“DEVELOPMENT AND VALIDATION OF SPECTROPHOTOMETRIC METHODS FOR QUANTITATIVE ESTIMATION OF LEVOFLOXACIN AND CIPROFLOXACIN IN TABLET DOSAGE FORM”

DISSERTATION PROTOCOL

Submitted to the

RAJIV GANDHI UNIVERSITY OF HEALTH SCIENCES,

BANGALORE, KARNATAKA
BY

SHAIKH DANISH MOHAMMED SALIM

M.PHARM, PART- I

DEPARTMENT OF QUALITY ASSURANCE

UNDER THE GUIDANCE OF

Dr. M.H.HUGAR,

M.Sc. Ph.D.,

DEPARTMENT OF QUALITY ASSURANCE

LUQMAN COLLEGE OF PHARMACY

GULBARGA-585102, Karnataka

2012-2013

AnneXUre II

Proforma for Registration of subjects for Dissertation

1. / Name of the Candidate and
Address (in Block Letters) / SHAIKH DANISH MOHAMMED SALIM
C/O SAYED ABDUL SATTAR,
DABIRPURA, UDGIR.
DIST-LATUR.
(M.S). PIN- 413517.
2. / Name of the Institution / LUQMAN COLLEGE OF PHARMACY
GULBARGA-585102

KARNATAKA

3. / Course of the Study and Subject /

Master of Pharmacy in Quality Assurance

4. / Date of Admission to the Course / 10-07-2012
5. /

Title of the Topic

/ “DEVELOPMENT AND VALIDATION OF SPECTROPHOTOMETRIC METHODS FOR QUANTITATIVE ESTIMATION OF LEVOFLOXACIN AND CIPROFLOXACIN IN TABLET DOSAGE FORM ’’

6  BRIEF RESUME OF THE INTENDED WORK

6.1  NEED FOR THE STUDY

Drug therapy may be complicated in hospitalized patients receiving nutrition via internal feeding tubes. Dosage form selection and appropriate administration methods are crucial in patients with feeding tubes. Although hospitalized patients receive nutritional support through various routes, oral nutrition is preferred. internal or parenteral nutrition may be used if oral intake is inadequate or inadvisable. Patients with functional gastrointestinal tracts usually receive internal nutrition. Administering oral medications through the internal feeding tube can lead to complications like tube clogging or decreased drug activity. However, drug therapy need not be compromised in patients receiving internal nutrition. Careful selection and preparation of dosage forms reduces the complications of medication administration. Flushing the feeding tube and screening for drug incompatibilities decreases the incidence of tube clogging and replacement.

Drug therapy need not be compromised in patients receiving internal nutrition. Careful selection and preparation of dosage forms reduces the complications of drug administration. Properly flushing the feeding tube and screening for incompatibilities lowers the risk of tube clogging and the need for replacement.

Drug therapy may be complicated in hospitalized patients receiving nutrition via internal feeding tubes. Although oral nutrition is preferred, patients may require internal or parenteral nutrition if oral intake is inadequate or inadvisable. Patients with functional gastrointestinal (GI) tracts usually receive internal nutrition through a feeding tube1. Some medications may be given through the internal feeding tube. However, tube obstruction, increased toxicity, or reduced efficacy may occur if an improper administration method is used. In one survey, 74% of hospital staff used at least two incorrect methods to administer drugs via feeding tubes2.This article describes an approach to dosage form selection and drug administer action methods in these patients.

A simple, rapid, and accurate high-performance thin-layer chromatography (HPTLC) method is described for the simultaneous determination of levofloxacin and Ciprofloxacin in tablet dosage form. The method is based on the HPTLC separation of the two drugs followed by ensitometric measurements of their spots at 298 nm. The separation is carried out on Merck TLC aluminium sheets of silica gel 60 F254 using nbutanol– methanol–ammonia (5:1:1.5, v/v/v) as mobile phase. The linearity is found to be in the range of 50–250 and 100–500 ng/spot for Levofloxacin and Ciprofloxacin respectively. The method is successively applied to pharmaceutical formulation because no chromatographic interferences from the tablet excipients are found. The suitability of this HPTLC method for the quantitative determination of the compounds is proved by validation in accordance with the requirements laid down by International Conference on Harmonization (ICH) guidelines.

