INVESTIGATION OF NEW VALIDATED ANALYTICAL METHODS

FOR THE ESTIMATION OF SOME ANALGESIC

DRUGS IN PHARMACEUTICAL DOSAGE FORMS

M. Pharm Dissertation Protocol

Submitted to

Rajiv Gandhi University Of Health Sciences,
Bangalore, Karnataka

By

harish n.babladkar

Under the guidance of

Dr. S.APPALA RAJU

M.Pharm., Ph.D.

DEPARTMENT OF PHARMACEUTICAL ANALYSIS

H.K.E.S’S MATOSHREE TARADEVI RAMPURE INSTITUTE OF PHARMACEUTICAL SCIENCES,

GULBARGA – 585105

2012-13

RAJIV GANDHI UNIVERSITY OF HEALTH SCIENCES KARNATAKA, BANGALORE

ANNEXURE-II

PROFORMA FOR REGISTRATION OF SUBJECTS FOR DISSERTATION

1. / Name of the Candidate and
Address (in block letters) / HARISH N BABLADKAR H.NO 98 PRAGATI COLONY BADEPURE SEDAM ROAD GULBARGA 585105 (KARNATAKA)
2. / Name of the Institution / H.K.E.S’s MATOSHREE TARADEVI RAMPURE INSTITUTE OF PHARMACEUTICAL SCIENCES,
Sedam Road, GULBARGA-585 105
3. / Course of Study and Subject / M.PHARM.
(Pharmaceutical Analysis)
4. / Date of Admission to Course / 24.01.2013
5. /

Title of the Research topic

/ “Investigation OF NEW VALIDATEDANALYTICAL METHODS FOR THE ESTIMATION OF SOME ANALGESIC DRUGS INPHARMACEUTICAL DOSAGE FORMS
6. /

BRIEF RESUME OF INTENDED WORK

6.1 Need for Study:

Flupirtine maleate is a non-opioid centrally acting, structurally dissimilar from other analgesics.it is used in the treatment of various types of pains, it is not official in any pharmacopoeial investigation of some new instrumental methods are in need for the quantitative estimation of Flupirtine in bulk drug and pharmaceutical dosage forms with high sensitivity ,accuracy precision and economical too.

6.2 Review of literature :

Flupirtine is chemically[ 2-amino-6-[[(4-fluorophenyl)methyl]amino]-3-pyridiniyl]carbamic acid ethyl ester(I). It is a non-opioid centrally –acting, structurally dissimilar form other analgesics. flupirtine is a unique centrally acting , non-opioid analgesic, with muscle relaxant and neuroprotective properties1-3 .


FLUPIRTINE
(I)
No analytical methods have been reported except RP-HPLC4 and UV5,6 for quantitative determination of Flupirtine in bulk drug and pharmaceutical dosage form. There is necessity to invent some of the more instrumentalfor Flupirtine in bulk drug and pharmaceutical dosage forms as an alternative.
6.3 Objective of Study

R-NH2: FLUPIRTINE

(I)

i) Since, Flupirtine(I) is having heterocyclic amino group, it can be condensed with various aromatic aldehydes (II) like p-dimethylaminobenzaldehyde (PDAB), p-dimethylaminocinnamaldehyde (PDACA) and vanillin to get colored Schiff’s bases (III) and can be used for quantitative estimation of drug by visible spectrophotometry.

R' = 1) N-(CH3)2 2) –OH (4); -CH3(5)


ii) Heterocyclic amino group can be diazotised with nitrous acid (HNO2) and coupled with chromogenic agents (IV) like N-(l-napthyl) ethelenediamine dihydrochloride, B-napthol, napthalamine and phloroglucinol to get colored chromogens (V) and drug can be estimated quantitatively by colorimetry.
Along with Bratton-Marshall Reagent, we can also use other coupling agents mentioned above and develop number of new analytical methods.
iii) The amino group in flupirtine allows the oxidative coupling reaction with 3-methyl-2-benzothiazolinone hydrazone (MBTH) in presence of Ferric chloride/Cerric ammonium sulphate and forms colored chromogen (VI) by which drug can estimated quantitatively by colorimetry.

