Simultaneous Determination of Aceclofenac and Rabeprazole sodium in Capsule Dosage Form by Spectrophotometry

 

R. S. Chaudhari*, B. N. Patel and C. N. Patel

Department of Pharmaceutical Chemistry, Shri Sarvajanik Pharmacy College, Mahesana-384001,Gujarat ,India

*Corresponding Author E-mail: ruchi.chaudhari@yahoo.co.in

 

ABSTRACT:

Two simple spectrophotometric methods have been developed for simultaneous estimation of Aceclofenac and Rabeprazole sodium from solid dosage form. Method I simultaneous equation method involves the measurement of absorbances at two wavelengths 277 nm (λmax of Aceclofenac) and 284 nm (λmax of Rabeprazole). Method II involves first derivative method in which absorbance is measured at two wavelengths 278 nm and 283 nm as zero crossing point for Aceclofenac and Rabeprazole sodium.  The method I and II were found linear between the range of 6-22 μg/mL for both the Aceclofenac and Rabeprazole sodium. The accuracy and precision were determined and validated statistically.Both the drugs obey Beer’s law in the concentration ranges employed for these methods. Both the methods showed good reproducibility and recovery with % RSD less than 2. The methods were found to be rapid, specific, precise and accurate and can be successfully applied for the routine analysis of Aceclofenac and Rabeprazole in bulk and combined dosage form.

 

KEYWORDS: Aceclofenac, Rabeprazole sodium, Simultaneous Equation method, First derivative method.

 

 


INTRODUCTION:

Aceclofenac (Fig. 1), {2, (2, 6 dichlorophenyl) amino phenyl acetic acid.}, is a phenyl acetic acid derivative with the improved gastric tolerance and is used for relief pain and inflammation in rheumatoid arthritis1.

Rabeprazole (Fig. 2), {2-([4-(3-methoxypropoxy)-3-methylpyridin-2-yl] methylsulfinyl) - 1H-benzo[d]imidazole} is a substituted benzimidazole that inhibits gastric acid secretion2. Rabeprazole neither exihibit anticholinergic nor histamine H-2 receptor antagonistic properties, but suppress gastric acid secretion by inhibiting gastric H+ K+ATPase at the secretory surface of the of the gastric parietal cell. Aceclofenac is reported for spectrophotometric3-5, RP-HPLC6-9 and simultaneous estimation with other combinations10. Similarly, Rabeprazole sodium also reported in combination with other drugs11-13. Since no spectrophotometric method is reported for simultaneous estimation of Aceclofenac and Rabeprazole sodium in combination therefore, in the present work, a successful attempt has been made to estimate both these drugs simultaneously by two simple UV spectrophotometric methods (simultaneous equation method and first derivative method).

 

The present paper describes a simple, accurate and precise method for simultaneous estimation of Aceclofenac and Rabeprazole in combined capsule dosage form.The proposed methods were optimized and validated as per the International Conference on Harmonization (ICH) analytical method validation guidelines 14-15.

 

MATERIALS AND METHODS:

Instrument used:

Instrument used is an UV-Visible double beam spectrophotometer, model 1700 (Shimadzu) with 1cm matched quartz cells.

 

Reagents and Solutions:

Working standards of Aceclofenac and Rabeprazole sodium were obtained as gift sample from Merril Pharmaceutical Ltd. Methanol was used as solvent. Combined dose capsule formulation was procured from local market.

 

EXPERIMENTAL:

Preparation of standard stock solution of Aceclofenac and Rabeprazole sodium:

The pure drugs accurately about 100 mg were weighed and dissolved in 100 mL methanol to give the standard stock solution of concentration 1000 µg/mL.

 

Preparation of test sample solutions:

To determine the content of Aceclofenac and Rabeprazole sodium in capsule (label claim: Aceclofenac:200mg/capsule and Rabeprazole:20mg/capsule),the contents of 20 capsule were weighed and their mean weight determined and finely powder.An equivalent weight of capsule content equivalent to 200 mg Aceclofenac  and 20 mg  Rabeprazole sodium transferred in to a 100-mL volumetric flask. Add 100 mL of diluent and sonicate it for 20 min. filter it through whattman filter paper. Further dilution was made to get the final concentration of Aceclofenac 20 µg/mL and Rabeprazole sodium    2 µg/mL.

 

Fig. 1: Chemical structure of Aceclofenac

 

Fig. 2: Chemical structure of Rabeprazole

 

Simultaneous equation method (Method–I):

From the stock solution of 1000 μg/mL, working standard solutions of drugs were prepared by appropriate dilution and were scanned in the range from 200-400 nm to determine λmax. Aceclofenac has λmax of 277 nm while Rabeprazole sodium has λmax at 284 nm respectively. Standard solutions were prepared having concentration of 6-22 μg/mL for both Aceclofenac and Rabeprazole sodium. The absorbances of theses standard solutions were measured at 277 nm and 284 nm for Aceclofenac and Rabeprazole sodium respectively and calibration curves were plotted. Both drugs followed the Beer’s-Lamberts law in the range of 6-22 µg/mL.

 

For estimation of drug form commercial formulation, the capsule sample solution prepared was diluted to concentration range of 20 µg/mL of Aceclofenac and 2 µg/mL of Rabeprazole sodium. Absorbance of  these solutions was measured at selected wavelengths of 277 nm for Aceclofenac and 284 nm for Rabeprazole sodium .The simple spectra of test sample was shown in figure 3.The overall studies of different parameters are represented in Table-1.

