Dept.

Pharmceutical Analysis
Sri Sai Educational Society Group
of Gate school of
pharmacy,Ramapuram,Kodad.
 

analytical method development and validation for

rabaeprazole and itopride in combined pharmaceutical
dosage form by rp-hplc
 

PRESENTED By

Under the guidance of KUMAR RITESH 138B1R0077

MR .S.VIKRAM ANNU KUMARI 138B1R0071
REDDY.M.Pharm, CHANDAN KUMAR 138B1R0073
SIYARAM YADAV 138B1R0094
LOVELY KUMARI 138B1R0079
 CONTENTS
 INTRODUCTION
 LITARATURE REVIEW
 Aim and OBJECTIVE
 DruG profile
 Excipients profile
 Materials and methods
 RESULTS & DISCUSSION
 CONCLUSION
 BIBLIOGRAPHY
 INTRODUCTION
Analytical chemistry is a scientific discipline used to study
the chemical composition, structure and behaviour of matter.
The purposes of chemical analysis are together and interpret
chemical information that will be of value to society in a wide
range of contexts.

Quality control (QC) in many manufacturing industries, the

chemical composition of raw materials, intermediates and
finished products needs to be monitored to ensure
satisfactory quality and consistency

Analytical techniques There are numerous chemical or

physico-chemical processes that can be used to provide
analytical information.
.
 LITERATURE REVIEW
The present investigation describes about a
simple, economic, selective, accurate,
precise reverse phase high performance
liquid chromatographic method for the
simultaneous estimation of Rabeprazole
sodium
: and Itopride hydrochloride in pure
and pharmaceutical dosage forms.
Rabeprazole and Itopride .
Aim and objectives of RABEPRAZOLE AND
ITOPRIDE
The literature review reveals t few HPLC methods for the
estimation of Rabeprazole and Itopride alone and in combination with
other drugs.

 Few methods are also reported for estimation of both drugs from
formulation .

we intend to develop a Stability indicating RP-HPLC method by

simultaneous determination with simple, rapid, greater sensitivity and

faster elution.

 
 IUPAC

drugprofile
.

Name : 2-({[4-(3-methoxypropoxy)-3-methylpyridin-2-
yl]methane}sulfinyl)-1H-1,3-benzodiazole
Chemical formula : C18H21N3O3S

Molecular weight : 359.443

pKa : 9.35

Solubility : freely soluble in water,

Insoluble in acetone, ether, chloroform.
Category : Enzyme Inhibitors,Anti

-Ulcer Agents
 EXCIPIENT PROFILE
ITOPRIDE

IUPAC Name : N-({4-[2-

(dimethylamino)ethoxy]phenyl}methyl)-3,4-
dimethoxybenzamide
. Chemical formula : C20H26N2O4
Molecular weight : 358.4314 , Monoisotopic:
358.18925733
pKa : 8.77
Cas No : 122898-67-3
Category : Cholinesterase Inhibitor
 MATERIALS AND METHODS
S.N MATERIALS DISTRIBUTOR/
O MANUFACTURER

1. 1
Potassiumdihydrogenorthophosphate Merck
1. 2 Merck
Sodium perchlorate
1. 3 Merck
Perchloric acid
4
1. 5 Merck
Ortho phosphoric acid
1. 6 Merck
Methanol
1. 7 Merck
Acetontrile
8

0.45 µm Nylon filter Axivia

List of Equipments& Instruments
S.NO. INSTRUMENT NAME MODEL
WATERS, software: Empower,
1. HPLC system 2695 separation module. 2996
PDA detector.

2. Semi micro balance Sartorius ME235P

Lab India ph. meter
3. PH Meter

4. Sonicator Ultrasonic cleaner power sonic

420
5. UV/VIS spectrophotometer LABINDIA UV

6. Constant temperature water bath Thermolab GMP

High-Performance Liquid Chromatography [HPLC] System
 Method Development
optimized method parameters

Chromatographic conditions:
Flow rate : 1.0 ml per min
Column : Agilent C18 (4.6 x 150mm,
5m)
Detector wavelength : 254 nm
Column oven : Ambient
Injection volume : 10l
Run time : 6 min
 RESULTS AND DISCUSSION
Chromatogram Of Trial 1

 
Standard Chromatogram for Optimised Method
For Rabeprazole:
AT WS DT P Avg. Wt
Assay% = -------------- x ----------x--------- x ----------x-------------- X 100
AS DS WT 100 Label Claim
Where:
AT = average area counts of sample preparation.
As= average area counts of standard preparation.
WS = Weight of working standard taken in mg.
P = Percentage purity of working standard
LC = label claim of Rabeprazole mg/ml.
For Itopride:
AT WS DT P Avg. Wt
Assay% = -------------- x ----------x--------- x ----------x-------------- X 100
AS DS WT 100 Label Claim
Where:
AT = average area counts of sample preparation.
As= average area counts of standard preparation.
WS = Weight of working standard taken in mg.
P = Percentage purity of working standard
LC = label claim of Itopride mg/ml.
Assay Results: (Rabeprazole)
1250595 10 0.3 100 10 99.9 1754.5
------------ x ----------x --------- x -------- x------- x --------- x100 x --------- =99.83%
1251360 10 10 1754.5 0.1100 300
Assay Results:(Itopride)
928829 10 0.3 10010 99.8 1754.5
----------- x -------- x--------- x ----------x------- x -------- x --------- x100 =98.89%
937364 10 10 1754.5 0.1100 300
 Summary and Conclusion
•A new method was established for simultaneous
estimation of Rabeprazole and Itopride by RP-HPLC
method.
• The chromatographic conditions were successfully
developed for the separation of Rabeprazole and
Itopride by using Agilent C18 column (4.6×150mm)
5µ, flow rate was 1ml/min, mobile phase ratio was
(70:30 v/v) methanol: Phosphate buffer (KH2PO4and
K2HPO4) pH 3 (pH was adjusted with
orthophosphoricacid), detection wavelength was
254nm. The
instrument used was WATERS HPLC Auto Sampler,
Separation module 2695, photo diode array detector
 BIBLIOGRAPHY
• Dr. Kealey and P.J Haines, Analytical Chemistry, 1stedition, Bios
Publisher, (2002), PP 1-7.
• Andrea Weston and Phyllisr. Brown, HPLC Principle and Practice,
1st edition,
Academic press, (1997), PP 24-37.
• Chromatography, (online).
URL:http://en.wikipedia.org/wiki/Chromatography.

• Draft ICH Guidelines on Validation of Analytical Procedures

Definitions and terminology. Federal Register, vol 60. IFPMA,
.
Switzerland, (1995), PP 1126.
.
• Yuri Kazakevich and Rosario Lobrutto, HPLC for Pharmaceutical
Scientists,
1stedition, Wiley Interscience A JohnWiley & Sons, Inc., Publication
, (2007),   PP 15-23.