Publication Ref No.

: IJPRD/2010/PUB/ARTI/VOV-2/ISSUE-7/SEP/004

ISSN 0974 9446

STUDIES IN OPTIMIZATION OF NON AQUEOUS FILM COATING PARAMETERS Rohokale BS1*, Jadhav VM2, Kadam VJ3. Bharati Vidyapeeth College of Pharmacy, CBD Belapur, Navi Mumbai-4000614.(MS) 2 Formulation and Development Department , Holden Medical Laboratories Pvt Ltd, Nashik (MS). Email: rajrohokale@yahoo.com
Rohakale BS
1

ABSTRACT The purpose of this research was to study the non-aqueous film coating of tablets utilizing a laboratory scale perforated coating pan apparatus. The important process parameter of with respect to film quality were evaluated by using trial batches. Tablet were evaluated for coating uniformity(mg), coating process efficiency (%) & surface roughness. The Spray rate, atomization air pressure, distance of nozzle from tablet bed, inlet air temperature, pan differential pressure, pan speed and % solid content these affect on final film quality of coated tablets. The process parameters related to perforated pan coating process can be identified and optimized. Key Words: Non-aqueous film coating, coating uniformity, coating coating pan. INTRODUCTION Film coating mask the undesirable taste or odor, improve appearance, provide tablet identity, facilitate swallowing & control or modify release of drug. Also it protect tablet from moisture, light & temperature effect. Some tablet may contain moisture sensitive ingredients the use of water creates problem of physical and chemical stability of the coated tablet (Ruotsalainen et al, 2003). process efficiency, perforated

As generalization there are very few tablets formulations that cannot be aqueously film coated (Tonadachie et al., 1977). Film coating depends on various factors, type of core tablet, coating material, coating equipment, shape of tablet, coating solvent & process conditions etc and all these parameter are interlinked. This work was carried out to study nonaqueous film coating process of tablet performed in perforated coating pan

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Publication Ref No.: IJPRD/2010/PUB/ARTI/VOV-2/ISSUE-7/SEP/004

ISSN 0974 9446

equipment. In this work seven process parameters (Spray rate, atomization air pressure, distance of nozzle from tablet bed, inlet air temperature, pan differential pressure, pan speed and % solid content ) of important with respect to coating uniformity, coating process efficiency and surface roughness were evaluated. MATERIAL AND METHODS: Opaspray blue O2K53395 (colorcon) was used as a coating material. The coating were done by pan-coating equipment (Ganson cota, Ganson Ltd). The core tablet composed of lactose ( Lactose India Ltd), starch ( Universal Starch co.), magnesium state (Nikita Chemicals co.). Preparation of coating solution: Required quantity (for 2% weight gain) isopropyl alcohol (Lee Chung Yung Chemical Co. ) was taken into solution preparation tank to this Opaspray blue (O2K53395) and dichloromethane ( Lee Chung Yung Chemical Co. ) was added with stirring till all Opaspray blue get mixed properly. Then this solution was filtered through 100 mesh. All operations was done in flame proof area. Coating of tablets : The tablet were coated with use of perforated coating pan equipment. Inlet air flow, exhaust air flow & pan differential pressure was kept constant at 100 cubic foot per minute (cfm), 150 cfm, 4-8 mm respectively. First quantity of tablet 3kg were kept in pan at inlet temperature 60c till outlet temperature reaches to 45c. Then actual weight was determined. Then connect spray assembly tubing to peristaltic spray pump & this pump to filtered solution tanks. After than various parameter like spray rate, inlet air temperature, pan speed, distance of nozzle from tablet bed, spray width,

peristaltic pump RPM were completion of coating tablet inlet temperature of 85c by for 20min. Then tablet were pan for evaluation. Evaluation parameters:

adjusted. After were dried at jogging of pan unloaded from

Coating uniformity(CU) CU was calculated as the difference in weight gain within coating process. The Standard deviation (SD) was calculated as Standard dviation (SD) ={[(wtai-wtbi)-X]2/(n 1)}1/2 Where wtai and wtbi are the weight of tablet i after and before coating respectively correct by drying to final weight , n is the number of tablet, X is average weight gain of the n measured tablets taken for coating. Coating process efficiency(CPE) CPE is actual percent weight gain respect to theoretical percent. CPE=(%wga/%wgt)100% Where wgt is therotical percent weight gain which is in this work is 2% and wga is actual percent weight gain which was calculated as %wga= [(wta-wtb)wtb] 100% wta and wtb is total batch weight gain after and before coating respectively. Surface roughness Surface roughness was measured visually and was graded from 1 to 10 from better to best.

