“NEW ANALYTICAL METHODS FOR THE QUANTITATIVE ESTIMATION OF MOXIFLOXACIN AN ANTIBACTERIAL DRUG IN
BULK AND PHARMACEUTICAL DOSAGE FORMS”
SYNOPSIS FOR
M.PHARM DISSERTATION
SUBMITTED TO
RAJIV GANDHI UNIVERSITY OF HEALTH SCIENCES
KARNATAKA
4TH ‘T’ BLOCK
Jayanagar, Bangalore.
BY
NATARAJ.VALMIKI
I M. PHARM
DEPARTMENT OF PHARMACEUTICAL ANALYSIS
BHARATHI COLLEGE OF PHARMACY
BHARATHI NAGAR
KARNATAKA -571422
RAJIV GANDHI UNIVERSITY OF HEALTH SCIENCES,
KARNATAKA.
annexure – II
PROFORMA FOR REGISTRATION OF SUBJECTS FOR DISSERTATION
1 / Name of the candidateAddress / NATARAJ.V
1st M. Pharm
Bharathi college of pharmacy
Bharathi nagara
Maddur(T)
Mandya(D)-571422
PERMANENT ADDESS
NATARAJ.V
D.NO.49/50A/87F/19D
Lakshmi Nagar
Kurnool-518002
Andhra Pradesh.
2 / Name of the institution / BHARATHI COLLEGE OF PHARMACY,
BHARATHI NAGARA,
MANDYA(DIST),
KARNATAKA-571422.
3 / Course of the study and subject / MASTER OF PHARMACY (Pharmaceutical Analysis)
4 / Date of admission / JUNE-10-2007
5 / Title of the Topic / “NEW ANALYTICAL METHODS FOR THE QUANTITATIVE ESTIMATION OF MOXIFLOXACIN AN ANTIBACTERIAL DRUG IN BULK AND PHARMACEUTICAL DOSAGE FORMS”
6.BRIEF RESUME OF THE INTENDED WORK:
6.1.Need For The Study:
Moxifloxacin is a synthetic Fluoro quinolone antibiotic used to treat bronchitis, pneumonia, sinusitis, and certain skin infections. It is a synthetic fluoro quinolone antibiotic agent. It is also used in ophthalmology for the treatment of conjunctivitis under the name Vigamox.
(1-cyclopropyl-7-[(1S,6S)-2,8-diazabicyclo[4.3.0]non-8-yl]-6-fluoro-8-
methoxy-4-oxo- quinoline-3-carboxylic acid)
Moxifloxacin
Moxifloxacin is a water insoluble solid having the molecular formulae of C21H24FN3O4 and molecular weight of 401.431 g/mol.
Category : Fluoro quinolone Antibiotic.
.
The literature survey reveals that Moxifloxacin was analyzed quantitatively by using HPLC1,HPTLC2 and Tandem mass spectroscopy3. But there are no methods are there for the quantitative estimation of Moxifloxacin by using spectroscopy. Hence there is a need for the development of a newer, simple, sensitive and accurate spectroscopial analytical methods for the quantitative estimation of Moxifloxacin in bulk and pharmaceutical dosage forms.
6.2) REVIEW OF LITERATURE:
From previous journals and web releases:
1) Tatar ulu.S1 has developed a sensitive high-performance liquid chromatographic (HPLC) method for the determination of Moxifloxacin in human plasma using fluorescence detection method.
2) Shah’s etal2. have developed a new simple, sensitive, specific and precise high performance thin layer chromatographic method has been developed for estimation of Moxifloxacin in its tablet formulation.
3) Viswanathan,k etal3. have developed a rapid, sensitive and selective method for the determination of Moxifloxacin.The method based on liquid chromatography electro spray ionization tandem mass spectrometry (LC/ESI-MS/MS) was developed and validated to quantitate Moxifloxacin in human plasma.
4) Sanjay K. Motwani etal. have developed a simple, sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for densitometric determination of Moxifloxacin both bulk and from pharmaceutical formulation.