Cryptospordiasis and giardiasis is the type of infectious diarrhoea caused by Cryptospordium Parvum and Giardia lamblia. Cryptospordium is a protozoan that enters gastrointestinal epithelial cells causing diarrhoea and enteritis.3-4 The effective medical treatment includes Antiprotozoal agent (Levofloxacin) and Fluoroquinolone antibacterial agent (Ciprofloxacin). Levofloxacin and Ciprofloxacin combination is useful for the treatment of diarrhoea caused by susceptible organisms.5-8

To increase the efficacy and to utilize complementary mechanism of action of Levofloxacin and Ciprofloxacin a combination of these two drugs has been introduced in recent days. This combination has been indicated for the treatment of diarrhoea caused by susceptible organisms.5, 10-11

A survey of literature revealed only spectrophotometric method9 and RPHPLC10 method for estimation of Levofloxacin alone and spectrophotometric method11 and HPLC12-13, HPTLC15 method for estimation of Ciprofloxacin alone or in combination with other drugs has been established. However so for no method is reported for simultaneous estimation of these two drugs in tablet formulation till to date. The present work is an attempt to develop and validate a precise, simple, accurate and less expensive method for estimation of Levofloxacin and Ciprofloxacin that can be used for routine analysis in various pharmaceutical preparations. This is an effort towards achieving analysis of Levofloxacin & Ciprofloxacin combination tablet using spectrophotometric methods.9-17

6.2.  REVIEW OF LITERATURE

The review of various published work related to subject and objective of the study has revealed the following.

·  Koda-Kimble M.A et al, developed a Applied therapeutics and the clinical use of

Drugs Levofloxacin and Ciprofloxacin

·  Belknap D.C, et al. developed Administration of medications through internal

feeding catheters

.

·  K.V.Lakshminarayana, et al. developed and validated a spectrophotometric

method for the estimation of Nitazoxanide in tablet dosage form.9

·  Narayana L.K.V. et al. developed and validated RPHPLC method for the estimation of Nitazoxanide in bulk drug and tablets.10

·  Mathur S.C. et al.developed spectrophotometric determination of Ofloxacin in pharmaceutical preparation. 11

·  S.Dhake, et al. developed RPHPLC method for quantification of Ofloxacin in tablets.12

·  M. Gandhimati, et al. validated HPLC method for simultaneous estimation of Ofloxacin and Ornidazole in tablet dosage form.13

·  Halkar Uma P., et al. developed RPHPLC determination of Ofloxacin and Tinidazole in tablet dosage form.14

·  Gupta K. R., et al. developed HPTLC estimation of Ofloxacin and Tinidazole from pharmaceutical dosage form.15

·  Nagori B.P., et al. developed spectrophotometric method for simultaneous estimation of Ofloxacin and Ornidazole in tablet dosage form.16

6.3.  MAIN OBJECTIVES OF THE STUDY

The present work is an attempt to:

1.  Develop selective, accurate, precise, specific and sensitive method for Quantitative estimation of Levofloxacin and Ciprofloxacin in tablet dosages form.

2.  The analytical method so far developed is to be validated.

  1. The work involves use of various analytical spectrophotometric techniques.

7. MATERIALS AND METHODS

7.1 SOURCE OF DATA

The preliminary data required for the experimental study is obtained from-

  1. CD-Rom search available at National Center for Scientific Information (NCSI), Indian institute of Sciences, Bangalore,
  2. Luqman college of Pharmacy, Gulbarga Library.
  3. Scientific abstracts.
  4. Scientific Journals.
  5. Internet sources and Relevant Books.
  6. The data will be collected by Laboratory investigation and Recording the data.

7.2.  METHODS OF COLLECTION OF DATA

(Including sampling procedure, if any)

Data pertaining for the present study is obtained from pharmaceutical chemistry research laboratory of Luqman College of Pharmacy. Drug samples Levofloxacin and Ciprofloxacin were kindly supplied as a gift sample by Glenmark Pharmaceuticals, Ltd., (Nashik, India). Methanol, ammonia, and n-butanol were used as solvents to prepare the mobile phase. All the reagents used were of analytical-reagent grade (S.D. Fine. Chemicals, Mumbai, India) and used without further purification.

