Validation of UV Spectrophotometric Method For Determination of Atenolol

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Validation of UV spectrophotometric method for determination of atenolol
Article · March 2014
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Shoaeb Mohammad Syed

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Research Article
Validation of UV Spectrophotometric Method for

Determination of Atenolol
SHOAEB SYED ∗, MUBASHIR MOHAMMED
Research Scholor Y B Chavan College of Pharmacy, Dr. Rafiq Zakaria Campus Rauza bagh, Aurangabad 431 001, India.
ABSTRACT
A rapid and sensitive UV spectrophotometric method for routine evaluation of atenolol in tablets was developed
and validated as per ICH guidelines. UV spectrophotometric method was performed at 226.6 nm, and samples
were prepared with a solution of phosphate buffer pH 6.8. The linearity demonstrated a correlation coefficient
of 0.9988, various validation parameters like accuracy, precision, LOD, LOQ, recovery study, range were
determined The proposed method was simple, rapid, precise, accurate and sensitive, and can be used for the
routine analysis of atenolol.
Key word: Atenolol, UV spectrophotometry, validation.
INTRODUCTION official methods and with other methods published. The

UV spectrophotometric method is simpler than the oth-
Atenolol, designated chemically as (RS)-4-(2hidroxy-3- ers studied because it does not need derivative and
isopropylaminopropoxy) phenylacetamide, is commer- chemometric assistance. Moreover, this method can be
cially available as a racemic mixture (Fig. 1), it is found used in dissolution studies because it uses its own dis-
in the form of tablets, oral solution, and sterile solution solution medium as diluent.
for injectable. Atenolol (ATN) is a β1 selective (cardiose-
lective) β-adrenergic receptor-blocking agent without
membrane-stabilizing or intrinsic sympathomimetic
(partial agonist) activities [1]. ATN is also used to treat
myocardial infarction (heart attack), arrhythmias
(rhythm disorders), angina (chest pains), and disorders
arising from decreased circulation and vascular con-
striction, including migraine [2] In the European Phar-
macopoeia [3], the described method for atenolol quan- Figure 1: Structure of atenolol
tification uses technique of titration with perchloric acid.
In the British Pharmacopoeia [4] the indicated methods MATERIALS AND METHODS
use spectrophotometric in the ultraviolet at 275 nm. The
UV spectrophotometric method is very simple, rapid, Instrumentation
economical, and it allows the determination in pharma- An UV-Visible double beam spectrophotometer (Varian
ceuticals with enough reliability. For the UV spectropho- Cary 100) with 10 mm matched quartz cells was used
tometric method, the survey of literature revealed very for Spectrophotometric method. All weighing were done
complex methods, using bands of the visible which on electronic balance (Model Shimadzu AUW-220D).
have used complexometry [5], derivative or chemomet- Spectroscopic grade methanol was used throughout the
ric assistance and interpolation on the calibration curve study. Ultrasonicator (Model 5.5 150H) was used for
[5]. The aim of this work was the development and fully sample solution preparation.
validation of a new UV spectrophotometric method,
which can be more economical and simpler than the Reagents and chemicals
∗Address for correspondance

Shoaeb Syed, Research Scholor Y B Chavan College of Pharmacy, Dr. Rafiq Zakaria Campus Rauza bagh, Au-
rangabad 431 001, India.
E-mail address: [email protected], Phone: +91-9730572605
Received: 12/11/2013, Revised: 30/11/2013, Accepted: 10/12/2013
International Journal of Pharmaceutical Research | January-March 2014 | Volume 6 | Issue 1 | 25

