formulation and characterizatin of transdermal patches by using ...

Bismi P. Cheriyan et al. / International Journal of Advances in Pharmaceutical Research 

IJAPR 

Available Online through 

www.ijapronline.org 

Research Paper 

ISSN: 2230 – 7583 

FORMULATION, DEVELOPMENT & EVALUATION OF DICLOFENAC SODIUM 

TABLETS BY USING STARCH PHOSPHATE TO IMPROVE THE SOLUBILITY 

Bismi P. Cheriyan * , Tarkeshwar Prasad Shukla, Govind Mohan, Shailesh Sharma, Manmohan Kaushik. 

Department of pharmaceutics; NIMS University, Jaipur 

Received on 10 – 07 - 2012 Revised on 17 – 08- 2012 Accepted on 20– 09 – 2012 

ABSTRACT 

The objective of the study is to prepare, characterize & evaluate starch phosphate, a new modified starch as a 

carrier in solid dispersion for enhancing the dissolution rate of diclofenac sodium. Diclofenac sodium is among 

most extensively used NSAIDs: employed in rheumatoid arthritis & osteoarthritis, affords quick relief of pain & 

wound edema. Starch phosphate prepared by reacting potato starch with di-sodium hydrogen orthophosphate 

anhydrous at elevated temperatures was found to be a white, crystalline, non-hygroscopic powder. As starch 

phosphate exhibited good swelling in water, it is considered as a promising disintegrant in tablet formulations. It 

was insoluble in water and has good swelling (400%) property without pasting or gelling when heated in water. 

Solid dispersion of diclofenac sodium in starch phosphate were prepared by solvent evaporation method employing 

various weight ratio of drug : starch phosphate such as 1:1(F1),2:1(F2),1:2(F3),1:3(F4) & were evaluated for 

dissolution rate. Diclofenac sodium (250 mg) tablets were prepared employing diclofenac sodium alone & its solid 

dispersions F1, F2, F3 & F4 by wet granulation method & were evaluated. All the solid dispersion prepared gave 

rapid & higher dissolution of diclofenac sodium when compared to pure drug. 

Keywords: diclofenac sodium, starch phosphate, solid dispersion, dissolution rate. 

INTRODUCTION 

The solid dispersion technique to improve the 

dissolution characteristics of poorly water - soluble 

drugs by the use of water-soluble carriers [1] . Many 

water –soluble carriers polyethylene glycols, 

polyvinyl pyrrolidone [2,3] . According to literature 

review, the starch phosphate is used as carrier in 

solid-dispersion technique to improve the solubility 

of the drug. It is also used as disintegrating agent. No 

reports are available on its use as pharmaceutical 

excipient. The objective of the present study is to 

prepare, characterize and evaluate starch phosphate 

as a carrier in solid dispersions for enhancing the 

dissolution rate of diclofenac sodium. 

Corresponding Author 

Ms. Bismi P. Cheriyan 

Department of pharmaceutics 

NIMS University, Shobha Nagar 

Jaipur, Rajasthan (303121) 

bismipcherian25@gmail.com 

91-8290814579 

MATERIALS & METHODS 

Diclofenac sodium, starch phosphate is prepared in 

the laboratory, dichloromethane, potato starch, 

lactose, acacia, talc, magnesium stearate. 

[4, 5, 6] 

Preparation of starch phosphate 

Starch phosphate was prepared based on the method 

of Choi et al with some modifications. Potato starch 

(100 g) and di-sodium hydrogen orthophosphate 

anhydrous (30 g) were suspended in 100 ml of water 

and continuously stirred for 20 min. This starch 

slurry was then filtered and the wet starch mixture 

was conditioned for 12 h at room temperature 

(280C). To enhance phosphorylation, this mixture 

was heated in a forced air oven at 130°C for 3 h. The 

product obtained was ground and sized. 

IJAPR / Oct. 2012/ Vol. 3 /Issue. 10 / 1188 – 1192 1188


8. Particle size: Particle size analysis was 

done by sieving using standard sieves. 

