“FORMULATION AND IN-VITRO CHARACTERIZATION OF

DILTIAZEM HYDROCHLORIDE FLOATING TABLETS”

M. Pharm. Dissertation Protocol Submitted to

Rajiv Gandhi University of Health Sciences, Bangalore

Karnataka

By

Mr. G. SATYANARAYANA REDDY, B. Pharm.

Under the Guidance of

MR. SATHEESH KUMMAR.N

Senior Lecturer

DEPARTMENT OF PHARMACEUTICS

EAST WEST COLLEGE OF PHARMACY

BANGALORE–560091

2011-2013

ANNEXURE II

PROFORMA FOR REGISTRATION OF SUBJECTS FOR DISSERTATION

1 / Name of candidate and address (In Block Letters) / MR. G SATYANARAYANA REDDY
#PENCHALAPADDU (VILLAGE), VIDAPANAKAL (MADAL), ANANTAPUR (DIST),
ANDHRA PRADESH
PIN-515842
2 / Name of the Institute / EAST WEST COLLEGE OF PHARMACY, BANGALORE-560 091
3 / Course of study and subject: / M.PHARM. ( PHARMACEUTICS)
4 / Date of admission of course: / (29/10/2011)
5 / Title of the topic:
“FORMULATION AND IN-VITRO CHARACTERIZATION OF
DILTIAZEM HYDROCHLORIDE FLOATING TABLETS”
6 / Brief Resume of this intended work:
6.1 Need for the study Enclosure-I
6.2 Review of Literature Enclosure-II
6.3 Objectives of study Enclosure-III
7 / Materials and Methods:
7.1 Source of data Enclosure-IV
7.2 Method of collection of data (Including sampling procedure, if any)
Enclosure-V
7.3 Does the study require any investigation or interventions to be conducted on patients of humans or animals? If so, please describe briefly.
------NO------
7.4 Has ethical clearance been obtained from your institution in case of 7.3?
------NOT APPLICABLE------
8 / List of References / Enclosure-VI
9 / Signature of the candidate / (Mr. G SATYANARAYANA REDDY)
10 / Remarks of the Guide / The proposed research work is recommended for registration and approval
11 / Name and designation of (in block letters)
11.1 Guide
11.2 Signature / SATHEESH KUMMAR.N
SENIOR LECTURER
DEPT. OF PHARMACEUTICS,
EAST WEST COLLEGE OF PHARMACY,
BANGALORE-560 091.)
11.3 Co-Guide (if any)
11.4 Signature / ------
------
11.5 Head of Department
11.6 Signature /
Dr. VENKATA RAJU. M. P
PROFESSOR AND HOD
DEPT.OF PHARMACEUTICS,
EAST WEST COLLEGE OF PHARMACY,
BANGALORE-560 091.
12 / 12.1 Remarks of the Chairman / Principal
12.2 Signature / Prof. K. A. SRIDHAR
PRINCIPAL,
EAST WEST COLLEGE OF PHARMACY,
BANGALORE-560 091

ENCLOSURE-I

6) Brief resume of the intended work:

6.1) Need for the study:

Hypertension is one of the most common worldwide disease affecting human beings. Various approaches have been pursuing to increase the retention of hypertension. It is a chronic epidemic medical condition in which the blood pressure is elevated. It can be classified as essential (primary) and non-essential (secondary) hypertension. Essential or primary hypertension is the definite cause for the rise in blood pressure is unknown. About 90-95% of hypertension is essential hypertension. Secondary hypertension indicates that the rise of blood pressure as a result of ( i.e., secondary to) another condition, such as renal, endocrine and vascular lesions. Persistent hypertension is one of the risk factor for strokes, heart attacks, heart failure and arterial aneurysm that leads to chronic renal failure.1

Oral drug delivery is the most preferred route because of ease administration. Drug bioavailability of pharmaceutical oral dosage form is influenced by various factors. One of the important factors is gastric residence time (GRT) of these dosage forms. Indeed, gastric retention has received significant interest in the past few decades as most of the conventional oral delivery system have shown some limitations related to fast gastric emptying time. A gastro retentive dosage form (GRDF) can overcome this problem and is particularly useful for drugs that are primarily absorbed in the duodenum and upper jejunum segments.2

Various studies have been conducted to prolong gastric retention time which includes floating system or hydro dynamically controlled systems that have sufficient buoyancy to float over the gastric content and remain buoyant in the stomach without affecting the gastric emptying rate. While the system is floating on the gastric content, the drug is released slowly at the desired rate from the system. After release of the drug, the residual system is emptied from the stomach. This results in an increased GRT and a better control over the fluctuations in plasma drug concentration.3

