“DEVELOPMENT AND VALIDATION OF SPECTROPHOTOMETRIC METHODS FOR THE ESTIMATION OF CICLOPIROX OLAMINE AND TERBINAFINE HYDROCHLORIDE”
M.PHARM DISSERTATION PROTOCOL
Submitted to the
RAJIVGANDHIUNIVERSITY OF THE HEALTH SCIENCES, KARNATAKA
BANGALORE
By
SOJITRA PRADIPKUMAR KHODABHAI
B.Pharm
UNDER THE GUIDANCE OF
G M SREENIVASA,
M.Pharm
ASSISTANT PROFFESOR,
P. G. DEPARTMENT OF QUALITY ASSURANCE
S.C.SCollege of Pharmacy, Harapanahalli-583131
KARNATAKA
2010
RajivGandhiUniversity of Health Sciences, Karnataka, Bangalore
Annexure – II
PROFORMA FOR REGISTRATION OF SUBJECTS FOR DISSERTATION
01 / Name and Address of the Candidate / SOJITRA PRADIPKUMAR KHODABHAI13, SARITA SAGAR SOC;
B/H HARIKUNJ SOC; CHIKUWADI,
NANA VARACHHA,
SURAT.-395006
GUJARAT.
02 / Name of the Institution / T. M. A.E. Society’s
S.C.S.College of Pharmacy,
Harapanahalli- 583 131
03 / Course of the Study
Branch / M. Pharm.,
Quality Assurance
04 / Date of Admission to Course / 3rd Sept.- 2009
05 / Title of the Topic / “DEVELOPMENT AND VALIDATION OF SPECTROPHOTOMETRIC METHODS FOR THE ESTIMATION OF CICLOPIROX OLAMINE AND TERBINAFINE HYDROCHLORIDE”
06 / Brief Resume of the intended work
6.1 Need for the Study /
Enclosure- I
6.2 Review of the literature / Enclosure – II6.3 Objective of the Study / Enclosure – III
07 / Materials and Methods
7.1 Source of Data / Enclosure – IV
7.2. Methods of collection of data / Enclosure – V
7.3 Does the study require any
Investigation on animals?
If yes give details / Enclosure - VI
-NO-
7.4. Has ethical clearance been
obtained from your institution
In case of 7.3. / -NOT APPLICABLE -
08 / List of References / Enclosure – VII
09 / Signature of the Candidate / ( SOJITRA PRADIPKUMAR KHODABHAI )
10 / Remarks of the Guide / The present research work is original and not published in any of the journals with best of my knowledge upon extensive literature review. This work will be carried out in the Dept. of Quality Assurance laboratory by the above said student under my supervision.
11 / Name and Designation of
( In Block Letters )
11.1 Guide
ACA/CDC/PGT-M.ph/SCS/02/2005-06/19.01.09.
11.2 Signature
11.3 Co-Guide
ACA-2/RP-TEA/O1/97-98/3-9-98
11.4 Signature
11.5. Head of the Department
Signature / Mr.G. M.SREENIVASA
M.Pharm.
ASSISTANCE PROFESSOR,
S.C.S.COLLEGEOF PHARMACY,
HARAPANAHALLI- 583 131,
DIST.- DAVANGERE
Dr. E.JAYACHANDRAN
PROFESSOR & HEAD,
DEPT. OF PHARMACEUTICAL CHEMISTRY, S.C.SCOLLEGE OF PHARMACY
HARAPANAHALLI-583131.
DIST. - DAVANGERE.
Dr.R.NAGENDRA RAO
PROFESSOR & HEAD,
DEPT. OF QAULITY ASSURANCE,
S.C.S.COLLEGE OF PHARMACY,
HARAPANAHALLI -583131
12 / Remarks of the Principal
Signature / The candidate has been permitted to carry
Out the said above mentioned title in the Dept. Of Quality assurance.
PROF. K.PRABHU
Principal
S.C.S.College of Pharmacy
Harapanahalli-583131
KARNATAKA
ENCLOSURE - I
6. BRIEF RESUME OF THE INTENDED WORK:
6.1 NEED FOR THE STUDY
Ciclopirox Olamine and terbinafine hydrochloride are antifungal drugs which are clinically effective in the treatment of Dermatophytosis in human.It is caused by fungi of several different species. The fungi that cause parasitic infection (dermatophytes) feed on keratin, the material found in the outer layer of skin, hair, and nails. These fungi thrive on skin that is warm and moist, but may also survive directly on the outsides of hair shafts, or in their interiors1-2.