Figure no: 1 reaction on starch & 

disodium hydrogen O-phosphate 

[7, 8, 

EVALUATION OF STARCH PHOSPHATE 9] : 

Characterization of Starch Phosphate 

The starch phosphate prepared was evaluated for 

following 

1. Solubility: 

Solubility of starch phosphate was tested in water, 

aqueous buffers of pH 1.2, 4.5, and 7.4 and organic 

solvents such as alcohol, dichloromethane, 

chloroform, acetone and petroleum ether. 

2. pH: 

The pH of 1% w/v slurry was measured. 

3. Melting Point: 

Melting point was determined 

by using melting point apparatus. 

4. Viscosity: 

Viscosity of 1% dispersion in 

water was measured using Ostwald Viscometer. 

5. Swelling Index: 

Starch phosphate (200 mg) 

was added to 10 ml of water and light liquid paraffin 

taken in two different graduated test tubes and 

mixed. The dispersion in the tubes was allowed to 

stand for 12h. The volumes of the sediment in the 

tubes were recorded. The swelling index of the 

material was calculated as follows. 

water – Volume 

paraffin ×100 

S.I (%) = 

light liqiud Paraffin 

Volume of sediment in 

of sediment in light liquid 

Volume of sediment in 

6. Test for gelling property 

The gelling 

property (gelatinization) of the starch and starch 

phosphate prepared was evaluated by heating a 7% 

w/v dispersion of each in water at 100°C for 30 min. 

7. Moisture absorption 

The hygroscopic nature 

of starch phosphate was evaluated by moisture 

absorption studies in a closed desiccator at 84% 

relative humidity and room temperature. 

9. Density: Density (g/cc) was determined by 

liquid displacement method using benzene 

as liquid. 

10. Bulk density: 

Bulk density (g/cc) was 

determined by three tap method in a graduated 

cylinder. 

11. Angle of repose: 

Angle of repose was 

measured by fixed funnel method. 

12. Compressibility index: 

Compressibility 

index (CI) was determined by measuring the initial 

volume (Vo) and final volume (V) after hundred 

tapping of a sample of starch phosphate in a 

measuring cylinder. CI was calculated using 

equation. 

Compressibility index (CI) = Vo – V × 100 

Vo 

Caliberation Curve 

100 mg of diclofenac sodium was taken in a conical 

flask & dissolve in 100ml of pH 6.8 phosphate 

buffer.10 ml of solution was pipette out from above 

solution & diluted up to 100 ml with pH 6.8 

phosphate buffer. Now pipette out 1, 2, 3, 4, & 5ml 

solution from above solution & dilute up to 10 ml 

with pH 6.8 phosphate buffer. Measure the 

absorbance at 283nm by using UV visible 

spectrophotometer & plot the graph of concentration 

(µg/ml) versus absorbance. 

Table No1: Calibration curve 

CONCENTRATION ABSORBANCE 

0 0 

10 0.367 

20 0.595 

30 1.203 

40 1.502 

50 1.900 

Preparation Of Solid Dispersion Of Diclofenac 

Sodium In Starch Phosphate [10, 11, 12] : 

Diclofenac sodium was dissolved in 

dichloromethane (10ml) in a dry mortar to get a clear 

solution. Starch phosphate was then added and 



mixed. The thick slurry was kneaded for 15 min. for 

complete evaporation of dichloromethane and then 

dried at 55°C until dry. The dried mass was 

pulverized and sieved through mesh no. 100. 

Preparation Of Diclofenac Sodium –Sd [13, 14, 15] : 

Compressed tablets each containing 50mg of 

diclofenac sodium were prepared by wet granulation 

method employing diclofenac sodium alone & its 

solid dispersion in starch phosphate in the ratio of 

drug : starch phosphate (1:1), (1:2), (1:3), (2:1). 

Lactose was used as diluents to adjust weight to 

250mg. acacia 2%, talc 2% & magnesium stearate 

2% were incorporated respectively as binder & 

lubricants. 

