SPECTROSCOPIC METHOD DEVELOPMENT FOR LOSARTON POTASSIUM IN TABLET By Ninad M. Phadke
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Transcript of SPECTROSCOPIC METHOD DEVELOPMENT FOR LOSARTON POTASSIUM IN TABLET By Ninad M. Phadke
“SPECTROSCOPIC METHOD DEVELOPMENT FOR LOSARTON
POTASSIUM IN TABLET”
A project report in Pharmaceutical Analysis By
Ninad .M.Phadke
Under the guidance of :Mrs. Dabhade M.P.
(M.PHARM)
S.N.D. COLLEGE OF PHARMACY,YEOLA
INTRODUCTION TO ANALYTICAL CHEMISTRY “Analytical chemistry deals with methods for determining
the chemical composition of samples of matter.” The drug or dosage form for human use must have
excellent quality and purity, free from any impurity, because these dosage forms directly affects the life, hence their analysis is important which is carried out using analytical methods.
The analytical method development for new API and dosage form involves development and validation of method for testing those API and dosage form in QC laboratories routinely as part of regular Quality control sample testing using the methods of Analytical Chemistry.
Analytical Chemistry involves two branches Qualitative and Quantitative.
BRANCHES OF ANALYTICAL CHEMISTRY
QUALITATIVE ANALYSIS : Qualitative analysis deals with the identification of elements, ions or compounds present in a sample.
QUANTITATIVE ANALYSIS : Quantitative analysis deals with the determinations of how much of one or more constituents are present.
Classification of Analytical Methods
A) CLASSICAL METHODS: For classical qualitative analysis the separated compounds were treated with
reagents that could be recognized by either color, by their boiling or melting points, their
solubility in a series of solvents or their optical activities.
Advantages of Classical Methods:
• Procedure is simple and accurate.• The equipment needed is cheap.• Methods are based on absolute measurements.• Specialized training is not required.
Limitations of Classical Methods:
• Chemical environment is critical.• There is a lack of versatility.• There is a lack of specificity.• Accuracy decreases with decreasing amount.
B) INSTRUMENTAL METHODS :
Measurements of physical properties of analyte such as conductivity, electrode potential, light absorption or emission, mass to charge ratio and fluorescence forms the basis of Instrumental Qualitative Analysis .
Advantages of Instrumental Methods:
Small Samples can be used. High sensitivity is obtained. Measurements obtained are reliable. The determination is very fast. Complex samples can be handled.
Limitations of Instrumental Methods:
Skilled person is required. The sensitivity and accuracy depends on the instruments or wet
chemical methods. Cost of equipment is high. Sizable space is required.
APPLICATIONS OF ANALYTICAL CHEMISTRY
In medicine, analytical chemistry is the basis for clinical laboratory tests, which helps physicians, in diagnosis of various diseases and better recovery of patients.
In industry, it provides the means of testing raw materials and for assuring quality of finished products, like fuel, paints, and other pharmaceuticals products .
Suspected environmental contaminant testing is great achievement by analytical chemistry.
PRINIPLE OF UV VISIBLE SPECTROSOPY
The ultraviolet-visible spectroscopy is a common analytical technique for qualitative and quantitative analysis of solid, liquid or gas samples
The intensity of the absorbance is detected by Beer-Lambert’s law.
Lambert’s Law: At a given concentration (C) of a homogenous absorbing system the intensity of transmitted light decreases exponentially with increasing path length.
-dI / dT = KI Beer’s Law: For a layer of defined path length the intensity of
transmitted light decreases exponentially with increase in concentration (C) of a homogenous absorbing system.
It = Io e –ac
The combination of these laws gives the Beer-Lambert Law,
Log Io/ It = A = abc
Where, A = Absorbance of the solution at a particular
wavelength. Io = Intensity of the light beam.
It = Intensity of beam after passing through solution.
a = Absorptivity of molecule at the wavelength of beam. b = Path length of cell in cm. c = Concentration of solution in gm/lit.
CHOICE OF SOLVENT
SolventMinimum wavelength
( nm )
Acetonitrile 190
Water 190
Cyclohexane 195
Hexane 200
Methanol 200
Ethanol 200
Ether 215
Methylene chloride 220
chloroform 240
Carbon tetrachloride 257
Methods Of Quantitative Spectrophotometric Assay of Medicinal Substances
The concentration of a single component in a sample may be determined by a simple Spectrophotometric methods of absorbances, provided that the other components have a sufficiently small absorbance at the wavelength of measurements.
The single component & multicomponent mixture containing the API can be analyzed by either of following method :
Simultaneous equation method. Multicomponent analysis. Absorption ratio method.
The assay of an absorbing substance may be quickly carried out by preparing solution in a transparent solvent and measuring its absorbance at a suitable wavelength {i.e.maximum absorption (λmax)}.
INSTRUMENTATION OF U.V.
Diagram of double beam UV Spectrophotometer
An instrument for measuring the absorption of UV or visible radiation contains following important components :
Source of light –Hydrogen or deuterium lamp, tungsten lamp.
Prism or Gratings monochromator.Sample container-Quartz cuvettes.DetectorsSignal processor and readout.
Applications of UV-Visible SpectroscopyIdentification of various organic, inorganic
molecules and ions by matching their spectrum with reference spectra.
