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UV Spectrophotometric UV Spectrophotometric Method Development Method Development And Estimation of And Estimation of

BicalutamideBicalutamide in in Pharmaceutical Dosage Pharmaceutical Dosage

FormForm

ContentsContents

• Introduction• Aim & Objective• Drug Profile• Experimental Methods• Validation• Result & Discussion• Conclusion

IntroductionIntroduction• 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 Analytical methods are developed according to ICH guidelinesto ICH guidelines

Quality assurance is the process of verifying or Quality assurance is the process of verifying or determining whether products or services determining whether products or services meet or exceed customer expectations. Quality meet or exceed customer expectations. Quality assurance is a process-driven approach with assurance is a process-driven approach with specific steps to help define and attain goals. specific steps to help define and attain goals. This process considers design, development, This process considers design, development, production and service.production and service.

Quality assurance demonstrates that the drug Quality assurance demonstrates that the drug is 'FIT FOR USE' and can satisfy its consumers is 'FIT FOR USE' and can satisfy its consumers by lessening its defects and improving its by lessening its defects and improving its

usability and performanceusability and performance. .

Aim & ObjectiveAim & Objective• The aim of our project is to develop UV

Spectrophotometric method of Bicalutamide

• Under this method our objective is to 1. find λmax2. Find calibration curve3. Validation &4. Quantification

• 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 ProfileDrug 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 massMolecular mass : :430.373g/mol430.373g/mol

PkaPka : :Approx 12Approx 12

SolubilitySolubility : Practically insoluble in water, slightly : Practically insoluble in water, slightly soluble in chloroform, and absolute ethanol, soluble in chloroform, and absolute ethanol, sparingly soluble in methanol, and soluble in sparingly soluble in methanol, and soluble in acetone and tetrahydrofuran.acetone and tetrahydrofuran.

Bioavailability :Bioavailability :well absorbedwell absorbed

Routes :Routes :OralOral

MethodologyMethodologyUV 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 The choice of solvent is governed by the solubility of the absorbing substance and by the absorption of of the absorbing substance and by the absorption of the solvent at the given wavelengththe 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 MethodsExperimental Methods• Instrument SYSTRONICS UV-VIS Double Beam Spectrophotometer 2201

• Methodology Adopted• 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 Spectral characteristics of Bicalutamide R.SBicalutamide R.S

• Multiple wavelength analysis of Bicalutamide R.S from 400 - 190 nm, shows maximum absorption at 276nm.

• ie. Λmax = 276nm

Calibration curve of Calibration curve of Bicalutamide 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 Bicalutamideug/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 The data reveals that Beer's law is obeyed between is obeyed between

concentration range of 5-30 concentration range of 5-30 ug/ml.ug/ml.

Above 45 ug/ml the absorbance Above 45 ug/ml the absorbance value was found to be very high value was found to be very high

Y = 0.042286X + 0.11Y = 0.042286X + 0.11 Correlation coefficient =0.999Correlation coefficient =0.999standard deviation =0.39502 standard deviation =0.39502 standard error was 0.01465standard error was 0.01465

CALIBERATION CURVE

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

5 10 15 20 25 30

Concentration(ug/ml)

Ab

so

rban

ce

Validation of the Validation of the proposed methodproposed method

• Accuracy• Repeatability• LOD and LOQ• Linearity• Range

AccuracyAccuracy

• 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.

RepeatabilityRepeatability

• 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 LOQLOD 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 The limit of quantificationlimit of quantification (LOQ) is (LOQ) is defined as the lowest concentration of the defined as the lowest concentration of the standard curve that can be measured with standard curve that can be measured with

an acceptable accuracy, precision, and an acceptable accuracy, precision, and

variability.variability. LOQ = 10s/mLOQ = 10s/m

And was found to be 7µg/mlAnd was found to be 7µg/ml

LinearityLinearity

• 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