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1. DEVELOPMENT & VALIDATION OF UV
SPECTROPHOTOMETRIC METHOD FOR
DETERMINATION OFATENOLOL
Submitted by
Mr. SIPU KUMAR SAHU
B. Pharm, 8th semester
(Regd.No. 1803267085)
Under the guidance of
Mr. SATYAJEET BEHERA
(Asst. Professor)
Dept. of Pharmaceutical analysis
ROLAND INSTITUTE OF PHARMACEUTICAL SCIENCES,
KHODASINGI, BERHAMPUR-760010, ODISHA.

2. INTRODUCTION
UV-Visible spectrophotometry:
This is one of the most frequently
employed technique in pharmaceutical
analysis. It involves measuring the
amount of ultraviolet or visible
radiation absorbed by a substance in
solution.

3. ATENOLOL:
Introduction:
Atenolol (Tenormin) is a selective B1 receptor
antagonist, a drug belonging to the group of beta
blockers (sometimes written f-blockers), a class of
drugs used primarily cardiovascular diseases.

4. DRUG PROFILE OF ATENOLOL
Atenolol: Atenolol is a beta blocker medication primarily used to treat high blood
pressure and heart-associated chest pain. Atenolol, however, does not seem to improve
mortality in those with high blood pressure. Other uses include the prevention of
migraines and treatment of certain irregular heart beats.
Molar mass: 266.33 g/mol
Formula: C14H22N2O3
Metabolism: Liver
Protein binding: 3%
Common side effects.
• Feeling sleepy, tired or dizzy. As your body gets used to atenolol, these side effects
should wear off.
• Cold fingers or toes. Put your hands or feet under warm running water,
massage them and wiggle your fingers and toes.
• Feeling sick or being sick (nausea or vomiting).
• Diarrhoea.
• Stomach pain.

5. AIM AND OBJECTIVE
According to literature survey it was found that, there are four
spectrophotometric determinations were reported for estimation of Atenolol
by chemical derivatisation involving methanol water mixture methyl orange
and thymol blue in acidic and basic medium.
Further only one method is present which estimated the amount of
Atenolol in pharmaceutical dosage form. Hence the objective of the
present work is to develop simple and accurate method for the
determination of Atenolol in bulk and tablet dosage form using UVvisible
derivative spectroscopy.

6. MATERIALS
MATERIALS –
 Pure atenolol,
 three commercially available tablets were
purchased from the local market
 distilled water
 In addition to instruments like UV-Vis
spectrophotometer

7. METHODS
METHOD-
UV - VISIBLE SPECTROPHOTOMETRIC METHOD
Spectrophotometry is generally preferred especially by small scale
industries as the cost of the equipment is very less and maintenance
problems are minimal. The method of analysis is based on measuring the
absorption of a monochromatic light by a colorless compounds in the
near ultraviolet-visible part of spectrum(200-800 nm).The photometric
method of analysis is based on the Bouger-Lamberts-Beer's law. Which
establishes the absorbance of a solution is directly proportional to the
concentration of the analyte.
METHOD VALIDATION:
Method validation can be defined as (ICH)
Method validation is an integral pat of method development it is the
process of demonstrating that analytical procedures are suitable for their
intended use and that support the identity. quality, purity and potency of

8. EXPERIMENT
NEW SPECTROPHOTOMETRIC DETERMINATION OF
ATENOLOL IN BULK AND CAPSULES:
A simple, sensitive, accurate and rapid UV spectrophotometric method
has been developed in methanol for the estimation of Atenolol in
pharmaceutical dosage form. This was found to be at 224 nm. It obeys BeerLambert's law in the
concentration range of 1.0 - 30 pg/ml. The method was
validated with precision and accuracy studies according to ICH guidelines.
EXPERIMENTAL :
Instrumentation:
Spectral and absorbance measurements were made on a Shimadzu-1800
double beam UV-visible spectrophotometer by using | cm quartz cells. Afcoset
ER 200A electronic balance was used for weighing the samples. Commercially
available pharmaceutical dosages forms of Atenolol were procured from the
local market and estimated.
Reagentused-Methanol