Validation of analytical methods is of critical importance as it is the cornerstone of process validation. An attempt has been made to develop and validate a simple, economic, rapid and accurate method. Here some simple and sensitive extractive methods mentioned to estimate both drugs3-13
- Derivative spectrophotometry
- Difference spectrophotometry
- Assay as a single-component sample
- Simultaneous equation method
- Geometric correction method
- Ion-Pair complexformation
- Ratio Spectra Method
- Least square approximation
- Colorimetric method
- Area under curve method
Ciclopirox is a synthetic antifungal agent for topical dermatologic use. Its chemical name is 6-cyclohexyl-1-hydroxy-4-methylpyridin-2-one and 2-aminoehanol. Its chemical formula is C12H17NO2 · C2H7NO
It contains
Ciclopirox (C12H17NO2; Mol Wt- 207.3): 76.0 per cent to 78.5 per cent (dried substance).
2-aminoethanol (C2H7NO; Mol Wt- 61.1): 22.2 per cent to 23.3 per cent (dried substance)14
Ciclopirox olamine is a synthetic broad spectrum antifungal agent that inhibits the growth ofpathogenic dermatophytes, yeasts, and Malassezia furfur. Ciclopirox olamine exhibitsfungicidal activity in-vitro against isolates of Trichophytonrubrum, Trichophyton
mentagrophytes, Epidermophytonfloccosum, Microsporumcanis, and Candida albicans.
Ciclopirox Olamine is thought to act through the chelation of polyvalent metal cations, such as Fe3+ and Al3+. These cations inhibit many enzymes, including cytochromes, thus disrupting cellular activities such as mitochondrial electron transport processes and energy production. Ciclopirox also appears to modify the plasma membrane of fungi, resulting in the disorganization of internal structures. The anti-inflammatory action of ciclopirox is most likely due to inhibition of 5-lipoxygenase and cyclooxygenase.15
Ciclopirox Olamine is available in cream, lotion, shampoo and solution.
Terbinafine hydrochloride (Lamisil) is a synthetic allylamine antifungal. It is highly lipophilic in nature and tends to accumulate in skin, nails, and fatty tissues. Its chemical name is N,6,6-trimethyl-N-(naphthalen-1-ylmethyl)hept-2-en-4-yn-1-amine and chemical formula C21H25N
It is used for the treatment of interdigitaltinea infections and is hypothesized to act by inhibiting squaleneepoxidase, thus blocking the biosynthesis of ergosterol, an essential component of fungal cell membranes.16
Terbinafine is available in cream, spray and tablet.
ENCLOSURE – II
6.2 REVIEW OF LITERATURE:
The review of various published work related to subject and objectives of the study has revealed the following:
- Cardoso SG, Schapoval EE.; UV Spectrophotometry and Nonaqueous Determination of Terbinafine Hydrochloride in Dosage Forms. J AOAC Int. 1999 Jul-Aug; 82(4):830-3.
- Lakshminarayana KV, Manohara YN, Gurupadayya BM, Development and validation of spectrophotometric methods for the estimation of nitazoxanide in tablet dosage forms. Ind. J. of Ph. Sci.,Year: 2007,Vol:69,Issue:1Page : 147-149
- Walash M.I.; Rizk M.S.; Iibrahim Eid M; Fathy M.E.;Spectrofluorimetric Determination of CiclopiroxOlamine via Ternarycomplex with Tb(III)and EDTA.Acta Pharmaceutica;Vol.56 No.4 Dec2006, Page .431
- Gowri Sankar D*, Joy Babu P, Anil Kumar B and Madhavi Latha P V; Spectrophotometric Determination of Aceclofenac and Famciclovir. Int. J. of Chem. Sci; Vol.4 (3):2006, 725-728.
- El-Saharty YS, Hassan NY, Metwally FH.; Simultaneous Determination of Terbinafine HCL and Ttriamcinolone Acetonide by UV derivative spectrophotometry and spectrodensitometry. J Pharm Biomed Anal. 2002 May 15;28(3-4):569-80.
- Pandey V P, Vanjnathan S, and Stella Singh; Determination of Domperidone and Omeprazole in Capsule Dosage form by UV/Visible Spectrophotometer. Asian J. of Chem; Vol.22, No.3 (2010), 2305-2308.
- Abdel-Moety E M,Kelani K O, Abou al-Alamein A M;Spectrophotometric determination of Terbinafine in presence of its Photodegradation products,J Pharm Biomed Anal. 2002 Nov 7;30 (4):1023-33
[My paper]ENCLOSURE-III
6.3 MAIN OBJECTIVE OF THE STUDY
The present work is in an attempt to:
- To develop selective, precise and sensitive method for the development and estimation of the Cilcopirox olamineand Terbinafine Hydrochloride.
- The analytical method so far developed is to be validated.
- The work involves use of analytical techniques such as Spectroscopy.
- The method appears to be suitable for the quality control in pharmaceutical industry.
