Transcript anu

WELCOME
UV Spectrophotometric Method
Development And Estimation of
Bicalutamide in Pharmaceutical Dosage
Form
Contents
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Introduction
Aim & Objective
Drug Profile
Experimental Methods
Validation
Result & Discussion
Conclusion
Introduction
• Quality Control (QC) is a
system of routine technical activities,
to measure, ensure and control the quality in a product or service . The
basic goal of quality control is to ensure that the products, services or
processes provided meet specific requirements and are dependable,
satisfactory and physically sound.
•
Quality Control is the implementation of regular test procedures to
satisfy consumer needs and to prevent drugs of lesser than claimed
therapeutic value from entering into the market.
• the analytical studies are important to find out the exact amount of
active pharmaceutical ingredients present in the dosage form .
Analytical methods are developed according to ICH guidelines
Quality assurance is the process of verifying or determining whether
products or services meet or exceed customer expectations. Quality
assurance is a process-driven approach with specific steps to help
define and attain goals. This process considers design, development,
production and service.
Quality assurance demonstrates that the drug is 'FIT FOR USE'
and can satisfy its consumers by lessening its defects and improving
its usability and performance
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Aim & Objective
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The aim of our project is to develop UV Spectrophotometric method of
Bicalutamide
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Under this method our objective is to
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find λmax
Find calibration curve
Validation &
Quantification
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Through this project, an attempt is being made to develop and validate
simple, sensitive methods which include spectrophotometry for
quantitative monitoring of Bicalutamide in pure as well as
pharmaceutical dosage forms.
Drug Profile
• Bicalutamide is in a class of medications called nonsteroidal
antiandrogens which works by blocking the effect of androgen (a male
hormone), to stop the growth and spread of cancer (Prostate Cancer ).
• Bicalutamide is a racemate and the (R)-enantiomer is primarily
responsible for its anti-androgenic activity.
Molecular mass :430.373g/mol
Pka :Approx 12
Solubility : Practically insoluble in water, slightly soluble in chloroform,
and absolute ethanol, sparingly soluble in methanol, and soluble in acetone
and tetrahydrofuran.
Bioavailability :well absorbed
Routes :Oral
Methodology
UV SPECTROPHOTOMETRIC METHOD
• Many molecules absorb ultraviolet light.Absorption methods based
on ultraviolet (UV) radiation(200-400 nm) find wide spread
application for the identification and determination of organic and
inorganic species.
• Absorbance is directly proportional to the path length, b, and the
concentration, c, of the absorbing species. Beer's Law states that
A = abc, where a is a constant of proportionality, called the
absorptivity
• By plotting absorbance, A, against concentration, a straight line will
be obtained. This calibration line may then be used to determine
unknown concentration of solutions of the same material after
measurement of absorbance
•The choice of solvent is governed by the solubility of the absorbing
substance and by the absorption of the solvent at the given wavelength
• The absorption of UV radiation corresponds to the excitation of outer
electrons which involves transitions of π ,σ and n electrons.
σ to σ* Transitions : Requires high energy and shorter wavelength
π to π* Transitions :Requires low energy and longer wavelength
Experimental Methods
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Instrument
SYSTRONICS UV-VIS Double Beam Spectrophotometer 2201
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Methodology Adopted
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Preparation of standard solution
study of spectral characteristics of Bicalutamide R.S in THF
Calibration curve of Bicalutamide R.S in THF by UV absorption method
Development of an analytical method using this calibration plot
Comparative study of commercially available dosage form with Bicalutamide R.S
Statistical evaluation of the calibration plot
stability profile
Validation of the method
Spectral characteristics of
Bicalutamide R.S
• Multiple wavelength analysis of Bicalutamide R.S from 400
- 190 nm, shows maximum absorption at 276nm.
• ie. Λmax = 276nm
Calibration curve of
Bicalutamide
• Prepared 10 sets of dilutions.
• Wavelength at 276nm was fixed.
• Absorbance were found by using single wavelength analysis.
• Calibration curve was plotted by taking Absorbance Vs Concentration
Sl No.
Concentration of Bicalutamide
ug/ml
Absorbance at 276nm
1
5
0.312
2
10
0.531
3
15
0.747
4
20
0.976
5
25
1.116
6
30
1.229
7
35
1.464
8
40
1.454
9
45
1.555
The data reveals that Beer's law is obeyed
between concentration range of 5-30 ug/ml.
Above 45 ug/ml the absorbance value was found to
be very high
CALIBERATION CURVE
1.6
Absorbance
1.4
1.2
1
0.8
0.6
0.4
0.2
0
5
10
15
20
Concentration(ug/ml)
Y = 0.042286X + 0.11
Correlation coefficient =0.999
standard deviation =0.39502
standard error was 0.01465
25
30
Validation of the proposed
method
• Accuracy
• Repeatability
• LOD and LOQ
• Linearity
• Range
Accuracy
• It expresses the closeness of agreement between reference
value and value found .
• Accuracy was evaluated by carrying out a recovery study.
• And the method was found to be accurate.
Repeatability
• Repeatability expresses the precision under same operating
conditions over a short interval of time.
• It is usually expressed as the closeness of agreement between
a series of measurements obtained.
• It is usually expressed as the standard deviation, variance, or
relative standard deviation of a series of measurements.
LOD and LOQ
• The limit of detection (LOD) is defined as the lowest
concentration of an analyte that can be detected.
• But not necessarily quantified as an exact value.
• LOD = 3s/m
• And was found to be 2µg/ml.
The limit of quantification (LOQ) is defined as the lowest
concentration of the standard curve that can be measured with
an acceptable accuracy, precision, and variability.
LOQ = 10s/m
And was found to be 7µg/ml
Linearity
• The linearity of an analytical procedure is its ability to obtain
test results, which are directly proportional to the
concentration of the analyte in the sample.
• The calibration curve of Bicalutamide by the proposed
method was found to be linear over the range of 5-30 µg/ml