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Pharmaceutical Analysis

Pharmaceutical Analysis. Dr. Manodeep Chakraborty. Introduction of spectroscopy. Study of interaction of the electromagnetic radiation with sample substance Absorption Emission . Divisions. Based on atomic or molecular level Atomic spectroscopy

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Pharmaceutical Analysis

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  1. Pharmaceutical Analysis Dr. Manodeep Chakraborty

  2. Introduction of spectroscopy • Study of interaction of the electromagnetic radiation with sample substance • Absorption • Emission

  3. Divisions • Based on atomic or molecular level • Atomic spectroscopy e.g. Atomic absorption spectroscopy, Flame photometry • Molecular spectroscopy e.g. UV spectroscopy Visible spectroscopy IR spectroscopy Fluorimetry

  4. Based on absorption or emission of the radiation • Absorption Spectroscopy e.g. UV spectroscopy Visible spectroscopy IR spectroscopy Atomic absorption spectroscopy • Emission spectroscopy e.g. Atomic emission spectroscopy Flame photometry

  5. Introduction to chromatography • Based on separation mechanism • Adsorption chromatography e.g. Thin layer, Column • Partition chromatography e.g. Paper 0 Normal phase : Stationary phase : Polar 0 Reverse phase Mobile phase : Non Polar • Ion exchange Cation exchange resins : Sulfonated poly styrenes, carboxylic methacrylate Anion exchange resins : Quaternary ammonium poly styrene, phenol formaldehyde

  6. Size exclusion : Gel permeation / Gel filtration • Zone electrophoresis • Affinity chromatography • Chiral chromatography • Based on the mobile phase used • Liquid chromatography : liquid/solid, liquid/ liquid • Gas Chromatography : Gas/solid, Gas/liquid • Based on the stationary phase holding technique • PlanarChromatography : TLC, PC • Columnar Chromatography : HPLC, GC, Column • Based on purpose • Analytical : Qualitative, Quantative • Preparative

  7. Solution Concentration • Normality: Numberof equivalents of solute/L W N = EWxV • Percent Concentration Mass of solute Percent w/w = x 100 Mass of solution

  8. Volume of solute Percent v/v = x 100 Volume of solution Mass of solute Percent w/v = x 100 Volume of solution

  9. Molar Concentration Number of moles of solute M = Volume of solution in litre

  10. Formal Concentration Weight of solute in g F = x Formula weight Volume of solution in litre • Equivalent weight: Equivalent weight in neutralization reactions Molecular weight Equivalent weight = Basicity Molecular weight Equivalent weight = Acidity

  11. Equivalent weight in complexation reactions Molecular Weight Eq. Wt. = Valency of reacting ions

  12. Primary and Secondary Standard • Primary Standard Conditions • Cheap, easily available, purify and dry, remain pure state for long, • Should not absorb moisture • Composition unchanged • Taste impurities by some common & simple tests • High relative molecular mass, so that weigh error may be negligible • Readily soluble • Reaction should be stoichiometric and practically instantaneous. • Error should be negligible or easy to determine accurately experimentally

  13. Acidimetry and alkalimetry Sodium Carbonate Na2Co3 Sodium tetraborate Na2B4O7 Potassium hydrogen pthalate Borax Na2B4O7.10H2O Potassium hydrogen iodate • Complex formation reactions Metals (Cu, Zn, Mg, Mn) and salts • Redox titrations Potassium dichromate, Potassium bromate, Potassium iodate • Precipitation titration KCL, AgNO3, NaCl

  14. Preparation, standardization and storage of various volumetric solution • Preparation • Direct weighing • Titration and standardization against standard solution • Storage • Alkaline substance: Plastic container • I2 & AgNO3 : Glass ( Dark brown coloured) • EDTA : Plastic container

  15. Preparation and standardization • NaOH • H2SO4 • Sodium thiosulphate • Potassium permanganate • Ceric ammonium sulphate • Oxalic acid • HCl

  16. HCL • Prepare 1 N solution • 9 ml of con HCL dissolve in 1 L water • Storage • Standardisation (Borax or 0.1N sodium carbonate) Reaction Na2Co3 + Hcl NaCl + H2CO3 • Carbonate to hydrogen carbonate (PH 8.3) • Formation of CO2 (PH 3.8)

  17. Error • Numerical difference between a measured value and true value • Absolute error E = Xi - Xt • Relative error • Expressed as a percentage Xi - Xt Er = x 100 Xi • Expressed as Parts per thousand

  18. Accuracy and precision • Accuracy • Correctness of a measurement in comparison with the true or accepted value • Closeness of measurement • Expressed in terms of A.E and R.E • Precision • Degree of reproducibility of a series of measurement on the same property

  19. Methods of expressing precision • Deviation D = Xi – X • Average deviation d = ∑Xi – X ∕ N • Relative average deviation d ∕ X • Standard deviation S = √ ∑(Xi – X)2 ∕ N • Relative Standard deviation V= S / X x 100

  20. Variance : S2 • Standard error SE = S / √ N • Types of sources of error • Analytical error • Determinate / Systematic Instrumental Method Operational • Indeterminate • Mistakes

  21. Minimization of errors • Calibration of apparatus and application of corrections • Analysis of standard samples • Running a blank determination • Independent analysis • Running a parallel determination

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