RESEARCH ARTICLE PREPARATION AND EVALUATION OF LEVOFLOXACIN HEMIHYDRATES FLOATING TABLETS



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JOUN OF U IVY SCH SCH TIC PPTION N VUTION OF VOFOXCIN HMIHYTS FOTIN TBTS YK Y.B* 1, Sai kishore.v 2, TejaKrishna.M 1, Prasada ao. K.V.S. 1 1. ahul institute of Pharmaceutical Sciences and esearch,chirala. 2. Bapatla College of Pharmacy,Bapatla BSTCT In the present investigation, an attempt was made to formulate floating tablets of evofloxacin hemihydrates using with gum kondagogu, xanthum gum and HPMC K1M as release modifier. ight batches of floating tablets of evofloxacin hemihydrates were prepared by using different drug : polymer (evofloxacin hemihydrates, HPMC K1M + karaya gum) ratios viz. F 1,F 2,F 3,F 4 and drug : polymer (evofloxacin hemihydrates, HPMC K1M + xantham gum) ratios viz.f 5,F,F 7,F 8. The compressed tablets were evaluated for hardness, uniformity of weight, friability, drug content. ll the readings are within the prescribed limits. There was no interaction between the drug, polymer and excipients it was found out by I studies. Swelling index studies were also carried out. The in vitro release data were fitted to different order of reactions such as zero order and Korsmeyer-Peppas reaction. It was found that, the drug release follows Korsmeyer-Peppas reaction. KYWOS: evofloxacin hemihydrates, Karaya gum, Xantham gum, HPMC K1M, Wet granulation method INTOUCTION The oral route is considered as the most promising route of drug delivery. ffective oral drug delivery may depend upon the factors such as gastric emptying process, I transit time, drug release from the dosage form and site of absorption. astric emptying of dosage forms is an extremely variable process, due to unpredictable gastric emptying rate and short gastric residence time. astric retention provides, longer residence time in the stomach that improves bioavailability for drugs that are readily absorbed upon release in the I tract [1]. These drugs can be delivered ideally by slow release from the stomach. Floating drug delivery, this system basically floats in the gastric fluid because of its lower density, than the gastric medium. evofloxacin is a synthetic flouroquinoline antibacterial agent that inhibits bacterial N replication. It is -isomer of Ofloxacin. It has a half life of hrs and the absorption of evofloxacin is dose dependent, which increases with increase in dose. It is used in treating various infections caused by microorganisms like bacillus anthracis, Chlamydia infection, cystitis, epidydimitys, gonorrhea etc. The dose ranges from 25mg to 75mg.It is first choice drug used for treatment of H.pylori infections. Floating drug 1 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH delivery system of evofloxacin hemihydrates can localize the drug action within the stomach to treat gastric ulcers caused by Helicobacter pylori. In the present study, natural polymers such as gum kondagogu and xanthum gum are selected for the preparation of floating tablets of evofloxacin hemihydrates. Sodium bicarbonate was used as gas generating agent. Tablets were prepared by wet granulation method using these polymers. MTIS N MTHOS Materials evofloxacin hemihydrate.was obtained as gift sample from Hetero abs, Hyderabad, um kondagogu, um kondagogu, Xanthum gum, HPMC K1M, PVP K 3, Isopropyl alcohol, Hydrochloric acid. sodium bicarbonate, magnesium stearate, were obtained from commercial sources. Preparation of evofloxacin hemihydrate floating tablets Floating tablets of evofloxacin hemihydrate were prepared by using different drug: polymer (evofloxacin hemihydrates + HPMC K1M + Natural polymer) ratios. The tablets were formulated by employing wet granulation method using PVP K 3 as binder and isopropyl alcohol as granulating fluid. ll the formulations contain 25 mg of evofloxacin hemihydrate, sodium bicarbonate as gas generating agent, magnesium stearate as lubricant and talc added as glidant. The details of composition of each formulation are given in Tables 1-2. VUTION PMTS Flow properties of granules. [2] a) Bulk ensity ( b ): It is the ratio of total mass of granules to the bulk volume of granules. It was measured by pouring the granules (passed through standard sieve # 2) into a measuring cylinder and initial weight will be noted. This initial volume is called bulk volume. From