5) Sanjay K Motwani etal. developed a new, simple, cost effective, accurate and reproducible UV-spectrophotometric methods were developed and validated for the estimation of Moxifloxacin in bulk and pharmaceutical formulations.
6) Cruz, L.A etal. have developed enantiomeric purity assay of Moxifloxacin hydrochloride by capillary electrophoresis.
7) Boubakar B.Ba etal. have developed a new method for the development of Moxifloxacin in growth media by HPTLC.
8) Lemonie T etal. developed a new method for the determination of Moxifloxacin in human plasma and lung tissue by HPLC with ultra violet detection using a fully automated extraction with a new polymeric cartridge.
9) Tobin CM etal.have developed an isocratic high performance liquid chromatographic (HPLC) assay for Moxifloxacin 8-methoxy fluoro quinolone.
10) Kumar YR etal. have studied about the structural identification and characterization of impurities in Moxifloxacin.
6.3OBJECTIVE OF THE STUDY:
1. To establish a sensitive and an accurate method for the quantitative estimation of Moxifloxacin as an active ingredient in bulk drugs by various spectrophotometric and chromatographic methods.
2. To validate the newly developed methods in accordance with the analytical validation parameters mentioned in the USP and ICH guidelines.
3. To applying the newly developed and validated analytical method for the
Quantitative estimation of Moxifloxacin in formulations.
7. MATERIALS AND METHODS:
MATERIALS:
In the present investigation of newer analytical method development for the quantitative estimation of Moxifloxacin, the chemicals and other reagents required will be procured from standard companies. The methods will be standardized on Systronics 2201 double beam spectrophotometer and other chromatographic instruments using calibrated volumetric glass apparatus. The pure sample of Moxifloxacin for the research work will be procured from Aurobindo pharma limited, Hyderabad.
The following analytical methods are planned to develop with high sensitivity, accuracy, precision and economy.
1. Acid dye method.
2. Difference spectrophotometric method.
Acid dye method:
Since Moxifloxacin is having heterocyclic imino group it can be condensed with amine in its ionized form to an ionized acidic dye11 by acid dye method.
Eg: using Methyl orange / Bromocresol purple /cresol red etc which yields a salt (ion pair) that may be extracted into an organic solvent such as chloroform / dichloromethane. The indicator dye will be added in excess and the PH of the aqueous Solution is adjusted if necessary to a value where both the imine and the dye are in ionized forms. The ion pair is then separated from the excess indicator by extraction into the organic solvent and the absorbance will be measured.
Difference spectrophotometric method:
Difference spectrophotometric method12 is the simplest and most commonly employed technique for altering the spectral properties of the analyte having the aromatic carboxylic acid group with the adjustment of the PH by means of aqueous solutions of acids / alkali / buffers.
Eg:
Imines are dependent on the state of ionization of the functional groups and consequently on the PH of the solution.
7.1 SOURCE OF DATA:
1. Bharathi college of pharmacy library, Bharathi nagara
2. e-library from Bharathi college of pharmacy library, Bharathi nagara
3. IISC library, Bangalore
4. RGUHS library ,Bangalore
5. IICT library, Hyderabad
7.2.METHOD OF COLLECTION OF DATA(including sampling procedures if any)
Data collected from:
Analytical and chemical abstracts, Indian institute of sciences, Bangalore
Journals:
Ø Journal of pharmaceutical and biomedical analysis
Ø Indian journal of pharmaceutical sciences
Ø Spectro chim Acta A Mol Biomol sciences
Ø Analytica chemica acta
Ø J.Antimicrob chemother
Ø Journal of chromatography B.Bio medical sciences and applications
Related links:
www.sciencedirect.com
www.pubmed.com
www.google.com
www.drugbank.com
www.dogpile.com
www.medline.com
7.3. Does the study require any investigation or investigations to be conducted on patients or other
humans or animals?
-NOT APPLICABLE-
7.5. Has ethical clearance been obtained from your institution in case of 7.4?
-NOT APPLICABLE-
8.BIBLIOGRAPHY:
1) Tatar ulu.S1, High performance liquid chromatography assay for Moxifloxacin:
Pharmaco kinetics in human plasma.
