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Principles and Applications of Analytical Techniques:

Pharmaceutical Analysis:

Series of tests to determine identity, purity, stability, toxicity, physical and chemical properties, and interactions, along with
the structure elucidation of drugs and related substances.

Classification of Analytical Techniques: (As discussed in Class)


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1. Chemical Analytical Techniques:


Techniques based on the chemical principles.
A. Volumetric Analysis:
Analysis based on measurement of volume of the analytes.
a. Aqueous Acid-Base titration:
P: Neutralization of acid and base to form salt and water
D: NaOH, ZnO
b. Non Aqueous Acid-Base titration:
P: The organic acids and bases are insoluble in water. These are extremely weak and cannot be analysed using
normal titrimetric methods so samples are dissolved in the non-aqueous solvents.
D: Metronidazole, Adrenaline
c. Redox titration:
P: The redox titration is mainly based upon the oxidation of the analyte by the oxidizing agent and the oxidation
and reduction of the reaction is determined by the indicators or by potentiometer.
D: Menadione, Tocopherol
d. Precipitation titration:
P: addition of the sample solution to the titrant in which the precipitating agent forms the precipitate and the
end point is detected by the indicators.
D: Drugs with chloride or sulphate ions.
e. Complexometric Titration:
P: reaction between the ligand and the metal ion to form a complex. The metal ion acts as Lewis acid and the
ligand acts as Lewis base which is the complexing agent.
D: aluminium glycinate, magnesium sulphate.
B. Gravimetric Analysis:
P: The principle involved in this method is that the sample is dissolved in a solvent and then the precipitating agent is
added. The resulting precipitate is filtered dried and weighed.
D: Nickel and Chromium containing products.

C. Gasometric Analysis:
P: Calculating amount of gases present in the sample.
D: CO2 and NO2 gases

2. Physical analytical techniques:

P: Based on the Physical properties of the substances

D: Determination of density, specific gravity, viscosity or conductivity of any drug or related product.

3. Physico-chemical Analytical Techniques:


Based on the physicochemical properties of the substances

A. Potentiometry:
P: The principle involved in the potentiometry is when the pair of electrodes is placed in the sample solution it shows
the potential difference by the addition of the titrant or by the change in the concentration of the ions.
D: % of acetyl salicylic acid in aspirin tablets, determination of the carbonate.
B. Polarography/Voltammetry:
P: The main principle in the polarography is the reduction process taking place at the electrode. This method has
limited sensitivity. The reduction at the electrode increases the voltage applied between the polarisable and non-
polarisable electrodes and the current is recorded that is, the metallic ions are reduced at the surface of the
electrode.
D: Vitamin C, Local anaesthetics
C. Absorption Techniques/Opticometric Methods:
a. UV-Visible Spectrophotometry:
P: measurement of interaction of electromagnetic radiation with the quantised matter at specific energy levels.
D: Diazepam, Acetazolamide, Paracetamol, Riboflavin
b. Mass Spectrophotometry:
P: Mass spectrometry (MS) is an analytical technique that ionizes chemical species and sorts the ions based on
their mass-to-charge ratio. In simpler terms, a mass spectrum measures the masses within a sample.
D: Propafenone, Amiodarone
c. IR Spectrophotometry:
P: The absorption is mainly based on the vibrations of the chemical substances after absorption of the infrared
radiation. The spectrum bands present in the IR spectrum represent the functional groups and bonds present in
the chemical substance. Hence, the IR spectrum is commonly known as the finger print of the chemical
substance.
D: identify functional groups of drugs, kinetics studies.
d. NMR spectroscopy:
P: measurement and interpretation of the radiofrequency which induces the transitions in the nuclei by
absorbing the radiofrequency waves and the spectra are known as the nuclear magnetic resonance spectra.
D: non-destructive analysis of aminoacids, proteins, RNA and DNA, number of carbon atoms present in the
sample.
e. Atomic Absorption spectroscopy:
P: The atoms present in the ground state absorb the radiation produced by the flame and excited to the excited
state and which is measured by the AAS spectrometer. Atomic absorption measures the amount of light at the
wavelength which is absorbed by the atoms. Atoms present in the sample are directly proportional to the
absorption intensity.
D: Arsenic, Trace elements in substances.
D. Separation Techniues:
a. Chromatography:
P: Separation of constituents of a sample due to difference in polarity or affinity.
D: Sensitive separation through high efficiency techniques.
b. Solvent Extraction:
P: Separation of components of a sample based on its miscibility
D: Separation of small batches of sample