Table no:2 description of trial taken 

INGREDIEN 

TS 

DICLOFEN 

AC 

SODIUM 

STARCH 

PHOSPHAT 

E 

F1( 

1:1 

) 

5O 

mg 

50 

mg 

DICHLORO 10 

METHANE ml 

LACTOSE 137 

mg 

ACACIA 4.4 

mg 

MAGNESIU 4.4 

M 

mg 

STEARATE 

TALC 4.4 

mg 

F2(2: 

1) 

50mg 

F3(1 

:2) 

50m 

g 

25mg 100 

mg 

10ml 

162m 

g 

4.4m 

g 

4.4m 

g 

10m 

l 

87m 

g 

4.4 

mg 

4.4 

mg 

F4(1 

:3) 

50m 

g 

150 

mg 

10m 

l 

37m 

g 

4.4 

mg 

4.4 

mg 

F5 

50 

mg 

- 

- 

187 

mg 

4.4 

mg 

4.4 

mg 

4.4m 4.4 4.4 4.4 

g mg mg mg 

WATER q.s q.s q.s q.s q.s 

Disintegration test 

To test for disintegration time, one tablet is placed in 

each tube and the basket rack is positioned in a 1 

litre beaker of water at 37°C+2°C. A standard motor 

driven device is used to move the basket assembly 

up and down through a distance of 5 to 6 cm at a 

frequency of 28 to 32 cycles per minute. When all 

six tablets have disintegrated, time is noted. 

F: IN-VITRO Dissolution test 

Dissolution rate was studied by using USP type II 

apparatus rotated at 75 rpm, 900 ml of phosphate 

medium. Temperature of dissolution medium was 

maintained at 37± 0.5 0 C. Aliquot of dissolution 

medium was withdrawn at specific time interval and 

it was filtered. Absorption of filtered solution was 

checked out by UV spectroscopy at 283 nm & drug 

content was determined from standard curve, 

dissolution rate was studied for all designed 

formulation . 

RESULTS 

Evaluation of starch phosphate 

The starch phosphate was characterized on 

the basis of solubility, pH, melting point, 

viscosity, swelling index, angle of repose, bulk 

density, tapped density. 

Table No:3 Characterization of starch phosphate 

Sr.No. Property Result 

1. Solubility Insoluble in all 

aqueous and 

organic solvents 

tested 

2. PH (1% w/v aqueous 7.25 

dispersion) 

3. Melting Point Charred at 

210 o C 

4. Viscosity (1% w/v 

aqueous dispersion) 

2.11 cps 

5. Swelling Index 400 

6. Gelling Property No gelling and 

the swollen 

particles of 

starch phosphate 

separated from 

water. Whereas 

in the case of 

starch, it was 

gelatinized and 

formed gel. 

7. Moisture Absorption < 4.0 % 

8. Particle Size 152 μm (80/120 

mesh) 

9. Density 1.667 g/cc 

10. Bulk Density 0.534 g/cc 

11. Angle of Repose 20.040 

12. Compressibility Index 11.01 % 



Figure no: 2 caliberation curve 

ratio. Among all the batches F10 shows high % drug 

release because F10 contain high amount of starch 

phosphate..According to all parameter of evaluation, 

batch F4 was optimized one, because it shows high 

% drug release when compared to other batch within 

30 min. & all other parameter was also found to be 

optimum for F4. 

ACKNOWLEDGMENT 

Authors are grateful and thankful to Dr. Balvir S 

Tomar, Chancellor & Dr. K.C. Singhal, Vice 

Chancellor NIMS University, Jaipur for providing 

necessary facility. 

Table No: 4 disintegration time 

formulation Disintegration 

time (sec.) 