this the bulk density was calculated according to the formula mentioned below. It is expressed in g/ml and is given by Bulk ensity (g/ml) = Mass of the powder/bulk Volume b) Tapped ensity ( t ): It is the ratio of total mass of the granules to the tapped volume of the granules. Volume was measured by tapping the granules for 75 times and the tapped volume will be noted, if the difference between these two volumes is less than 2%. If it is more than 2%, tapping was continued for 125 times and tapped volume was noted. Tapping was continued until the difference between successive volumes is less than 2 % (in a bulk density apparatus). It is expressed in g/ml and is given by Tapped density (g/ml) = Mass of the powder/tapped volume c) ngle of epose (ө): The friction forces in greanules can be measured by the angle of repose (ө). It is an indicative of the flow properties of the powder. It is defined as maximum angle possible between the surface of the pile of granules and the horizontal plane. The granules were allowed to flow through the funnel fixed to a stand at definite height (h). The angle of repose was calculated by measuring the height and radius of the heap of granules formed. = tan -1 (h / r) 2 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH Where, is the angle of repose. h is the height in cms r is the radius in cms d) Carr s index (or) % compressibility: It indicates granule flow properties. It is expressed in percentage and is given by Carr s Index (%) = [(Tapped density Bulk ensity) / Tapped ensity] 1 e) Hausner ratio: Hausner ratio is an indirect index of ease of granules flow. It is calculated by the following formula. Hausner s atio = Tapped density / Bulk ensity valuation of tablets a) Hardness [3] : The hardness of the tablet was measured by Monsanto hardness tester. The lower plunger was placed in contact with the tablet and a zero reading was taken. The plunger was then forced against a spring by tuning a threaded bolt until the tablet fractured. s the spring was compressed a pointer rides along a gauge in the barrel to indicate the force. The hardness was measured in terms of kg/cm 2. b) rug content [4] : 2 tablets were weighed and powdered the powder weight equivalent to 1mg of evofloxacin trihydrate was dissolved in 1ml of.1n HCl and filtered. 5ml of this was diluted to 5ml with water and drug content was estimated using UV-VISIB spectrophotometer at 293nm. c) Weight variation [3] : Formulated tablets were tested for weight uniformity, 2 tablets were weighed collectively and individually. From the collective weight, average weight was calculated. The percent weight variation was calculated by using the following formula. verage Weight - Individual Weight % Weight Variation = verage Weight d) Friability [3] : The oche friability test apparatus was used to determine the friability of the tablets. Twenty preweighed tablets were placed in the apparatus and operated for 1 revolutions and then the tablets were reweighed. The percentage friability was calculated according to the following formula. Initial Weight - Final Weight Friability = X1 Initial Weight e) Swelling Index [5] : Formulated tablets were weighed individually (W ) and placed separately in Petri dish containing 5 ml of.1 N HCl. The Petri dishes were placed in an incubator maintained at 37±.5 o C. The tablets were removed from the petri dish, at predefined intervals of time and reweighed (Wt), and the % swelling index was calculated using the following formula: % W U = (Wt Wo/Wo) 1 Where: W U Water uptake Wt Weight of tablet at time t Wo Weight of tablet before immersion f) In vitro buoyancy study [] : This test is characterized by floating lag time and total floating time. The test was performed using USP-Type II paddle apparatus using 9 ml of.1n HCl at paddle rotation of 1 rpm at 37 ±.5 C. The time required for tablet to rise to surface of dissolution medium and duration of time the tablet constantly float on dissolution medium was noted as floating lag time and total floating time. 3 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH g) In vitro dissolution test [7] : The release of evofloxacin hemihydrate from the tablet was studied using USP-Type II paddle apparatus. rug release profile was carried out in 9 ml of.1n HCl maintained at 37 ±.5 C temperatures at 1 rpm. 5 ml of samples were withdrawn