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Pharmaceutical Analysis

This document provides a thorough introduction to spectroscopy and chromatography, crucial techniques in pharmaceutical analysis. It explores the interaction of electromagnetic radiation with samples, detailing absorption and emission methods at atomic and molecular levels. Key types of spectroscopy such as Atomic Absorption, UV, and Infrared are discussed. The text further delves into chromatography, outlining separation mechanisms in various forms including thin layer, gas, and high-performance liquid chromatography (HPLC), emphasizing their application in quantitative analysis.

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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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