Diltiazem Hydrochloride is a calcium channel blocker belonging to the benzothiazepine family, has molecular weight of 414.518 and molecular formula C22H26N2O4S (2S,3S)-5-[2-(dimethylamino)ethyl]-2-(4-methoxyphenyl)-4-oxo-2,3,4,5-tetrahydro-1,benzothiazepin-3-yl acetate). It is freely soluble in water. it is widely prescribed for the treatment of hypertension and angina. It undergoes an extensive biotransformation, mainly through cytochrome P-450 CYP3A, which results in less than 4% of its oral dose being excreted unchanged from urine. It is absorbed only in the upper part of the GI tract and insoluble at lower part of GI tract (i.e., at higher pH) and is subject to undergo an extensive first-pass metabolism. It has elimination half life of 3.5 hrs. The recommended adult oral dosage of DTZ HCL for angina pectoris is 60mg 3 times a day and for hypertension 60 to 120mg twice a day which can be increased to 360mg a day.4,5

The drug candidate is selected to achieve increased gastric residence time for the dosage form and sustained drug release. The current study is designed to formulate sustained release oral floating tablets of Diltiazem Hydrochloride and to evaluate in-vitro characterization of the formulated tablets.

ENCLOSURE-II

6.2) Review of literature:

Literature review was helped for understanding the concept of current study by referring various articles published in National and International Journals, standard reference books and websites.

Gambhire MN et al., developed floating matrix tablets of Diltiazem Hydrochloride to prolong gastric residence time and to increase its bioavailability. The tablets were prepared by direct compression technique using polymers such as HPMC, Methocel K100CR, Compritol 888 ATO either individual or in combination with other excipients. Sodium bicarbonate was incorporated as a gas generating agent. A 32 factorial design was applied systematically to optimize the drug release profile. The amount of Methocel K100CR and Compritol 888 ATO were selected as dependent variables. The results of factorial design showed that a high level of both Methocel K100 CR and Compritol 888 ATO favored the preparation of floating controlled release of DTZ HCL tablets. Comparable release profiles between the commercial products and the designed system were obtained. The linear regression analysis and model fitting were shown that all formulations followed. Korsmeyer and Peppas model, which had a higher value of Correlation coefficient (r).5

Pathan AB et al., They have designed floating tablets of Diltiazem Hydrochloride by direct compression method. Sodium bicarbonate was used as a gas generating agent and dicalcium phosphate was used as a channeling agent. They evaluated on the prepared tablets for their dimensions, hardness, friability, and weight variation test, content of active ingredient, floating lag time, floating time and dissolution profiles. The in-vitro dissolution studies were shown that the sustained release for more than 6hrs.The study revealed that increased concentration of polymer retarded the rate of drug release.6

Enami J et al., They have developed prolonged release of gastro retentive formulations of Ciprofloxacin Hydrochloride. A variety of polymers and effervescent properties were utilized to optimize the desired disposition profile. Tablets were prepared by direct compression technique by using polymers like HPMC K100M, CP 971P, Xantham gum, NaCMC, Crospovidone and sodium bicarbonate. The prepared tablets were evaluated for physical properties, swelling, floating and drug release characters. Plasma concentration of Ciprofloxacin Hydrochloride was measured by a very sensitive and reliable HPLC method .The method was validated for linearity, accuracy, precision. Cmax was found to be 0.945 ± 0.29ug/ml. AUC0-∞ was found to be 8.54± 1.87 .7

Sivabalan M et al., have formulated and evaluated hydro dynamically balanced controlled drug delivery system of glipizide. The formulated tablet showed increased bioavailability and reduction in dosing frequency. The formulation was designed by adopting optimization technique, which helped in setting up experiments to obtain the efficient and pricing information. The tablets were formulated using various polymers such as HPMC; MC and EC. The tablets were prepared by direct compression and evaluated the drug content, in vitro release profile and buoyancy. The dissolution study was carried out in simulated gastric fluid using dissolution test apparatus by employing paddle stirrer. The maximum buoyancy was observed that the formulated tablet with HPMC as polymer which had a high level of drug polymer ratio. The optimized formulation consists of HPMC as polymer exhibited controlled release of drug of 59.25% when evaluated for in-vitro release profile .8

Chandra RM et al., They have formulated and evaluated gastro retentive drug delivery of gastro-prokinetic drug, Itropride Hydrochloride. They developed the floating tablets of Itropride Hydrochloride, which on oral administration, causes prolonged gastric residence time and there by increases drug release rate, and drug bioavailability. They fabricated floating tablets using direct compression method; containing Itropride Hydrochloride with polymers such as HPMC K100M, HPMC K15M and Carbopol-934 P, along with gas generating agents like sodium bicarbonate and citric acid. They added Carbopol that aided in the reduction of the drug dissolution due to their in hydrophobic nature. They optimized the concentration of these agents to get desired controlled release of drug They evaluated floating tablet for its physical characterization, assay, swelling index, in vitro drug release, hardness, friability and weight variation, corresponding results indicated that gas powered floating tablet of Itropride Hydrochloride containing 125mg HPMC K100M, 40mg HPMC K15M, and 40mg Carbopol provided a better option for 24hrs release action and improved bioavailability. They carried out accelerated stability study, at 400C/75% RH, of optimized formulation for one month and no significant change was observed. They worked on the concept that would help in promoting gastrointestinal transit and speed up gastric motility, and there by relieve the symptoms associated with it. 9