with

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Publication Ref No.: IJPRD/2010/PUB/ARTI/VOV-2/ISSUE-7/SEP/004

ISSN 0974 9446

RESULT AND DISCUSSION: 1. Optimization of spray rate Coating was performed at different spray rate of 4,6,8,10,12 ml/min at constant atomizing pressure(1.5 kg/cm2), inlet air temperature (60C), pan speed (5RPM), % solid content ( 8%) & distance of nozzle from tablet bed (18cm) and spray rate was optimized for CU,CPE & surface roughness. Result was as shown in table no 1. At lower spray rate solution was evaporated before reaching to tablet surface and at higher spray rate white spot, sticking & picking observed. It was reported that at lower and higher spray rate CPE was lower. Hence it was concluded that at 8 ml/min has to be used for coating process for further study. 2.Optimization of atomizing air pressure Coating was performed at different atomizing air pressure 0.5,1,1.5,2,2.5 kg/cm2 at constant spray rate 8ml/min, inlet air temperature 60C, pan speed 5 RPM, % solid content 8% & distance of nozzle from tablet bed (18cm) . Atomizing air pressure was optimized for CU, CPE & surface roughness. Result was as shown in table no 2. At lower and higher atomizing air pressure unsatisfactory spray pattern was reported. At lower atomizing air pressure droplets formed of larger size due to this rough surface was observed. Hence CPE reported was not satisfactory at lower and higher atomizing air pressure. It was observed that at 1.5 kg/cm2 atomizing air pressure satisfactory CPE reported. 3.Optimization of distance between tablet bed and spray gun Coating was performed at different distance between tablet bed and spray gun of 12,14,16,20 & 22 centimeter(cm) at constant atomizing air pressure(1.5 kg/cm2 ), inlet air temperature 60C , pan speed (5 RPM), %

solid content (8%) and spray rate 8ml/min. Distance was optimized for CPE,CU & surface roughness. Result was as shown in table no.3. At minimum distance white spot & rough surface was observed because solution was sprayed at high speed over tablet. On other hand at maximum distance unsatisfactory coating observed because solution get evaporated before reaching tablet surface. Hence coating CPE was lower at minimum & maximum distance. At 16cm distance coating was excellent. 4.Optimization of inlet air temperature Coating was performed at different inlet air temperature 40,50,60,70 & 80C at constant % solid content (8%), atomizing air pressure (1.5 kg/cm2 ), spray rate (8ml/min), distance of nozzle from tablet bed (18cm)& speed of pan (5RPM) and inlet air temperature was optimized for CPE, CU & surface roughness. Result was as shown in table no 4. At lower temperature sticking, picking and tablet get stick to pan. At high temperature solution get evaporated before reaching over tablet surface & nozzle block observed. Hence CU, CPE and surface roughness was noted at low and high temperature. But at 60C all parameter was found excellent and it was recommended that this temperature should be used for further study. 5.Optimization of pan differential pressure (DP) Coating was performed at different pan D P (with respect to coating area) 2,3,4,5 & 6 mm (D P was adjusted by changing inlet air CFM) at constant spray rate (8ml/min), inlet air temperature (60C ), pan speed (5RPM), atomization air pressure (1.5 kg/cm2), % solid content (8%) & distance of nozzle from tablet bed (16cm) and pan differential pressure was optimized for CU, CPE & surface roughness. Result was shown as per table no 5. At lower pan DP undercoat, overcoat 3

