1. METHOD DEVELOPMENT AND VALIDATION OF
VERAPAMIL BY RP-HPLC
Under the guidance of
E.PUSHPALATHA REDDY M.Pharm
COLLEGE OF PHARMACY. N.H-7, CHINNATEKUR,
AIM AND OBJECTIVE
METHOD DEVELOPMENT STEPS IN RP-HPLC
INSTRUMENTATION OF RP-HPLC
VALIDATION PARAMETERS OF RP-HPLC
3. AIM AND OBJECTIVE OF STUDY
• To develop a simple accurate and precise method for
Verapamil in drug substances and drug product and to validate
the method as per ICH guidelines.
5. • DESCRIPTION: A calcium channel blocker that is a class IV
• SOLUBILITY: SOLUBLE IN WATER,METHANOL
• MECHANISM OFACTION: Verapamil inhibits voltage-
dependent calcium channels. Specifically, its effect on L-type
calcium channels in the heart causes a reduction in ionotropy
and chronotropy, thuis reducing heart rate and blood pressure.
Verapamil's mechanism of effect in cluster headache is thought
to be linked to its calcium-channel blocker effect, but which
channel subtypes are involved is presently not known.
7. LITERATURE SURVAY
1. iN-VITRO INTERACTION STUDIES OF VERAPAMIL WITH
FLUOROQUINOLONES USING FIRST ORDERDERIVATIVE UV
column: CLC-ODS (6.0 X 150 mm) column.
Mobilephase:mobile phase constituted of acetonitrile: water (45:55)
Flow rate: 1.2 mL min-1 at 230 nm
2.VALIDATION OF BIOANALYTICAL METHOD FOR VERAPAMIL BY HPLC
8. 3.METHOD DEVELOPMENT OF VERAPAMIL IN PRESENCE OF NSAIDS USING
Mobile phase:mobile phase constituted of acetonitrile: water (45:55)
9. METHOD DEVELOPMENT STEPS IN RP-HPLC
ANALYTICAL METHOD DEVELOPMENT:
• Method development usually requires selecting the method
requirements and deciding on what type of instrumentation to
utilize and why.
• The wide variety of equipment, columns, eluent and
operational parameters involved makes HPLC method
10. There are several reasons for developing new methods of
1. A suitable method for particular analyte in the specific matrix
is not available.
2. Existing methods may be too error or they may be unreliable
(have poor accuracy or precision)
3. Existing methods may be too expensive, time consuming.
11. HPLC method development generally follows the following
Step 1-selection of the HPLC method and initial system.
Step2-Selection of optimum conditions.
Step4-system parameter optimization.
14. VALIDATION PARAMETERS OF RP-HPLC
Typical validation characteristics which should be
considered are listed below:-
b. intermediate precision
4. Detection limit
5. Quantitation limit
1) Quality Assurance of Pharmaceuticals. A compendium of
guidelines and related materials, vol. 2, updated editing, Good
Manufacturing practices and inspection Geneva, World Health
2) Sharma B. K.,Instrumental methods of chemical analysis,
GOLE publishing house (2004),23.
3) Khopkar S. M., Basic concepts of analytical chemistry, New
age International Ltd. Publishers, New Delhi, (1998), 2, 178-
4) Settle F., Handbook of Instrumental techniques for analytical
chemistry, Prentice Hall PTR, NJ, (1997), 17-19, 56-57.
16. 5)Skoog D. A., F.J. Holler and S.R. Crouch, Principle Of
Instrumental Analysis, Thomson Publications, India, (2007), 6,
1-3, 145-147, 180.
6)Mendham J, R.C. Denney, J.D. Barnes, and M. Thomas,
Vogel’s Textbook of Quantitative Analysis. Pearson Education,
Singapore, (2003), 8-9.
7)Sharma B. K., Instrumental Methods Of Chemical Analysis,
Goel Publication Co., Meerut, (1983), 25, 3, 6.
8)Christian G. D., Analytical Chemistry, John Wiley and Sons,
(2003), 5, 35-42, 131-132.
9)Michael W. Dong,”Modern HPLC for practicing scientist” A
John Wiley & Sons, Inc., Publication, 194,217.