iv) Flupirtine forms colored complex (VII, VIII) with 1,10-phenanthroline and 2,2’-bipyridine in presence of Fe(III) which can be utilized for quantitative estimation of Flupiritine in pharmaceutical formulation.
v) Phosphomolybdo tungstic acid well known as Folin-Ciocalteu reagent in alkaline pH forms colored chromogens with Flupirtine due to presence of heterocyclic amino group by redox reaction which can be used for quantitative estimation of Flupirtine in bulk drug and its pharmaceutical formulations.
vi) Visible spectrophotometric methods can also be developed using chromogenic reagent like Gibb’s reagent due to presence of heterocyclic amino group in the drug.
vii) Simultaneous spectrophotometric and HPLC methods can also be developed.
viii) Various HPTLC methods also can be developed.
ix) Reversed phase HPLC methods can be developed by varying the conditions for estimation in bulk drugs and pharmaceutical formulation.
7. /

MATERIAL AND METHODS

In the present investigation of new instrumental methods for quantitative estimation of Flupirtine, we are in need and using Shimadzu 1800 double beam UV/visible spectrophotometer, HPLC (Shimadzu class up series 6.01), chromatographic instruments and volumetric glass apparatus. Drug sample will be collected from Lupin Pharmaceuticals.Inc.Bandra East Mumbai.

7.1 Source of Data

a) Internet, Library
b) Gulbarga University, Gulbarga
c) I.I.Sc. Library, Bangalore
d) I.I.C.T. Library, Hyderabad
e) R.G.U.H.S. Library, Bangalore.
7.2 Methods of Collection of Data (including sampling procedure, if any)
Data collected from
i) Internet, H.K.E.S. College of Pharmacy, Gulbarga.
ii) Analytical abstract and chemical abstract Gulbarga University, I.I.C.T. & I.I.SC. Libraries.
iii) Journals like – Indian J. Pharmaceutical Sciences, Indian Drug & Indian J. Analytical Chemistry.
iv) e-Journals
v) Drug sample of Flupirtine will be collected from Lupin Pharmaceuticals.Inc.BandraEast Mumbai.
7.3 Does study require any investigation or interventions to be conducted on patients or other 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. /

REFERENCES:

1.O’ Neil MJ. editor, The Merck Index: An Encyclopedia of Chemicals, Drug, Biological, 14th edn. Merck & Co. Inc.: 2006: p. 4363.
2. Sweet man SC. editor, Martindale: The Complete Drug Reference, 35th edn. Pharmaceutical Press, London: 2007: p. 41.
3.Karen Methling et.al investigation of the in vitro metabolism of analgesic Flupirtine, The American society for pharmacology and experimental therapeutics ,2008,pp.1-49
4.
5. Aneesh TP et.al, “ Method development and validation for the estimation of flupirtine maleate in bulk and pharmaceutical dosage forms using UVspectrophotometry”, international research journal of pharmacy 2011,2(12), 179-182.
6. Article/ppaqa/1028/13.aspx.
9. / Signature of Candidate /

HARISH N. BABLADKAR

10. / Remarks of the Guide / The work undertaken is novel and results oriented and may lead to new research findings.
11. / Name & Designation of (in block letters)
11.1Guide / Dr.S.APPALA RAJU M.Pharm., Ph.D.
PRINCIPAL
DEPT. OF PHARMACEUTICAL ANALYSIS, H.K.E.S’s MATOSHREE TARADEVI RAMPURE INSTITUTE OF PHARMACEUTICAL SCIENCES,GULBARGA.
11.2Signature
11.3Head of the Department / Dr. S.M.MALIPATIL, M.Pharm, Ph.D
PROFESSOR
DEPT. OF PHARMACEUTICAL ANALYSIS, H.K.E.S’s MATOSHREE TARADEVI RAMPURE INSTITUTE OF PHARMACEUTICAL SCIENCES,GULBARGA.
11.4Signature
12. / 12.1Remarks of the Chairman & Principal
12.2 Signature