9. OPTIMIZATION:
Scanning and determination of maximum wavelength (λmax):
In order to ascertain the wavelength of maximum absorption (λmax) of the
drug.
different solutions of the drags (10µ/ml and 20 µg/ml) ln Methanol were
scanned using spectrophotometer within the wavelength region of 200 -
400
am against Methanol as blank. The resulting spectra were shown in fig: | and
the absorption curve showed characteristic absorption maxims at 224 nm
for
Atenolol .
Instrument: Shimadzu 1800 double beam UV visible
spectrophotometer

10. METHOD
Preparation of Stock Solutions:
Standard stock solution was prepared by dissolving 25 mg of each drug
in 25
ml Methanol of to get concentration of 1mg/mi (1000 µg/ml) solutions .
Preparation of Working Standard Solutions and construction of standard
graph:
The prepared stock solution was further diluted with Methanol to get
working
standard solutions of 0.1 g/ml and 100 mg/mi of Atenolol to construct
Beer's
law plot for pure drug, different aliquots of Atenolol were taken and
diluted to
10 mi with Methanol. The absorbance was measured at 224 nm ( maxima

11. Table 2: Linearity

12. Table 3: Optical Characteristic

14. Method:
For analysis of commercial formulations, 20 tabs were accurately
weighed the
contents of the capsule were taken. The powder equivalent to 10 mg
of
Atenolol was taken in a 100 mi volumetric flask, containing 70 ml of
Methanol
and sonicated for 30 minutes. The volume was made up to 100 mi
with
Methanol and filtered to get a solution of concentrations 100 pg/ml.
This was
further diluted with Methanol to get a concentration within the
linearity range
and the absorbances were measured against the blank at 224 nm and
the

15. VALIDATION:
Precision:
The precisi precision of the proposed method was ascertained by actual determination of eight
replicates of fixed concentration of the drug within the Beer’s range and finding out the
absorbance by the proposed method. From these absorbances, Mean, Standard deviation, %
RSD was calculated.

16. Accuracy:
To determine the accuracy of the proposed method, recovery
were carried out by adding different amounts (80%, 100%, 120%) of bulk
samples of Atenolol within the linearity range Were taken and added to
the pre-analyzed formulation of concentration !0ug/ml. From that
Percentage recovery values were calculated.

17. RESULTS
From the optical characteristics of the proposed method, it was found that
mesalamine obeys linearity within the concentration range of 1-100 g/ml.
From the results shown in Table 5, it was found that the % RSD is 0.149 which
is less than 2 %, which indicates that the method has good reproducibility.
From the results shown in accuracy Table 6, it was found that the percentage
recovery values of pure drug from the preanalyzed solution of formulation
were in between 97-103 %. which indicates that the proposed method is
accurate and also reveals that the commonly used excipients and additives in
the pharmaceutical formulations were not interfering in the proposed method.

18. CONCLUSION
The proposed method was simple, sensitive and reliable with
good precision and accuracy. The proposed method is specific while
estimating the commercial formulations without interference of
excipients and other additives. Hence, this method can be used for
the routine determination of Atenolol in pure samples and
pharmaceutical formulations.

19. REFERENCES
 R.Brent Miller A validated high-performance liquid chromatographic method for the determination of
Atenolol in whole blood.
 Alaa EL-Gindy , et al HPLC and chemometricassisted spectrophotometric methods for simultaneous
determination of atenolol, amiloride hydrochloride and chlorthalidone.
 A,P. Argekar, et alSimultaneous determination of atenolol and amlodipine is tablets by hghperformance
thin-layer chromatography, Journal of Pharmaceutical and Biomedical Analysis.
 AV Kasture, et al Simultaneously UV - Spectrophotometric method for the estimation of atenolol and
amlodipine bestlate in combined dosage form,
 Sanjay Bari, et al Spectrophotometric method for simultaneous estimationof atenolol in combination
with losartan potassium and hydrochlorothiazide in bulk and tablet formulation
 Gantala Venkatesha, et al Development and validation of RP-HPLC-UV method for simultaneous
determination of buparvaquone, atenolol, propranolol, quinidine and verapamil

20. THANK YOU