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Publication Ref No.: IJPRD/2010/PUB/ARTI/VOV-2/ISSUE-7/SEP/004

ISSN 0974 9446

and sticking was recorded and at high DP spray pattern was disturbed because spray pattern was moving upward direction so white spot and undercoat tablets was observed. Hence CU, CPE & surface roughness was found unsatisfactory. But at 5mm DP spray pattern was observed satisfactory. 6 Optimization of pan speed (RPM) Coating was performed at different pan speed of 3,4,5,6 & 7 RPM at constant spray rate (8ml/min), inlet air temperature (60C ), atomization air pressure (1.5 kg/cm2), % solid content (8%) & distance of nozzle from tablet bed (16cm) & pan DP 5mm and pan speed was optimized for CU, CPE & surface roughness. Result was shown as per table no 6. At minimum speed sticking, picking was recorded and as speed of pan increased the CU,CPE and surface roughness was found satisfactory because tablet mixing and distribution was done properly but at 5 RPM pan speed CU, CPE and surface roughness observed effective. Hence for further study 5RPM was used for investigation. 7. Optimization of % solid content Coating was performed at different % solid content of 6, 8 & 10 at constant spray rate (8ml/min), inlet air temperature (60C ), atomization air pressure (1.5 kg/cm2), speed of pan (5RPM), distance of nozzle from tablet bed (16cm) & pan DP 5mm and % solid content was optimized for CU, CPE & surface roughness. Result was shown as per table no 7. At lower % solid content particle get dried before reaching tablet surface hence CU, CPE and surface roughness was recorded good but as % solid content increased larger droplet was formed with non-uniform distribution of solution over tablets. But at 8% solid content CU, CPE and surface roughness was excellent.

CONCLUSION At lower spray rate un-uniform coating was reported and at high rate white spot, sticking and picking problem was recorded. Variation in atomization air pressure affect over quality of coating process because at high atomization air pressure small droplet was formed and at low atomization air pressure big droplet was formed. As distance between tablet bed and spray gun increased disturbed spray spray pattern was observed even at minimum distance sticking & white spot over tablet noted. At low inlet air temperature rough surface, sticking, picking & white spot was observed and at high temperature white spot & rough surface observed. As pan DP reduced spray was disturbed. Higher RPM of pan increase the mixing and distributions of spray over the tablet. At high % solid content create problem like roughness over tablet. Hence optimized parameter which was recommended for further study as spray rate (8ml/min), atomization air pressure (1.5kg/cm2), distance of nozzle from tablet bed (16cm), inlet air temperature (60C), pan differential pressure (5mm), pan speed (5RPM) and % solid content(8%) . ACKNOWLEDGEMENT: The authors are greatful to Holden Medical laboratories Pvt Ltd ,Nsahik (M.S) for providing necessary facilities to carry out this work. REFERENCES: 1. Cole GC.,(1998). Pharmaceutical coating technology, Taylor and Francis Ltd,6-52. 2.PorterBruno,(1980)Coatingof pharmaceutical solid-dosage forms,Pharm.Tech.,4(3):66. 3.Wilson K E Crossman E(1997).The influence of tablet shape and pan speed on intra tablet

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film coating uniformity, Drug Dev.Ind.pharm,23:239-1243. 4.Tobiska S , Klienbudde P,A.(2001). Simple method for evaluating the mixing efficiency of new type of pan coater,Int. J. Pharm,224;141149. 5 Franz RM , Doonan GW.(1983)Measuring the surface temperature of tablet beds using infrared thermometry, Pharm Techno (l)7:55-67. 6. Porter SC,Verseput R, Cunningham C R(1997). Process Optimization using design of experiments, harm Technol,21:60-70. 8.Twitchell AM, Hogan JE Aulton M E(1995). The behaviour of the film coating droplet on the impingement onto uncoated and coated tablet,S.T.P Pharm. Sci, 5:190-195. 9.Banker G. S.(1966). Film coating theory and practice, J. Pharm. Sci.,55(1):81-89. 10.Pickard J.F, Rees J.E(1972). Morden trends in pharmaceutical coating, Pharm. Ind.,43(11):833-839. TABLES AND FIGURES:

11.Hogan J.E,(1982). Aqueous versus organic solvent film coating, Int. J. Pharm. Tech. Prod. Mfr 3(1):17-20. 12.M.Ruotsalainen et al, studies in aqueous film coating of tablets in side vented perforated pan coater, ISBN -10-1041-X, 2003 Helsinki, 352.