F1 82 

F2 70 

F3 59 

F4 52 

F5 102 

Table no: 5 dissolution profile 

TIME F1 F2 F3 F4 F5 

(MIN) 

0 0 0 0 0 0 

5 25.6 28.8 38.5 43.8 22.2 

10 40.9 44.5 62.3 66.7 35.1 

15 62.3 65.8 77.5 87.5 55.1 

20 73.2 76.7 85.1 94.5 69.9 

25 78.9 82.5 91.4 97.5 74.5 

30 90.8 91.4 94.5 98.2 87.4 

DISCUSSION 

The present work was carried out to formulate and to 

improve the solubility of diclofenac sodium by using 

starch phosphate. The flow property of starch 

phosphate was found to be good. The flow property 

depends upon the angle of repose & compressibility 

index & the value was found to be 20.04 0 & 11.01% 

respectively. 

The dissolution of all batches F1-F4 was compared 

with F5. F5 does not contain starch phosphate & all 

other batches contain starch phosphate in different 

REFERENCES 

1. Sekiguchi, & Obi, ‘Studies on absorption of 

eutectic mixture’, Chemical Pharm. 

Bulletin, 1961,vol. 9, 866-872. 

2. Hirasawa, N., Ishise, S. & Miyata H., ‘An 

attempt to stabilize Nivaldipine solid 

dispersion by the use of ternary systems’. 

Drug Development and Industrial 

Pharmacy, 2003,vol. 29, 997-1004. 

3. Rawat, S. & Jain, S., ‘Rofecoxib-betacyclodextrin 

inclusion complex for 

solubility enhancement’, Pharmazie,2003, 

vol. 58, 639-641. 

4. Chowdary K.P.R.,Entury V.,Pallavi T.V., 

“Formulation development of etoricoxib 

tablets by wet granulation & direct 

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6. Vaghela B.J,Kayastha R.R., Bhatt 

N.M.,Pathak et al “Formulation & 

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diclofenac sodium”, Int.J.Pharm Res & 

Dev,2011,3(6), 17-22. 

7. Chowdary k.P.R, Entury V.,Rani 

A.S.,“Preparation and evaluation of starch 

phosphate- A new modified starch as a 

disintegrant in tablet formulation” 

Int.J.Chem.Sci,2011,9(2),889-899. 

8. Pandey V.P.,Reddy K.V.,Amarnath R. 

“Studies on diluents for formulation of 

tablets”Int.J.Chem.Sci,2009,7(4),2273- 

2277. 

9. Prashanthi N.L., Manikiran S.S., Rao N.R., 

“Invitro drug release studies of ziprasidone 

from tablets using natural gums from 



biosphere”, 

Arch.Appl.Sci.Res,2011,3(2),513-519. 

10. Meiczingen M., Dences J., Marton G., & 

Dences B. “Investigation of research 

occurring at starch phosphorylation, 

American chem. society-2005. 

11. Kumar S. & chowdary K.P.R., 

“Formulation development of selected 

antiretroviral drugs by direct compression 

method”, Int.J.Pharmacy Sci,2012, 4(2), 

185-188. 

12. Chowdary K.P.R., Enturi V., “Enhancement 

of dissolution rate &formulation 

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starch citrate-A new modified starch”, J. 

Appl. Pharm Sci, 2011,1(5),119-123. 

13. Chowdary K.P.R., Chandra D.U., Parimala 

V.,Indira M., “A factorial study on 

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Int. J. Pharma Sci Res,2012, 3(1),189-193. 

14. Jubril I.,Muazu J. & Moahmmaed G.T. 

“Effect of phosphate modified & 

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formulations”,J. App. Pharm. Sci.,2012, 

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INTERNATIONAL CONGRESS IN PHARMACY AND HEALTH SCIENCES 

Pharma Science Tech Association, Foundation No: AP/PSTA/56/2012. 

Please visit for Details: www.icphsmembership.com 

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FICPHS (Fellowship in International Congress in Pharmacy and Health Sciences), MICPHS (Member in International Congress in 

Pharmacy and Health Sciences), AMICPHS (Associate Member in International Congress in Pharmacy And Health Sciences) 

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