 

Fig. 3: Spectra of marketed formulation using simple UV spectroscopy

 

First order derivative method (Method- II):

The wavelengths selected for Aceclofenac and Rabeprazole sodium in first derivative mode in such a way that at one particular wavelength one drug shows some absorbance whereas the other one should show absorbance equivalent to zero. The working standards of both the drugs were scanned separately in the 200-400 nm in D1 mode and the wavelengths selected were 278 nm and 283 nm for aceclofenac and Rabeprazole sodium respectively. Standard solutions were prepared having concentration of 6-22 μg/mL for both Aceclofenac and Rabeprazole sodium. The absorbances of theses standard solutions were measured at 278 and 283 nm and  D1 values calibration curves for both the drugs were plotted separately.

 

For estimation of drug from commercial formulation, the capsule sample solution prepared was diluted to concentration range of 20µg/mL of Aceclofenac and 2µg/mL Rabeprazole sodium. Dof these solutions was measured at selected wavelengths of 278 nm and 283 nm for Aceclofenac and Rabeprazole sodium respectively.The derivative spectra of test sample was shown in figure 4


 

Table 1. Summary of Validation Parameter

Parameters

Simultaneous equation method

First order derivative method

 

Aceclofenac

Rabeprazole

Aceclofenac

Rabeprazole

Linearity range (µg/mL)

6-22

6-22

6-22

6-22

Correlation-coefficient

0.9999

0.9989

0.9998

0.9991

Regression equation

y=0.032x +0.030

y = 0.046x-0.041

y =0.0023x-0.0003

y =0.0042x-0.0034

Intercept

0.030

-0.041

-0.0034

-0.0003

Slope

0.032

0.046

0.0042

0.0023

Precision(%RSD)

Intraday precision

Interday precision

 

0.4 - 0.6

0.26 - 0.4

 

1.01 - 1.1

0.93 -1.06

 

0.62 - 1.02

0.1- 0.8

 

0.8 - 1.14

0.3 - 0.7

% Mean Recovery

99.64 - 101.2

100.8% - 101.2 %

99.9 - 100.2

100.5 -100.6

Limit of Detection  (µg/mL)

0.67

0.8

0.5

0.7

Limit of Quantification  (µg/mL)

0.9

1.04

1.2

1.6

Table 2 Estimation of Aceclofenac and Rabeprazole in capsule dosage form by proposed methods.

Drug name

Label claim

(mg/tablet)

Simultaneous equation method

First order derivative spectroscopy

Amount found (mg/tablet)

Mean± S.D (n=3)

% Assay Mean ± S.D (n=3)

Amount found (mg/tablet)

Mean± S.D (n=3)

% Assay Mean ± S.D (n=3)

Aceclofenac

200

198.3±0.16

99.15±0.055

201±0.23

100.5±0.36

Rabeprazole

20

20.3±0.19

101.5±0.22

20.2±0.28

101±0.39

 

 

Table 3 Results for Recovery Studies

Recovery level

Simultaneous equation method

First order derivative spectroscopy

Amount of drug added (µg/mL)

%RSD Recovery*

Amount of drug added (µg/mL)

%RSD Recovery*

 

Aceclofenac

Rabeprazole

Aceclofenac

Rabeprazole

Aceclofenac

Rabeprazole

Aceclofenac

Rabeprazole

50%

5

2

99.64±0.2

101.2±0.2

5

2

99.9±0.4

100.5±0.2

100%

10

4

101.2±0.11

100.8±0.06

10

4

100±0.21

100.6±0.15

150%

15

6

99.98±0.11

100.9±0.9

15

6

100.2±0.28

100.53±0.1

*RSD for Six Determinations

 

 


Precision:

Precision was checked out by performing interday variation and intraday variation studies. In interday variation the absorbance for standard solution was measured on three consecutive days. In intraday variation the absorbances were measured three times in a day. The results were satisfactory and presented in Table 1.

 

Recovery study:

To study the accuracy of the proposed methods, recovery studies were carried out by standard addition method at three different levels. A known amount of drug was added to preanalyzed tablet powder and percentage recoveries were calculated. The results of recovery studies were satisfactory and are presented in Table-3.

 

Fig. 4: Spectra of marketed formulation using 1st derivative spectroscopy

 

RESULT AND DISCUSSION:

For both the two methods linearity was observed in the concentration range of 6-22 μg/mL for Aceclofenac and Rabeprazole sodium. Marketed brand in capsule was analyzed and amount of drug determined by proposed methods ranges from 99.15 to 101.5% as shown in Table 2. The proposed methods were validated as per ICH guideline. The accuracy of method was determined at 50, 100 and 150 % level. The % recovery ranges from 99.64 to 101.2 for both the two methods. Precision was calculated as interlay and intraday variations (%RSD is less than 2) for both drugs. The proposed methods were found to be simple, accurate and rapid for the routine determination of Aceclofenac and Rabeprazole sodium  in capsule formulation. The two methods can be successfully used for simultaneous estimation of Aceclofenac and Rabeprazole sodium.

 

CONCLUSION:

The results of the study showed that the proposed UV Spectrophotometric method are simple, rapid, precise, accurate, specific and sensitive for determination of Aceclofenac and Rabeprazole sodium without any interference from excipients. Hence, this method is suitable for analysis of Aceclofenac and Rabeprazole sodium in bulk and its capsule dosage form.

 

ACKNOWLEDGEMENTS:

The authors are grateful to, The Principal and the Management, Shri Sarvajanik Pharmacy College, Mahesana, for providing the required facilities for providing the gift sample for the research work.

 

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Received on 19.04.2011       Modified on 02.05.2011

Accepted on 17.05.2011      © RJPT All right reserved

Research J. Pharm. and Tech. 4(8): August 2011; Page 1256-1259