For qualitative and quantitative analysis of drugs in pharmaceutical industry.
Monitoring of reaction rates (chemical kinetics)Enzyme assaysEnvironmental remote sensingUsed as detectors in various systems like HPLC,
electrophoresis etc.
STEP BY STEP PROCEDURE FOR UV –VISIBLE SPECTROSCOPIC ANALYSIS OF DRUG
Literature Review Objective Of Work Plan Of Work Experimental Work Results and discussionMethod Validation Conclusion
PLAN OF WORKLosarton Potassium
Calibration Of Apparatus
Calibration Of UV Instrument
Selection of suitable solvent
Determination of max
Calibration curve
Estimation of drug from tablet formulation
Recovery studies
Result and conclusion
OBJECTIVE OF WORK
The objective of this investigation was to devise simple, precise, rapid and economical method for the estimation of Losarton Potassium in bulk drug and the tablet formulation.
Tablets procured from the market were analyzed by the proposed method. In this method, the tablets were crushed and dissolved in solvent and diluted further. Sufficient amounts of the samples were withdrawn and their absorbances were noted at 238.4 nm against reagent blank.
Optical characteristics and precision
Absorption
maxima(nm)
238.4nm
Absorption maxima(nm) 238.4nm
Beer’s law limit (g/ml) 03-30µg/ml
Correlation coefficient(r2) 0.9871
Regression equation 0.0154x + 0.0198
TABLET ANALYSISSR. NO. Amt taken in
(g/ml)
Amt found in
(g/ml)
Amt found in
%
1. 18 17.99 99.94
2. 18 18.01 100.05
3. 24 23.99 99.95
4. 24 24.01 100.04
5. 30 29.99 99.96
6. 30 30.01 100.03
Statistical validation of tablet formulation
Amt
found in
(%)
MEAN Standard
deviation
Coeffecie
nt of
variation
Standard
error
100.03 23.83 ± 0.15379 0.932 0.002124
Recovery study of Losarton PotassiumName of drug
Level
of
Perce
ntag
e
Reco
very
Conc
.
used
µg/
ml
Conc
.
adde
d
µg/
ml
Total
conc.
absor
banc
e
Conc.
Recov
ered in
µg/ml
%
Recov
ery
MEA
N
Losarton
Potassium
50 12 6 18 0.298 17.99 99.94 99.97
50 12 6 18 0.297 18.01 100.05
50 12 6 18 0.298 17.99 99.94
100 12 12 24 0.440 23.99 99.95 99.99
100 12 12 24 0.441 24.01 100.04
100 12 12 24 0.440 23.99 100.00
150 12 18 30 0.597 29.99 99.96 99.98
150 12 18 30 0.596 30.01 100.03
150 12 18 30 0.597 29.99 99.96
Statistical validation of recovery studies of tablet formulation
Level of
recovery
MEAN %
Recovery
Standard
Deviation
Coeffecien
t Of
Variation
Standard
Error
50 % 99.97
±0.076895 0.466 0.001062
100 % 99.99 ± 0.15379 0.932 0.002124
150 % 99.98 ±0.30758 1.864 0.004248
Statistical Results Of Analysis
Sr. No. Tablet Label
claim(mg)
S.D.* %Recover
y*
1. LOSAR 50 ±0.15379 99.98 %
Thus the statistical study was performed.The value obtained for S.D seemed to be within range. This showed the suitability of procedure.
METHOD VALIDATION
Linearity-Linearity was observed in the range of 03-30g/ml. The calibration curve yielded coefficient of correlation (r2) 0.9871.
Assay result- Losarton Potassium tablets of a marketed brand was analyzed by proposed methods, the percentage in tablet were determined and presented in the above table.
Accuracy and precision-The % Recovery was found to be in the range of 99.80-100.5%,indicates the non-interference from the formulation excipient and confirm the accuracy and precision of the method.
CONCLUSION
All the above result indicates that, the method employed here is a very simple, economical and can be used for routine analyses of the drug, Losarton Potassium.
The proposed method was found to be accurate, simple and rapid for routine analysis of the drug. The recovery was 100.43% (LOSAR) which is close to 100% indicating reproducibility and accuracy of the method.
References Govt. of India, Ministry of Health and Family Welfare. Vol. 2. Delhi:
Publication by Controller of Publication; 2007. Indian Pharmacopoeia;
pp. 484–554.
British Pharmacopoeia. (International ed.) 1993;Vol. 1:429, 483.
Published on the Recommendation of the Medicines Commissions
Pursuant to Medicines Act 1968, 1993.
Martindale, The Extra Pharmacopoeia, 33rd ed., Royal Pharmaceutical
Society, London, 2002; pp 921-922.
United States Pharmacopoeia 29 NF 24, Published on the
Recommendation of the Medicines Commissions Pursuant to Medicines,
page no. 587
Skoog, West, Holler, Crouch, “Fundamentals of analytical chemistry” ,
eighth edition, 2009 (Indian edition), cengage learning India pvt ltd ,
New delhi, pageno. 271-280.
A.V Kasture, K.R Mahadik, S.G Wadodkar, H.N. More, “A textbook of
pharmaceutical analysis, Instrumental methods” , Nirali Prakashan,
vol.2, 9th edition, page no. 5-7, 28-30
THANKING YOU