at regular time intervals. The samples was replaced by its equivalent volume of dissolution medium and was filtered through.45 µm Whatman filter paper and analyzed at 293 nm by UV spectrophotometer. h) Infra ed Spectral analysis [8] : I Spectral analysis was used to study the interactions between the drug, polymer and the excipients. The drug and excipients must be compatible with one another to produce a product stable, efficacious and safe. SUTS N ISCUSSION Floating tablets (F 1 -F 4 ) of evofloxacin hemihydrate were prepared by varying the concentration of HPMC K 1 M and gum kondagogu. The composition of formulations (F 1 -F 4 ) is shown in table.1.the formulated granules were subjected to various micromeritic properties and the values were shown in table.3.the formulated tablets were subjected to various quality control tests like hardness, friability, weight variation and drug content various physical properties are shown in table 4.The formulations(f 1 -F 4 ) containing xanthum gum in combination with HPMC K1M increase in drug release with increase in concentration of gum kondagogu when compared formulation containing only HPMC K1M. The drug release from formulation F 5 containing only gum kondagogu showed a maximum drug release at end of 1 hours. rug release from the formulation containing HPMC K1M was lesser owing to its high viscosity and also due to less permeability of water, as the drug release rate is dependent on the viscosity grade and the concentration of the polymers used. To ascertain the mechanism of drug release, the dissolution data was analyzed by zero order, first order, and Higuchi and Peppas equations. The correlation coefficient values (r) revealed that the dissolution profiles follows Zero order kinetics and the mechanism of drug release was governed by Peppas model. The n values are found to be more than.5 (n>.5) indicted that the drug release was predominantly controlled by non fickian diffusion. The in-vitro drug release kinetic data was shown in table 5 and figures 1,2 and 3.The swelling index studies showed a gradual increase with increase in concentration of gum kondagogu which indicates the natural tendency of it to swell 5-1 times of its original value. The swelling index values are shown in table. and figure.4. The influence of xanthum gum concentration on drug release, formulations (F 5 -F 8 ) were prepared using different concentrations of xanthum gum with HPMC K1M by wet granulation method. The composition of formulations (F 5 -F 8 )is shown in table.2.the formulated granules were subjected to various micromeritic properties and the values were shown in table.7. The formulated tablets were subjected to various quality control tests like hardness, friability, weight variation and drug content various physical properties are shown in table.8.the formulations(f 5 -F 8 ) containing xanthum gum in combination with HPMC K1M showed decrease in drug release with increase in concentration of 4 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH xanthum gum when compared formulation containing only HPMC K1M(F 1 ). The drug release from the formulations (F -F 8 ) showed very slow release as compared to other formulations. The in vitro release data for formulations (F -F 8 ) was presented in table.9 and figure.5,. The release rate followed zero-order release kinetics and the data was fitted in the Peppas plots.the exponential coefficient from the Peppas plots was found to be in between.75 to.88, indicating non fickian mechanism of drug release.the release rate of evofloxacin hemihydrate was found to be retarded by xanthum gum with an increase in its concentration. The swelling index of tablets formulated with xanthum gum (F -F 8 ) was found to be higher than that of other formulations which can be attributed to high viscosity and high water retention property of both HPMC K1M and xanthum gum. The values of swelling index are tabulated in table.1 and shown in figure.8. From the above table 11 it is clearly evident that the invitro release of drug from the floating tablet was influenced by nature of natural polymer. Based on the release rate constant and % of drug release at the end of 12 hours the release retarding capacities of the natural polymers were arranged in the following order. Xanthum gum> gum kondagogu. Table.1 : Composition of evofloxacin hemihydrate