Development and Validation by Ashwini

8/6/2019 Development and Validation by Ashwini

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DEVELOPMENT AND VALIDATION OF

SIMPLE ANALYTICAL METHODS FOR THEESTIMATION OF MOXIFLOXACIN IN BULK

AND PHARMACEUTICAL DOSAGE FORM

UNDER THE GUIDANCE OF:

Dr.Ravindranath.

HOD,Pharmaceutical Analysis.

PRESENTED BY:

G.Ashwini

Regd no.100809885003

M. PHARM IN PHARMACEUTICALM. PHARM IN PHARMACEUTICALANALYSISANALYSIS

DISSERTATIONDISSERTATION

www.pharmacygraduates.org


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TABLE OF CONTENTSS.NO CONTENTS PAGE NO

Introduction 3-4

Drug profile 5-6

Objectives 7

Instrumentation 8-10

Methodology 11

conclusion

Reference 1



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Pharmaceutical analysis comprises the procedures necessary to

determine the identity, strength, quality and purity of substances

of therapeutic importance. Quality is important in every product or service, but it is vital in

medicines as it involves life.

Analytical techniques that are generally used for drug analysis are

o Chromatographic methods,

o Spectral methods,o Biological and Microbiological methods.

INTRODUCTIONINTRODUCTION



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Validation of Analytical Method

validation is the process used to confirm that the analytical

procedure employed for a specific test is suitable

for its intended use.The various validation parameters are:

Accuracy,

Precision (Repeatability and Reproducibility),

Linearity and Range,

Limit of detection (LOD) / Limit of quantitation (LOQ), Selectivity / Specificity,

Robustness / Ruggedness,

Stability and System suitability studies



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y Moxifloxacin is a fourth-generation synthetic fluoroquinolone antibacterial

agent

DRUG PROFILEDRUG PROFILE



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Nomenclature:1-cyclopropyl-7-[(1s,6s)-2,8-diaz[4.3.0]non-8-yl]-6-fluoro-8-

methoxy-4-oxo-quinoline carboxylic acid

Molecular formula : C21H24F N3O4.HCL. .

Molecular weight : 401.431 g/mol .

Appearance : It occurs as a Yellow to yellow crystalline substance

Solubility : It is soluble in methanol, sparingly soluble in water and

practically insoluble in acetone.

Category : Antibacterial agent.



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The Objective of this dissertation work is as follows

Aim of the present work is to Develop some new analytical methods for the

estimation of moxifloxacin in bulk and drug formulations

To Develop rapid, sensitive and selective method

Economic and accurate method

Method validation according to ICH guidelines.

OBJECTIVESOBJECTIVES



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INSTRUMENTATION HPLC is one mode of chromatography,

Chromatographic processes can be defined as separation techniques

involving mass-transfer between stationary and mobile phases.

HPLC utilizes a liquid mobile phase to separate the components of amixture.

These components (or analytes) are first dissolved in a solvent, and then

forced to flow through a chromatographic column under high pressure. In

the column, the mixture is resolved into its components.

As a result, HPLC acquires a high degree of versatility not found in otherchromatographic systems and has the ability to easily separate a wide

variety of chemical mixtures.



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BLOCK DIAGRAM OF HPLC:



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Selection of analytical wavelength

Preparation of stock solutions

Calibration curve for the Moxifloxacin

Sample preparation for determination of Moxifloxacin from dosage

form

Validation of Spectrophotometric methods

METHODOLOGYMETHODOLOGY

PART A: UV SPECTROSCOPYPART A: UV SPECTROSCOPY



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Gather / generate background information obtain Physico-chemical

properties,

Determine, if special handling / treatment of sample is needed,

From physic-chemical properties select detector,

Select LC mode and perform initial runs,

Optimize separation conditions; peak Rs , equation parameters,

Summarize methodology finalize documentation, Validate method / Transfer to control Laboratory.

PA RT B: HIGH PERFORMANCE LIQUIDPA RT B: HIGH PERFORMANCE LIQUID

CHROMATOGRAPHYCHROMATOGRAPHY



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Optimized Chromatographic Conditions for HPLCOptimized Chromatographic Conditions for HPLC

InstrumentHigh Performance Liquid Chromatography

( Agilent technologies 1200 series

with Eglite software)

Injector

Column

Wavelength

Flow rate

Injection volume

Mobile phase

Temperature

Run timewww.pharmacygraduates.org


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Reference

y Validated spectrophotometric methods for the estimation of moxifloxacin in

bulk and pharmaceutical formulations.

Motwani SK, Chopra s, Ahmad FJ, Khar RK.

Department ofPharmaceutics, Faculty ofPharmacy, Jamia Hamdard,Hamdard Nagar, New Delhi 110062, India. [email protected]

Validated spectrophotometric methods for the estimation of moxifloxacin in

bulk and pharmaceutical formulations

References and further reading may be available for this article.

Sanjay K. Motwani , Shruti Chopra Farhan J. Ahmad1 and Roop K. Khar1, a

aDepartment ofPharmaceutics, Faculty ofPharmacy, Jamia Hamdard,

Hamdard Nagar, New Delhi 110062, India



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y Optimization and validation of the direct HPLC method for the

determination of moxifloxacin in plasma Aleksandra Laban-Djurdjevia,

Milena Jeliki-Stankovb and Predrag Djurdjevi

aMedicines and Medical Devices Agency of Serbia, V. Stepe 458, 11152Belgrade, Serbia and MontenegrobFaculty ofPharmacy, V. Stepe 450,

11152 Belgrade, Serbia and MontenegrocFaculty of Science, P.O. Box 60,

34000 Kragujevac, Serbia and Montenegro

y Web sites:

www.pubmed.comwww.sciencedirect.com

www.google.com




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Development and Validation by Ashwini