Kendra PN et al., have developed and formulated single unit controlled delivery system of theophylline floating matrix tablets by direct compression method using gas generating agent and various viscosity grades of hydrophilic polymers (HPMC K15M, K4M;HPC and carbopol934). Formulations were optimized on the basis of buoyancy and in-vitro drug release profile. The prepared tablets were tested by various methods like hardness, thickness, weight variation, friability swelling index and erosion index. The release rate was efficiently modified by varying the matrix forming polymer, the use of polymer blends and addition of water soluble or insoluble fillers (dicalcium phosphate, mannitol, lactose). All formulations showed that good matrix integrity and retarded the release of drug for 20 hrs. The release pattern of theophylline was fitted to korsmeyer equation indicating that diffusion along with erosion could be the mechanism of drug release.10

Jagdale SC et al., They have developed a gastroretentive drug delivery system of Propranolol Hydrochoride and studied various factors affecting bioavailability. They investigated that the ability of various polymers were retained the drug release when polymers used in different concentrations. HPMC K4M, HPMC E 15 LV, HPC; Klucel HF, Xantham gum and Sodium alginate were evaluated for their gel-forming abilities. Floating tablets of Propranolol HCL tablets were formulated with HPC, Sodium alginate and HPMC E 15 LV failed to produce matrix of required strength, where as it was found that tablet formulated with xantham gum showed good drug retaining ability but failed in floating property. Therefore floating tablets were formulated finally with HPMC K 4M and HPC.11

ENCLOSURE-III

6.3) Objective of the study:

ü  To formulate sustained release oral floating tablets for various release pattern of Diltiazem Hydrochloride using different concentration of polymers as well as gas generating agents.

ü  To optimize the formulations.

ü  To evaluate the floating lag time of the tablets.

ü  To study compatibility between the drug and polymer.

ü  To evaluate in-vitro drug release.

ü  To evaluate water uptake study (swelling studies).

ENCLOSURE-IV

7) Materials and Methods:

Materials

Drug: Diltiazem hydrochloride

Polymers and excipents: HPMC K-15M, HPMC K-4M, HPMC K-100M, Carbopol 934P, Xantham gum, Guar gum, Sodium bicarbonate, Citric acid, MCC, Dicalcium phosphate, Talc, Magnesium stearate, Lactose, or any other appropriate polymers and excipents may be selected.

Methods:

Diltiazem Hydrochloride tablets will be prepared by direct compression method using suitable excipents and polymers.

7.1) Source of data:

Data is collected from:

1.  Textbooks and reference books.

2.  International and National journals.

3.  Research publications.

4.  Presentations like pharmaceutical poster presentation.

5.  Science Direct and other internet facilities.

6.  RGUHS Library.

ENCLOSURE-V

7.2) Method of collection of data:

Ø  Compatibility studies of drug with excipients

Ø  To evaluate the pre compression parameters for granules

Pre-compression parameters

·  Angle of repose

·  Bulk density

·  Tapped density

·  Hausner’s ratio

·  Carr’s index

Ø  Preparation of gastro retentive floating tablets of Diltiazem Hydrochloride by direct compression method.

Ø  To investigate the post compression parameters of prepared tablets.

Post-compression parameters

·  Weight variation

·  Thickness

·  Friability

·  Hardness

·  Floating lag time

·  Drug content

Ø  To carry out in-vitro drug release studies for the prepared formulations.

Ø  Fitting the data to various kinetic equations and to find the release parameters

ENCLOSURE-VI

8) List of references:

1.  Satoskar RS, Bhandarkar SD: Pharmacology and Pharmacotherpeutics revised 18th Edition, 2005; 396-97.

2.  Prinderre P, Sauzet C, Bruno MC, Nicolas M, Kister J, Piccerelle P. An innovative floating gastro retentive dosage system: Formulation and in-vitro evaluation. Int J Pharm 2009; 378:23-29.

3.  Yadav S, Tiwari A. A review of work done on floating drug delivery system containing cardio vascular drugs. Int Res J Pharm 2012; 3(3):97-101.

4.  Siddiqui AI, Bakde BV, Dr. Tappar KK. Needs of floating drug delivery system for diltiazem hydrochloride. J Pharm Bio Sci 2011;5(5):1-7.

5.  Gambhire MN, Ambade KW, Kurmi SD, Kadam VJ, Judahav KR. Development and in-vitro evaluation of an oral floating matrix tablet formulation of diltiazem hydrochloride. AAPS Pharm Sci Tech 2007;8(3):E1-E9.

6.  Pathan AB, Kulkani AS, Mhadeshwar AP, Kumbhar SS. Design and evaluation of floating tablets of diltiazem hydrochloride. Int J Pharm Bio Sci 2012; 3(1):447-53.