Submitted To: Dr. Ayesha Mohy-ud-dinSubmitted 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

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

INTRODUCTIONDiclofenac SodiumDiclofenac 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

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

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

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

MATERIALS AND METHODSComparison of different parameters which is taken in the

comparative study of different three papers.

METHOD OF PAPER 1 Preparations of Standard stock solutions

100 ml

METHOD OF PAPER 1Preparation of Working Standard SolutionsConcentration 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.

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

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

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

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

METHOD VALIDATIONDifferent Parameters

System suitability, Calibration of Pump, Injector, Detector and

Column as well as depends on analyst, method, and preparation of

sample.

RESULTS AND DISCUSSIONMethod 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)

RESULTS AND DISCUSSIONMethod development of Paper 1, Paper 2 and Paper 3

(b) (c)

RESULTS AND DISCUSSIONTotal 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.

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.

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.

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hakeel Khan, Im

ran Ali (U

MT)

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