floating tablets formulated with different concentrations of gum kondagogu Ingredients F 1 (mg) F 2 (mg) F 3 (mg) F 4 (mg) evofloxacin hemihydrate 25 25 25 25 HPMC K 1 M 9 3 um Kondagogu 3 9 12 Sodium bicarbonate 1 11 11 11 PVP K 3 5 5 5 5 Magnesium stearate 12 7.5 7.5 7.5 Talc 13 7.5 7.5 7.5 Total 5 5 5 5 5 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH Table.2 : Composition of evofloxacin hemihydrate floating tablets formulated with different concentrations of xanthan gum. Ingredients F 5 (mg) F (mg) F 7 (mg) F 8 (mg) evofloxacin hemihydrates 25 25 25 25 HPMC K 1 M 9 3 um Xanthum 3 9 12 Sodium bicarbonate 11 11 115 115 PVP K 3 5 5 5 5 Magnesium stearate 7.5 7.5 5 5 Talc (2%) 7.5 7.5 5 5 Total weight 5 5 5 5 Table.3 : Micromeritic properties of evofloxacin hemihydrate granules formulated with different concentrations of gum kondagogu Formulation code ngle of repose Bulk density Tapped density Compressibility index Haussners ratio F 1 29.89±.241.28±.11.37±.25 12.7±.19 1.145±.19 F 2 28.41±.25.271±.21.313±.17 13.41±.11 1.154±.14 F 3 29.33±.214.28±.17.32±.31 12.5±.24 1.142±.25 F 4 3.81±.233.281±.15.319±.19 12.7±.1 1.14±.17 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH Table.4 : Physical properties of evofloxacin hemihydrates floating tablets formulated with different concentrations of gum kondagogu. Formulation Hardness (kg/cm 2 ) Weight variation (mg) Friability (%) rug content (%) Floating lag time (min) Total floating time (hrs) F 1 4.8±.44 5.47±.44.2±.24 99.45±.15 1.4 >14 F 2 4.7±.27 51.39±.94.37±.12 11.89±.1 2 13 F 3 4.2±.82 499.54±.55.37±.11 99.58±.17 2.15 13 F 4 4.5±.23 5.34±..39±.124 11.45±.13 3.15 11 Table.5 : In vitro drug release kinetic data of evofloxacin hemihydrate floating tablets formulated with different concentrations of gum kondagogu. Correlation Coefficient Value elease xponentia ate Formulatio l T Constant 5 n Zero First Matri Peppa T Coefficient 9 Order Order x s (mg/hr)k (n) F 1 F 2 F 3 F 4.989 2.97 1.973 3.978 8.949.975.972 5.941.938.9742 17.7442.825 7.9552.971 19.4295.271.4.92.978 21.125.449 5.9 12. 7 11. 1..9451.9543 22.778.37 5.5 9.9 7 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH Figure.1 : Comparative in vitro drug release profile of evofloxacin hemihydrate floating tablets formulated with different concentrations of gum kondagogu. % U S 1 8 4 2 2 4 8 1 12 14 TIM(hours) F 1 F 2 F 3 ж F 4 Figure.2 : Comparative Zero order plots of evofloxacin hemihydrate floating tablets formulated with different concentrations of gum kondagogu 3. M O U N T O F U S ( m g ) 25. 2. 15. 1. 5.. 5. 2 4 8 1 12 14 TIM(hours) F 1 F 2 F 3 ж F 4 8 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH Figure.3 : Comparative Peppas plots of evofloxacin hemihydrate floating tablets formulated with different concentrations of gum kondagogu O % U S 2.5 2 1.5 1.5.2.4..8 1 1.2 O TIM F 1 F 2 F 3 ж F 4 Table. : Swelling index values of evofloxacin hemihydrate tablets formulated with different concentrations of gum kondagogu Formulation code Swelling index Time in hours after 1 hour after 2 hours after 8hours F 1.99 83.89 148.5 F 2 8.34 8.49 157.5 F 3 57. 8.91 155.4 F 4 5.31 79.35 137.42 Figure.4 : Comparative swelling index plot of evofloxacin hemihydrate floating tablets formulated with different concentrations of gum kondagogu S W I N I N X ( % ) 18 1 14 12 1 8 4 2 1 2 3 4 5 7 8 9 TIM(hours) F 1 F 2 F 3 ж F 4 9 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH Table.7 : Micromeritic properties of evofloxacin hemihydrate granules formulated with different concentrations of xanthum gum. Formulatio ngle of Bulk n code repose density F 5 25.7±.5.255±.2 5 F 2.4.±..271±.2 7 1 F 7 27.32±.9.314±.1 8 F 8 2.54±.13.353±.2 7 Tapped density.291±. 5.31±.1 1.3±.1 9.4±.1 4 Compressibilit Haussners y index ratio 12.37±.24 1.142±.1 4 14.24±.19 1.1±.1 9 14.27±.27 1.15±.1 1 11.75±.17 1.133±.2 7 Table.8 : Physical properties of evofloxacin hemihydrate floating tablets formulated with different concentrations of xanthum gum. Formulation Hardness (kg/cm 2 ) Weight variation (mg) Friability (%) rug content (%) Floating ag time Total floating time (hrs) F 5 4.±.48 51.3±.54.39±.25 11.52±.23 1.98 min >15 F 4.4±.32 51.±.49.35±.19 99.87±.41 3.25 min >18 F 7 4.7±.29 499.91±.39.42±.2 11.93±.1 5.2 min >22 F 8 5.2±.54 5.8±.51.4±.32 1.23±.4 min >22 Table.9 : Comparative in vitro drug release profile of evofloxacin hemihydrate floating tablets formulated with different concentrations of xanthum gum Formulatio n F 5 F F 7 F 8 Correlation Coefficient Value Zero Order.995 8.98.984 9.997 3 First Order.92.947.949 9.971 Matri x Peppa s elease ate Constant (mg/hr)k 1 Volume 2 Issue 1 213 www.earthjournals.org xponentia l Coefficient (n) T 5.95.997 1.5772.9411 7.5.8822.989 1..8777 7.8.8835.979 15.1187.933 8.3.981.9943 14.1717.97 8.8 T 9 13. 14. 1 14. 9 15. 9