Syed & Mohammed / Validation of UV spectrophotometric method for determination of atenolol
Pure drug sample of atenolol was kindly supplied asa Where, S is slope of the calibration curve and σ is the
gift sample by WOCKHARDT LIMITED Waluj Aurangabad. residual standard deviation
Tablet formulation manufactured by Zydus cadilla In-
dustries was purchased from local market containing Recovery Study
ATEN 50 Containing atenolol 50 mg per tablet. Accuracy of the method was studied by recovery exper-
iments. The recovery was performed at three levels,
Preparation of standard stock solution 80,100 and 120% of atenolol standard concentration.
Standard drug solution of Atenolol was prepared by dis- The recovery samples were prepared in a before men-
solving 100 mg in phosphate buffer pH 6.8 and the vol- tioned procedure. Three samples were prepared for
ume was made up to 100 ml to obtain stock solution of each recovery level. The solutions were then analyzed
1000 µg/ml concentration. Ultrasonication was done to and the percentage recoveries were calculated from the
obtain a clear solution. calibration curve.
Determination of analytical wavelength RESULTS AND DISCUSSION
From the standard stock solution, 0.1 ml was pipette
Precision
out into 10 ml volumetric flask. The volume was made
up to 10 ml with phosphate buffer solution of pH 6.8. Precision of method was evaluated for atenolol. The
The resulting solution containing 10µg/ml was scanned reproducibility (inter-day precision) of the method and
between 200 and 400 nm. repeatability (intra-day) was evaluated in the same la-
boratory. The relative standard deviation (RSD) values
Preparation of Calibration curve of Atenolol obtained were 0.1973 and 0.2569 respectively (Table
in PBS pH 6.8 1).
Aliquots of 0.1 to 0.6 ml portion of stock solutions were
transferred to a series of 10 ml volumetric flasks, and Table 1: Precision determination
volume made up to the mark with phosphate buffer pH
6.8. The serial dilution of the range of 10, 20, 30, 40, Intra-Day Inter-Day
Sample no.
50, and 60 µg/ml was prepared. The absorbance was Precision* Precision*
measured at λmax 226.6 nm.
1 99.98 98.71
UV Method Validation
2 99.85 98.52
Linearity and range
The linearity of the response of the drug was verified at 3 99.65 98.65
10 to 60 µg/ml concentrations. The calibration graphs
were obtained by plotting the absorbance versus the Mean ± SD 99.68 ± 0.0026 98.62 ± 0.0020
concentration data and were treated by linear regres- %RSD 0.2569 0.1973
sion analysis. The equation of the calibration curve for *mean values of three determination
atenolol obtained. The linearity range of calibration
curve and correlation coefficient (r2) of determination Accuracy (Recovery Study)
was obtained. Accuracy of the method was studied by recovery exper-
iments. The recovery was performed at three levels,
Precision 80,100 and 120% of atenolol standard concentration.
The accuracy of the method was determined by recov- Three samples were prepared for each recovery level.
ery experiments. Each solution was recorded in tripli- The solutions were then analyzed and the percentage
cate and the percentage recovery was calculated. The recoveries were calculated from the calibration curve.
precision of the method was demonstrated by intra-day The recovery value for atenolol is 99.21±0.275 and RSD
and inter-day variation studies. In intra-day studies, is 0.321which is less than 2, which shows that the
three repeated measurements of standard and sample method has good reproducibility (Table 1).
solutions were made in a day and percentage RSD were
calculated. In inter-day studies, three repeated meas- Limit of detection (LOD) and Limit of quan-
urements of standard and sample solutions were made tification (LOQ)
on three consecutive days and percentage RSD were Limit of detection and Limit of quantification was found
calculated. to be 0.2586 and 0.7788 respectively.
Limit of detection (LOD) and Limit of quan- Specificity
tification (LOQ):
Specificity is the ability of the method to accurately
LOD and LOQ were calculated by the equations; measure the analyte response in the presence of all
LOD = 3.3σ / S and LOQ = 10σ / S potential sample components (excipients). The results
were compared with the analysis of a standard atenolol
26 | International Journal of Pharmaceutical Research | January-March 2014 | Volume 6 | Issue 1

Syed & Mohammed / Validation of UV spectrophotometric method for determination of atenolol
and tablet formulations. Excipients of the solid dosage

