ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF DICLOFENAC SODIUM IN SOLID DOSAGE FORM BY USING HPLC.

M. Pharm. Dissertation Protocol Submitted to

Rajiv Gandhi University of Health Sciences, Karnataka Bangalore –560041.

By

Mr. MANISH DWIVEDI B.Pharm

Under the Guidance of

SRI. C.S.HALLIKERIM. Pharm,

LECTURER

DEPT. OF PHARMACEUTICAL CHEMISTRY,

Department of Pharmaceutical Chemistry SET’s College of Pharmacy, S. R. Nagar, Dharwad, Karnataka –580002. RAJIV GANDHI UNIVERSITY OF HEALTH SCIENCES,

BANGALORE, KARNATAKA

ANNEXURE –II

PROFORMA FOR REGISTRATION OF SUBJECT DISSERTATION

1. NAME OF THE CANDIDATE Mr. MANISH DWIVEDI AND ADDRESS DEPT. OF PHARMA CHEMISTRY SET’s COLLEGE OF PHARMACY S.R.NAGAR, DHARWAD- 580002.

2. NAME OF THE INSTITUTION SET’s COLLEGE OF PHARMACY S. R. NAGAR, DHARWAD- 580002.

3. COURSE OF STUDY AND MASTER OF PHARMACY IN SUBJECT PHARMACEUTICAL CHEMISTRY

4. DATE OF ADMISSION TO THE JULY – 2013 COURSE

5. TITLE OF THE TOPIC

“ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF DICLOFENAC SODIUM IN SOLID DOSAGE FORM BY USING HPLC”

2 BRIEF RESUME OF THE INTENDED WORK:

6.1 Need for the study: Diclofenac sodium is a non-steroidal anti-inflammatory drug (NSAID) prescribed to reduce inflammation and as an analgesic in conditions such as arthritis. It can also be used to reduce menstrual pain, dysmenorrhea. The mechanism of action is inhibition of prostaglandin synthesis by inhibition of cyclooxygenase (COX). 1 A high performance liquid chromatography method is described for the determination of diclofenac sodium, its related compounds and degradation products in commercial sources of raw materials and solid dosage forms. This method is specific, accurate and stability indicating. The method employs a reverse-phase octylsilane (C18) column with a mobile phase composed of acetonitrile/methanol/pic B- 6 (25:25:50) and detection at 229 nm. The method resolves six principal related compounds with quantitation in the range 0.3-1.5%. Assay recoveries by spiking commercial formulations with diclofenac sodium were 99.64 ± 1.30%. Drug content in several commercial formulations are reported. Accelerated stability tests were conducted on raw materials and drug products and 1-(2,6- dichlorophenyl)-2-indolin-2-one was identified for the first time as a degradation product in solid dosage forms which are stressed under humidity and heat. Validation of analytical method: - Validation of analytical method is a process by which is established by laboratory studies, Industrial knowledge etc. It is the process of verifying the suitable method which is applicable for purpose or not. Method validation is an important element of quality control. Validation helps provide assurance that a measurement will be reliable. Different guidelines like ICH, WHO etc. suggest that analytical methods used for the analysis must be stability indicating and validated. There are different parameters that need to be evaluated for the purpose of validation of developed method such as, accuracy, precision, specificity, LOD (LOSS ON DRYING), robustness, linearity, and range. Various chromatographic methods such as HPLC, HPTLC, and GC etc. are used because it fulfills requirement of various guidelines. So the interest of work is emphasized on the HPLC technique, because in the modern pharmaceutical industry, high performance liquid chromatography (HPLC) is the major and integral analytical technique applied in all stages of drug discovery, development, and production.2 Most of the drugs in multicomponent and combination dosage form can be analyzed by HPLC method because of the several advantages like rapidity, specificity, accuracy, precision, and ease of automation in these methods. HPLC method eliminates tedious extraction and isolation procedures. There are different modes of separation in HPLC. They are Normal Phase Mode, Reversed Phase Mode, Reversed Phase Ion Phase Chromatography, Affinity Chromatography and Size Exclusion Chromatography.3  Normal Phase Mode: In these the stationary phase is polar and the mobile phase is non-polar 3 in nature. In these techniques, non-polar compounds travel faster and are eluted first. This is because of the lower affinity between the non-polar compounds and the stationary phase. 9. SIGNATURE OF THE STUDENT

10. REMARK OF THE GUIDE The above mentioned information and literature has been extensively investigated, verified and was found to be correct. The present study will be carried out under my supervision and guidance.

11. 11.1 NAME AND Sri. C.S.HALLIKERIM. Pharm DESIGNATION OF THE Lecturer GUIDE DEPT. OF PHARMA - CHEMISTRY, SET’s COLLEGE OF PHARMACY, S.R.NAGAR, DHARWAD- 580002.

11.2 SIGNATURE 11.3 NAME AND DESIGNATION OF CO-GUIDE

11.4 SIGNATURE ------

11.5 HEAD OF THE Dr. S. D. JOSHI M. Pharm, PhD. DEPARTMENT PROFESSOR AND HEAD DEPT. OF PHARMA - CHEMISTRY, SET’s COLLEGE OF PHARMACY, S.R.NAGAR, DHARWAD- 580002.

11.6 SIGNATURE

12. 12.1 REMARK OF THE The above mentioned information is correct and I PRINCIPAL recommend the same for approval.

12.2 SIGNATURE

Dr. V.H. KULKARNI M. Pharm, PhD. PROFESSOR & PRINCIPAL, SET’s COLLEGE OF PHARMACY, S.R.NAGAR, DHARWAD- 580002.

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