ENCLOSURE-IV
7. MATERILAS AND METHODS
7.1 SOURCE OF DATA.
The preliminary data required for the experimental study was obtained form
- British Pharmacopoeia 2009
- Chemical sources
- Scientific sources
- Journals
- Internet sources
- From the helinet service of RGUHS, Bangalore.
- Relevant books
- Library, S.C.SCollege of Pharmacy
ENCLOSURE-V
7.2METHODS OF COLLECTION OF DATA
Data pertaining for the present study will be obtained from Quality Assurance Laboratory of S.C.S College of Pharmacy, Chemical abstracts, Scientific abstracts, Journals and Internet sources etc..,
ENCLOSURE - VI
7.3Does the study require any investigation to be conducted on patients/ Humans/ Animals? If so describe briefly
Not Applicable
7.4 Has ethical clearance been obtained from your institution in case of 7.3?
Not Applicable
7.5 METHODOLOGY:
- The experimental and spectral data pertaining for the present study is obtained from the various techniques adopted in the estimation of cefotaxime & ceftriaxone, in pharmaceutical preparation.
- The Spectrophotometric method shall be developed and validated in Q.A. lab of S.C.S.College of pharmacy.
- The study does not require any investigation on patients or humans or animals.
ENCLOSURE – VII
9. LIST OF REFERENCES:
- accessed on the date 26 May-2010
- Goodman & Gilman’s the Pharmacological basis of Therapeutics - 11th Ed.2006,
Chapter 48: Antimicrobial Agents: Antifungal Agents.HTML.
- Mahmoud Chamsaz, Mohammad HosseinArbabzavar, Tahereh, heidari* and Akram
Hajinia. Spectrophotomertic Determination of Trace Amounts of Beryllium in
Water using Mean Centering of Ratio Spectra Method and Partial Least Squares
Regression. Asian J. of Chem.2010, Vol.22, No.6, 4717-4726. - PatilShamkant*, DhabalePandurang andKuchekarBhanudas; Development and
Statistical Validation of Spectrophotometric Method for Estimation of
Esomeprazolein Tablet Dosage Form.Asian J. Research Chem. April.-June,
2009, Vol. 2(2)
- ManikyaSastry T., Trilochan Padhi and Ramakrishna K; Development and
Validation of Spectrophotometric Method for the Determination of Abacavir
Sulphate in Bulk and Pharmaceutical formulations. Int. J. Chem Sci,
2009, Vol: 7(2), 1053-1060.
- BalaSekaran C*, and Prameela Rani A.; Development and Statistical Validation of
Spectrophotometric Methods for the Determination of ACE Inhibitor in
Pharmaceutical formulation. Int. J. Chem, 2009 Sci.:7(2), 1153-11558.
- Ivana Savić1, Goran Nikolić1, Vladimir Banković; Development and Validation of
Spectrophotometric Method for Phenylephrine Hydrochloride estimation in Nasal
Drops formulation.Macedonian Journal of Chemistry and Chemical Engineering,
2008 Vol. 27, No. 2, , 149–156
- Maheshwari P, AppalaRaju S and SobhaManjunath. Development and Validation of
Spectrophotometric Methods for the Estimation of Balsalazide in bulk and
Pharmaceutical formulation. Int. J. Chem.2009, Sci.: 7(2), 1249-1254.
- EmirhanNemutlu* / SedefKır, Validated Determination of Meloxicam in Tablets by
Using UV Spectrophotometry, Hacettepe University, Journal of Faculty of
Pharmacy, January 2004, Vol. 24, No.1, 13-24.
- Lakshminarayana KV, Manohara YN, Gurupadayya BM; Development and
validation of spectrophotometric methods for the estimation of nitazoxanide in
tablet dosage forms. Ind. J. of Pharm Sci; Year: 2007, Vol: 69 Issue: 1, Page: 147-
149.
- Various UV spectrophotometric Simultaneous estimation methods, Pharmainfo.net,
2006, Vol- 4, issue -2.
- Ravindra N and Shingvi I; Spectrophotometric Method for the Estimation of
Aripirazole from Pharmaceutical Dosage form. Int. J. of Chem. Sci; 2006,
Vol4 (2), 241-244.
- Lakshmi KS, Ilango K, NithyaMathi N, Balaji S, Kige D, Victor Wathugi and
Sathish Kumar V; Visible Spectrophotometric Method for the Determination of
Ceftriaxome Sodium in Vials. Int. J. of Chem, 2006, Sci. Vol4 (2):347-350.
- British Pharmacopoeia 2009, Volume I & II, Monographs: Medicinal and
Pharmaceutical Substances, Ciclopirox Olamine, 1302.
- Drug Bank- Drug card for Ciclopirox (DB01188) from
- Drug Bank - Drug card forTerbinafine (DB00857) from
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