.6521

* Average of nine determinations; S.D.: standard deviation. R.S.D.: relative standard deviation.

Table No.6: Results of Intraday Precision:


% Label claim estimated* (Mean ± S.D.)

R.S.D.

CAP

CAP

T-1

100.12±1.2864

1.2938

T-2

100.31±1.3159

1.3686

T-3

100.56±1.2372

1.2561

*Average of nine determinations; S.D: standard deviation. R.S.D.: relative standard deviation.

Table No.7: Results of Interday Precision:

Day

% Label claim estimated*

(Mean ± S.D.)

R.S.D.

CAP

CAP

Day -1

100.36±1.2435

1.2542

Day -2

100.50±1.2918

1.2958

Day -3

100.18±0.9628

0.9565

* Average of nine determinations; R.S.D., Relative Standard Deviation.

Table No.8 Limit of Detection and Limit of Quantitation:

Name of Drug

LOD μg/ml

LOQμg/ml

CAP

0.037

0.072

* Average of six determinations; R.S.D., relative Standard Deviation.

Table No.9: Results of robustness (using methanol solution):

Analyte

Label

claim(mg)

Tablet Analysis% Label claim estimated*(Mean ± S.D.)

R.S.D.

CAP

150

99.341.1490

1.29

* Average of nine determinations; R.S.D., relative Standard Deviation.

Table No.10: Optical characteristics:

Parameters

Values for CAP

Beer’s law limit (μg/ml)

1-20

Correlation coefficient

0.998

Regression equation(y*)


Slope (B)

0.0353

Intercept (A)

0.0357

Y= A + B*C, where C is the concentration in µg/ml and Y is absorbance unit

RESULT AND DISCUSSION:
The proposed method for simultaneous estimation of CAP utilizes the spectrum mode of analysis of Shimadzu UV1601 spectrophotometer. CAP exhibits a substantial difference in absorbance in the two solvents that is in 0.01 N HCL and 0.01 N NAOH at 295 nm so determination of CAP by difference spectroscopic method was thus attempted. Beer’s law was obeyedin the concentration range of 1 -20 µg ml -1for CAP. Interlay and intradaystudies showed high degree of repeatability of an analytical method under normal operating conditions. Results of tablet analysis showed standard deviation in the range of 98.42 to 101.95 % for CAP which indicate repeatability of the method. The accuracy of the method was determined by investigating the recovery of the drugs using spiked concentrations of the standard drug.

The results indicated excellent recoveries ranging from 98.45 to 101.70 % for CAP with a mean of 99.12 %.

Recoveries obtained do not differ significantly from 100% showed that there was no interference from the common excipients used in the tablet formulation indicating accuracy and reliability of the method. Precision for tablet analysis was determined by analysis of tablets containing CAP.  Lower limit of detection for CAP was found to be 0.037 µg ml -1 Limit of quantitation was found to be 0.072 µg ml -1

CONCLUSION:
The proposed method for different spectrophotometric estimation of CAP was found to be simple, accurate and reproducible for routine estimation of CAP in tablet formulation. The recoveries obtained 98.45 to 101.70 % for drug which do not differ significantly from 100 %. There were no interferences from common excipients used in the formulation indicating accuracy and reliability of the method. Recoveries obtained do not differ significantly from 100% showed that there was no interference from the common excipients used in the tablet formulation indicating accuracy and reliability of the method.

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