Table 1: Optimization of spray rate. Batch no Spray rate (ml/min ) 4 6 8 10 12 CU CPE (mg) (%) Surface roughnes s 4 5 6 5 3 Observation

NA/FC/TB1 NA/FC/TB2 NA/FC/TB3 NA/FC/TB4 NA/FC/TB5

1.6 1.8 2.0 2.2 2.4

70.10 86.50 88.90 75.10 60.20

Ok Ok Ok White spot Sticking, picking & white spot.

NA/FC/TB= Non aqueous/ film coating/tablet batch.

Table 2: Optimization of atomizing air pressure.

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Batch no

NA/FC/TB 1 NA/FC/TB 2 NA/FC/TB 3 NA/FC/TB 4 NA/FC/TB 5

Atomizing air CU pressure(kg/c (mg) 2 m) 0.5 2.6 1.0 1.5 2.0 2.5 1.8 2.1 2.2 2.4

CPE (%) 62.10 86.10 90.94 80.10 53.00

Surface roughnes s 5 6 8 6 4

Observation

Sticking & picking Ok Ok Ok Disturbed spray pattern, dust generation

Table no 3 Optimization of distance between nozzle and tablet bed. Batch no Distance CU betn. nozzle (mg) & tablet bed (cm) 12 14 16 20 22 2.5 2.2 2.0 1.5 1.8 CPE (%) Surface observation roughness

NA/FC/TB1 NA/FC/TB2 NA/FC/TB3 NA/FC/TB4 NA/FC/TB5

58.20 74.70 89.90 82.20 70.20

3 5 8 6 4

White spot Ok Ok ok White spot

Table no 4. optimization of inlet air temperature. Batch no Inlet air CU (mg) CPE Surface observation Temp( C) (%) roughness NA/FC/TB1 40 2.8 72.65 6 Sticking& picking NA/FC/TB2 50 2.4 80.60 5 Ok NA/FC/TB3 60 2.0 86.98 8 Ok NA/FC/TB4 70 1.8 70.70 4 White spot NA/FC/TB5 80 1.5 65.20 3 White spot& nozzle chock

Table no 5 optimization of pan differential pressure(DP) 6

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Publication Ref No.: IJPRD/2010/PUB/ARTI/VOV-2/ISSUE-7/SEP/004

ISSN 0974 9446

Batch no NA/FC/TB1 NA/FC/TB2 NA/FC/TB3 NA/FC/TB4 NA/FC/TB5

Pan DP(mm) 2 3 4 5 6

CU (mg) 2.6 2.4 1.8 2.1 2.5

CPE (%) 60.50 74.20 86.20 94.60 70.80

Surface observation roughness 4 Undercoat & nozzle chock 6 Ok 7 Ok 8 ok 5 Spray pattern disturbed & undercoat

Table no 6 optimization of pan speed (RPM) Batch no NA/FC/TB1 NA/FC/TB2 NA/FC/TB3 NA/FC/TB4 NA/FC/TB5 Pan speed CU (RPM) (mg) 3 3.0 4 5 6 7 2.4 2.0 2.2 2.6 CPE (%) 68.20 84.60 94.20 82.30 64.50 Surface observation roughness 4 Sticking picking 6 Sticking picking 8 Ok 5 ok 3 Undercoat

& &

7. Optimization of % solid content Batch no Solid content (%) 6 8 10 CU (mg) 2.4 2.2 2.8 CPE (%) observation Surface roughness 5 6 4 Sticking & picking Sticking & picking Ok

NA/FC/TB1 NA/FC/TB2 NA/FC/TB3

80.40 89.60 70.20

7
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