The experimental data would be obtained from various techniques adopted in the estimation of Levofloxacin and Ciprofloxacin in pharmaceutical preparation.

7.3 Does the study require any investigations or interventions to be conducted on patients or other humans or animals? If so please describe briefly.

The study does not require any investigations on patients or humans or animals.

7.4  Has ethical clearance been obtained from your institution in case of 7.3?

……………………..Not Applicable……………………………………

8.  LIST OF REFERENCES

1. Koda-Kimble MA et al, Applied Therapeutics: The Clinical Use of Drugs. 6th ed.

Vancouver: 1995, 34.1–28.

2. Belknap DC, et al, Am J Crit Care. Administration of medications through enteral feeding catheters

1997, 6(5). 382–392.

3. Doumbo O. et al, Am J Trop med Hyg 1997; 56(6): 637-639

4. Caroline Barranco, Nature Clinical Practice Gastroenterology and Hepatology (2006) 3; 302-303

5. Drug Profile –CIMS-97, Apr-July-2007 (Update-2); 102

6. Sweetman S.C.Martindale, The Complete drug reference (Pharmaceutical press),

34th edition; 239 and 612

7. Maryadele J.O.Neil, The Merk Index, 14th edition-2006; 6567 and 6771

8. British Pharmacopoeia-2004, Vol-2, General Notices, Monograph, Medicinal and

Pharmaceutical Substances; 1412

9. K.V.Lakshminarayana, et al, “Development and validation of spectrophotometric

method for the estimation of Nitazoxanide in tablet dosage form”. Indian Journal

of Pharmaceutical Science, Jan-Feb-2007, 69(1): 147-149

10. Narayana L.K.V. et al, “Development and validation of RPHPLC method for the

estimation of Nitazoxanide in bulk drug and tablets”. Indian Drugs June

2006,43(6): 503-506

11. Mathur S.C. et al “Development of spectrophotometric determination of Ofloxacin

in pharmaceutical preparation”.Indian Drugs1992, 29(8): 376-377

12. S.Dhake. et al, “Development of RPHPLC method for quantification of Ofloxacin

in tablets”. Indian Journal of Pharmaceutical Science, July-Aug-2005, 67(4):

479-480

13. M.Gandhimati. et al,”Validated HPLC method for simultaneous estimation of

Ofloxacin and Ornidazole in tablet dosage form”. Indian Journal of

Pharmaceutical Science, Nov-Dec-2006, 68(6): 838-840

14. Halkar Uma P. et al, “RPHPLC determination of Ofloxacin and Tinidazole in

tablet dosage forms”. Indian Drugs, Dec-2000, 37(12): 585-588

15. Gupta K.R. et al,”HPTLC estimation of Ofloxacin and Tinidazole from

pharmaceutical dosage form”. Indian Drugs, March-2004, 41(3): 160-164

16. Nagori B.P. et al, “Spectrophotometric method for simultaneous estimation of

Ofloxacin and Ornidazole in tablet dosage form” Indian Drugs, Aug-2006, 43(8):

676-678

17. A.H.Beckett, J.B.Stenlake, Practical Pharmaceutical chemistry, Fourth edition

2004, Part-2: 284-289

9 / Signature of the candidate
10 / Remarks of the Guide / Topic selected for Dissertation work is satisfactory.
This can be carried out in our Laboratory.
11 / Name and Designation of
(In Block Letters)
11.1  Guide
11.2  Signature / Dr. M.H.HUGAR, M.Sc, Ph.D.,
PROFESSOR
DEPT.OF QUALITY ASSURANCE
LUQMAN COLLEGE OF PHARMACY
GULBARGA-585102.
KARNATAKA.
11.3  Co – Guide
(If any)
11.4  Signature
12 / 12.1  Remarks of the Chairman and Principal
12.2  Signature / The selected topic is satisfactory.
The dissertation work is feasible in our laboratory.

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