JOUN OF U IVY SCH Figure.5 : Comparative in vitro drug release profile of evofloxacin hemihydrate floating tablets formulated with different concentrations of xanthum gum % U S 8 7 5 4 3 2 1 5 1 15 TIM(hours) F F 7 F 8 F 9 F F 7 F 8 ж F 9 Figure. : Comparative Zero order plots of evofloxacin hemihydrate floating tablets formulated with different concentrations of xanthum gum M O U N T O F U 25. 2. 15. 1. S 5.. 2 4 8 1 12 14 TIM(hours) F F 7 F 8 ж F 9 11 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH Figure.7 : Comparative Peppas plots of evofloxacin hemihydrate floating tablets formulated with different concentrations of xanthum gum 2 1.8 1. O 1.4 1.2 % 1.8 S. U.4.2.2.4..8 1 1.2 O TIM F F 7 F 8 ж F 9 Table.1 : Swelling index values of evofloxacin hemihydrates tablets formulated with different concentrations of xanthum gum Swelling index Formulation code Time in hours after 1 hour after 2 hours after 8hours F 52.9 7.4 145. F 7 53.53 89.89 154. F 8 58.53 9.1 18.5 F 9 5.33 15.41 171.34 12 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH Figure.8 : Comparative swelling index plot of evofloxacin hemihydrate floating tablets formulated with xanthum gum 18 S 1 W I 14 N 12 1 8 I X N % 4 2 ( ) 2 4 TIM(hours) 8 1 F F 7 F 8 ж F 9 Figure.9 : I spectrum of evofloxacin hemihydratre. 13 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH Figure.1 : I spectrum of evofloxacin + gum kondagogu. Figure.11 : I spectrum of evofloxacin + xanthum gum 14 Volume 2 Issue 1 213 www.earthjournals.org

JOUN OF U IVY SCH Table.11: Comparative invitro release parameters of evofloxacin hemihydrates floating tablets formulated with various natural polymers and HPMC K 1 M.(1:1 ratio) Formulation % rug release at end of 12 hours. F 3 (evofloxacin+ gum kondagogu) 85.9 19.43 elease ate Constant k (mg/hr) F 7 (evofloxacin+xanthum gum) 73.33 15.11 CONCUSION The natural polymers used showed drug release retarding nature high viscosity value and good drug release retarding capacity and the release retarding nature of Xanthum gum was greater than gum kondagogu..from this study it could be concluded that natural polymers can be used in the preparation of floating tablets and in combination with synthetic polymers. Floating tablets of evofloxacin hemihydrate prepared by employing natural polymers could be used for treatment of gastric ulcers caused by H.pylorii infection by prolonging the gastric residence time and its controlled release in the gastric environment thus completely eradicating the H.pylo from IT. FNCS 1. Shivanand Pandey, Viral evmurari, Shukla Paridhi, athanand Mahalaxmi. evelopment and In Vitro valuation of Propranolol Hydrochloride Based astro-etentive Floating Tablet.er Pharmacia ettre, 2 (1); 21. p.75-8. 2. ebjit Bhowmik, Chiranjib.B, Krishnakanth, Pankaj,.Margret Chandira.Fast issolving Tablet: n Overview.Journal of Chemical and Pharmaceutical esearch. 1(1); 29. p.13-177. 3. The United State Pharmacopoeia.United state Pharmacopoeial Covenction, ockville, M. sian dn. 2. 4. Frick,, Möller, H and Wirbitzki,, ur. J. Pharmaceutics and Biopharmaceutics, 4,1998. p.35 5. eshpande, Shah NH, hodes CT, Malick W. evelopment of a novel controlled release system for gastric retention. Pharm esearch.14 ();1997 p. 815-819.. avi Kumar, M. B. Patil, Sachin. Patil, Mahesh S. Paschapur. Formulation and valuation of ffervescent Floating Tablet of Famotidine. International Journal of PharmTech esearch. 1 (3); 29. p. 754-73. 7. Patel VF, Patel NM. Statistical evaluation of influence of viscosity of polymer and type of filler on ipyridamole release from floating matrix tablets. Ind J Pharm Sci. 9 (1):27. pp. 51-57. 8. S.K. Sreekanth, S. Palanichamy, T. aja Sekharan,. Thanga Thirupathi.: Formulation and valuation Studies of Floating Matrix Tablets of Nifedipine. International Journal of Pharma and Bio Sciences. 1 (2);21. pp. 1-8. 15 Volume 2 Issue 1 213 www.earthjournals.org