form did not interfere with the analyte (Table 2). ACKNOWLEDGEMENT
CONCLUSION We are thankful to Padmashree Mrs Fatema Rafiq Za-
karia for providing infrastructure and facilities for carry-
UV method was validated for atenolol as per ICH guide- ing out the work. We are also thankful to WOCKHARDT
lines. The proposed UV spectrophotometric method is LIMITED Waluj Aurangabad for providing atenolol as gift
simple, sensitive, accurate, precise and cost effective sample.
and hence can be used for the routine analysis of
atenolol in bulk, tablet formulations and for dissolution REFERNCES
studies.
1. The Indian Pharmacopoeia Commission. Indian
Table 2: Validation parameter pharmacopoeia Ministery of Health and Family
Welfare. Government of India, New Delhi. 2007;
Parameter Result 144,257,747
Absorption maxima
226.6 2. The United States Pharmacopoeia National
(nm) Formulary U.S. Pharmacopeial convention Inc.,
Linearity range (µg/ml) 10-60 Rockville, MD. 2009, 27, 1956-57.
Standard regression
y = 0.032x + 0.019 3. European Pharmacopoeia, Council of Europe,
equation (y) France. 2005(5); 1 and 2.
Correlation coefficient
0.998 4. British Pharmacopoeia, London: The stationary
(r2 )
office, 1988; (1): 49.
Slope (m) 0.032
5. Weich A., Oliveira D. C., Melo J., Goebel K., Rolim
Y-Intercept(c) 0.019
C. M. B., Validation of UV Spectrophotometric and
Accuracy (% recovery
99.21 ± 0.275 HPLC Methods for Quantitative Determination of
± SD)
Atenolol in Pharmaceutical Preparations, Latin
Precision
99.68 % ± 0.0026 (Intra-day) American Journal of Pharmacy, 2007; 26 (5): 765-
98.62 % ± 0.0020 (Inter-day)
70.
A 10 µg/ml sample of std. at 6. Bhatia N.M, Mohite A.S, Bhatia M.S., Simultaneous
Specificity absorbance 226.6 nm, spectrophotometric estimation of atenolol and
99.21% ± 0.27 amlodipine besylate by multi-wavelength method,
LOD (µg/ml) 0.2586 The Indian Pharmacist, 2007; 6(59): 59-62.
LOQ (µg/ml) 0.7788 7. Kasture A.V., Ramteke M., Simultaneous UV
spectrophotometric method for the estimation of
atenolol and amlodipine besylate in combined
dosage form, Indian Journal of Pharmaceutical
Sciences, 2006; 68(3):394.
8. ICH Harmonized Tripartite Guideline, ICH Q2(R1)
(Oct 1994), Validation of analytical procedures:
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9. Saminathan J., Vetrichelvan T., Validation of UV
Spectrophotometric Method for Determination of
Riluzole in Pharmaceutical Dosage Form,
International Journal of Chem. Tech. Research,
Figure 2: U.V. Spectrum of Atenolol at λmax = 2011; 3(2):560-564.
226.6 nm 10. Aarelly K., Bheemanapally K., Kumar M., Nerella R.,
Validated UV-spectrophotometric method for the
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y = 0.032x + 0.019 estimation of naftopidil in bulk and tablet formulation,
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2 R² = 0.9988 Scholars Research Library Der Pharmacia Lettre,
b 2013; 5(1):1-7.
s 1 11. Vijaya Lakshmi N., Koteswara Rao G. S. N., Roja
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0 20 40 60 Validation of UV Spectrophotometric Method for the
Concentration µg/ml Estimation of Finasteride in Tablets, International
Journal of Pharma Sciences, 2013; 3(1):123-125.
Figure 3: Calibration curve of Atenolol
International Journal of Pharmaceutical Research | January-March 2014 | Volume 6 | Issue 1 | 27
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See discussions, stats, and author profiles for this publication at: https://www.researchgate.

Validation of UV spectrophotometric method for determination of atenolol

Article · March 2014

Shoaeb Mohammad Syed

Osmotic Drug Delivery System View project

Gastroretentive Drug Delivery System View project

The user has requested enhancement of the downloaded file.

Validation of UV Spectrophotometric Method for

Key word: Atenolol, UV spectrophotometry, validation.

INTRODUCTION official methods and with other methods published. The

∗Address for correspondance

International Journal of Pharmaceutical Research | January-March 2014 | Volume 6 | Issue 1 | 25

26 | International Journal of Pharmaceutical Research | January-March 2014 | Volume 6 | Issue 1

and tablet formulations. Excipients of the solid dosage

International Journal of Pharmaceutical Research | January-March 2014 | Volume 6 | Issue 1 | 27

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