Journal of pharmaceutical and biomedical analysis.
Vol.43, No.1, 320-324(2007).
2) Rathodi.S; Suhagia.BN; Baldaniya M.V2- High performance thin layer Chromatographic method for estimation of Moxifloxacin in tablet dosage forms.
Indian Journal of pharmaceutical sciences .Vol.67(1), 112-15.(2005).
3) Viswanathan, k; Bartlett.M.G; Stewart.J.T3 –Determination of Moxifloxacin in human
plasma by liquid chromatography electro spray ionization Tandem mass spectrometry
Journal of pharmaceutical and biomedical analysis
Vol.30, No.4, 961-968(2002).
4) Sanjay K. Motwani, Roop K. Khar, Farhan J. Ahmad, Shruti Chopra, K. Kohli
and S. Talegaonkar-Application of a validated stability indicating densitometric
thin-layer chromatographic method to stress degradation studies on
Moxifloxacin.
Anal chim Acta: 2007 Jan 16; 582(1):75-82.
5) Sanjay K Motwani , Shruti Chopra , Farhan J Ahmad , Roop K Khar-Validated
Spectrophotometric methods for the estimation of Moxifloxacin in bulk and
Pharmaceutical dosage forms.
Spectro chim Acta A Mol Biomol Spectrosc 2006 Nov 24.
6) Cruz, L.A; Hall, R. Enantiometric purity assay of Moxifloxacin hydrochloride by capillary electrophoresis.
Journal of pharmaceutical and biomedical analysis
Vol.38, No.1,8-13(2005).
7) Boubakar B.Ba;Renaud Etiene;Dominique Ducint;Claudine Quertin and Marie-claude
saux –Determination of Moxifloxacin in growth media by HPTLC.
Journal of chromatography B:Bio medical sciences and applications
Vol.74, issue 1, 15 April 2001, 107-112.
8) Lemonie T,Breih D,Ducint D,Dubez J,Jougon J,Velly JF,Saux –Determination
of Moxifloxacin in human plasma and lung tissue by HPLC with ultra violet
detection using a fully automated extraction with a new polymeric cartridge
Journal of chromatography B:Bio medical sciences and applications
2000 JUN 9; 742(2):247-54.
9) Tobin CM, Sunderland J,White LO,Mac Gowan AP,Reves DS An isocratic high
performance liquid chromatographic (HPLC) assay for Moxifloxacin 8-methoxy
Fluoro quinolone.
Journal of Antimicrob chemother 1998 Aug;42(2):278-9.
10) Kumar YR; Prasad raju,V.V.N.K.V;Kumar;RR;Eswaraiah Mukkanti,K;
Suryanarayana,MV;Reddy,MS.; structural identification and Characterization of
Impurities in Moxifloxacin.
Journal of pharmaceutical and biomedical analysis.
11) Beckett A.H.,Stenlake J.B; practical pharmaceutical chemistry,4th edition,
Part Two; :293-304.
12) Kenneth A. Connors, Text book of pharmaceutical sciences, 3rd edition:484.
9 / Signature of the candidate: / Nataraj.V
10 / Remarks of the guide: / Recommened for study.
11 / Name and designation of
11.1 guide:
11.2 signature: / Dr. G.VIJAYA KUMAR
Professor And HOD,
Department Of Pharmaceutical Analysis
Bharathi College Of Pharmacy
Karnataka-571422
11.3 co-guide:
11.4 signature: / NOT APPLICABLE
11.5 Head of the Department:
11.6 Signature: / Dr. G. VIJAYA KUMAR
Professor and HOD
Department of pharmaceutical analysis
Bharathi college of pharmacy
Karnataka-571422.
12 / 12.1 Remarks of the Chairman and Principal:
Prof. Dr. T. TAMIZH MANI.
Principal,
Bharathi college of pharmacy,
Bharathi nagara.
Karnataka -571422
12.2 Signature