This document presents a comparative study of three research papers on RP-HPLC method development and validation for the estimation of diclofenac sodium from tablet dosage forms. The objective is to determine the most effective and cost-efficient method. The materials and methods from each paper are compared based on preparation of standard and sample solutions, run time, and validation parameters. The results show that Paper 1 has the fastest run time of 10 minutes and is more accurate, precise, sensitive and cost-effective than Papers 2 and 3. Paper 1 uses a more optimal column dimension. In conclusion, the RP-HPLC method from Paper 1 is deemed superior for the quantitative analysis of diclofenac sodium in tablet dosage forms.

1. Submitted To:
Dr. Ayesha Mohy-ud-din
Submitted By:
Shakeel Ahmad Khan (14003140007)
Programme: MS (Chemistry)
Department of Chemistry, University of Management and Technology
Lahore
Comparative study of RP-HPLC Method Development
and Validation for the Estimation of Diclofenac Sodium
from their tablet dosage form

2. LIST OF CONTENTS
 Introduction
 Diclofenac Sodium
 Objective of this Study
 Materials and methods
 Results and discussion
 Conclusion
 References

3. INTRODUCTION
Diclofenac Sodium
Diclofenac is chemically named as 2-(2-(2, 6-dichlorophenylamino)
phenyl) acetic acid.
Non-steroidal anti-inflammatory drugs (NSAIDs).
Figure 1: Chemical structure and commercially available
Diclofenac Sodium

4. Diclofenac Sodium
 Recommended dose for most conditions is 100-200 mg daily.
 Diclofenac sodium acts by potent cyclooxygenase inhibition, reduction
of arachidonic acid release, and enhancement of arachidonic acid
uptake.
Diclofenac (DIC) tablets can cause side effects

5. LITERATURE SURVEY
 Literature survey reveals that diclofenac sodium is estimated
individually or in combination with other drugs in the formulations by
UV Spectrophotometer, HPTLC, Atomic absorption
spectroscophotometer, Capillary electrophoresis, HPLC

6. OBJECTIVE OF THIS STUDY
 In this present work, an attempt of comparative study of three
research paper was made.
 To see that which method and formulation is best for the development
of a sample in that three research paper with cost effectiveness.
 To develop a simple economic, feasible and sensitive reverse-phase
high-performance liquid chromatographic method for the quantitative
determination of diclofenac sodium in suppositories and to validate
the proposed method as per ICH guidelines

8. MATERIALS AND METHODS
Comparison of different parameters which is taken in the
comparative study of different three papers.

9. METHOD OF PAPER 1
 Preparations of Standard stock solutions
100 ml

10. METHOD OF PAPER 1
Preparation of Working Standard Solutions
Concentration of stock-A solution in 10 ml volumetric flask
0.25ml 0.5ml 1.0ml 1.25ml 1.5ml 2.5ml
volume is make up 10ml with diluents
Solution strengths
Solutions of 12.5µg/ml, 25µg/ml, 50µg/ml, 62.5µg/ml, 75µg/ml and
125µg/ml respectively for Diclofenac obtained.

11. METHOD OF PAPER 1
 Preparations of Sample solutions
20 tablets
(e) From filtrate, 1 ml was pipetted and transferred into 10ml volumetric
flask and the solution was made up to the volume with diluent.
sonicated for 20 min

12. METHOD OF PAPER 2
 Preparations of Standard solutions
20mg
(e) collected the solution in an HPLC vial after discarded first 2
ml of filtrate (0.2 mg/ml of diclofenac sodium).
sonicated for 5 minute100 ml Flask

13. METHOD OF PAPER 2
 Preparations of Sample solutions
05 tablet
(e) collected the solution in an HPLC vial after discarded first 2
ml of filtrate (0.2 mg/ml of diclofenac sodium).
sonicated for 10 minute100 ml Flask

14. METHOD OF PAPER 3
 Preparations of Sample solutions
100 mg
(d) The flask was shaken and volume was made up to the mark with
methanol to give solutions containing 1000 μg/ml diclofenac sodium.
sonicated for 10 minute
50 ml methanol
100 ml Flask

15. METHOD VALIDATION
Different Parameters
 System suitability, Calibration of Pump, Injector, Detector and
Column as well as depends on analyst, method, and preparation of
sample.

17. RESULTS AND DISCUSSION
Method development of Paper 1, Paper 2 and Paper 3
 These are the following representative chromatogram (a), (b) and (c)
of Diclofenac for method development of determination according to
paper 1 paper 2 and paper 3 respectively.
(a)

18. RESULTS AND DISCUSSION
Method development of Paper 1, Paper 2 and Paper 3
(b) (c)

19. RESULTS AND DISCUSSION
Total run time
 The total run time required for the method 1 is only 10 minutes for
eluting Diclofenac so, this method is fast.
 The total run time required for the method 2 is 15 minutes for eluting
Diclofenac.
 The total run time required for the method is 20 minutes for eluting
Diclofenac.

20. CONCLUSION
 Paper 1 for the determination of Diclofenac quantitatively is better as
compared to other two methods that describe in paper 2 and paper 3.
The main reason of the superiority of method 1 of paper 1 as compared
to other two methods are
 On the basis of total run time.
 Method 1 of paper 1 is fast, accurate, precise and sensitive.
 Method 1 of paper 1 is cost effective as compared to method 2 and 3.
 One more important thing which makes the superiority of method 1 of
paper 1 is the column dimension.

21. REFERENCES
 Vemula V., R., B., and Sharma P., K., 2003. RP-HPLC
Method development and validation for simultaneous
estimation of diclofenac and tolperisone in tablet dosage
form. Asian journal of pharmaceutical and clinical research,
6(3), 186-189.
 Sivakumar N., Chenthilnathan A. and Vairamani A., 2014.
Development and validation of RP-HPLC method for the
quantitative determination of diclofenac sodium in
pharmaceutical dosage form. International journal of
pharmaceutical research and biomedical analysis, 3(2), 20-
30.
 Patel J. and Patel P. 2014. RP-HPLC method development
and validation for the estimation of diclofenac sodium,
tramadol hydrochloride and chlorzoxazone from their
combined tablet dosage form. International journal of
pharmacy and pharmaceutical sciences, 6(7), 632-637.

22. 01/16/16ShakeelKhan,ImranAli(UMT)
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