Analysis

Pharmaceutical Analysis

1. SBS GROUP OF EDUCATIONAL & TRAINING INSTITUTE WELCOMES YOU

2. Presented by:- Meraj Khan M pharma (Pharmacology) PHARMACEUTICAL ANALYSIS

3. Definition Pharmaceutical analysis is a branch of practical chemistry that involves a series of process for identification, determination, quantification and purification of a substance, separation of the components of a solution or mixture, or determination of structure of chemical compounds. The substance may be a single compound or a mixture of compounds and it may be in any of the dosage form. The substance used as pharmaceuticals are animals, plants, micro organisms, minerals and various synthetic products.

4. BASIC OF ANALYSIS Assay:-  is an investigative (analytic) procedure in Laboratory for qualitatively assessing or quantitatively measuring the presence, amount, or functional activity of a target entity (the analyte ). Analyte :- It is the chemical entity under assay e.g., HCl . Titrant :- It is the solution of known strength (or concentration) employed in the assay e.g., NaOH . Titration:- is the process of adding and then actually measuring the volume of titrant consumed in the assay. This volume is usually measured by the help of a calibrated burette.

5. Indicator:- is a chemical substance sensitive enough to display an apparent change in colour very close to the point in the ongoing titration process at which equivalent quantities of analyte and titrant . E.g. Methylene blue Equivalence Point (or Stoichiometric Point):- is the point at which one species neutralize the opposite species or is visibly spotted by the use of indicators. example The point at which Acid neutralize the base is Equivalence Point. End point :- The point at which color start to change during titration process. Titration Error:- Difference between end pont and equivalent point is called Titration Error.

6. Analyse :- The sample to be analysed is called as analyse . Standardization is the actual determination of either the normality or the molarity of a solution. Primary Standard is the substance of known purity (‘ AnalaR ’-grade reagents) whose carefully weighed quantity helps in the standardization of an unknown solution.Eg . Na2CO3 Secondary Standard is another standard solution that is used for standardization of an unknown solution. eg :- NaOH Titer is the weight of a substance chemically equivalent to 1 ml of a standard solution. Example : 1 ml of 1 N HCl contains 0.03646 g of HCl and hence is chemically equivalent to 0.04000 g of NaOH .

7.   TYPES OF ANALYSIS There are main two types of chemical analysis. 1. Qualitative (identification) 2. Quantitative (estimation) 1. Qualitative analysis:- It performed to establish composition of natural/synthetic substances. These tests are performed to indicate whether the substance or compound is present in the sample or not. Various qualitative tests are detection of evolved gas, formation of precipitates, limit tests, colour change reactions, melting point and boiling point test etc.

8. 2. Quantitative analytical:- These techniques are mainly used to quantify any compound or substance in the sample. These techniques are based in:- The quantitative performance of suitable chemical reaction and either measuring the amount of reagent added to complete the reaction or measuring the amount of reaction product obtained The charatristic movement of a substance through a defined medium under controlled conditions. Electrical measurement Measurement of some spectroscopic properties of the compound.

9. ON THE BASIS OF SIZE OF SAMPLE, THEY CAN BE CLASSIFIED AS :- Macro(0.1 g or more) Semi micro (0.01 g to 0.1 g) Micro(0.001 g to 0.01 g) Sub micro (0.0001 g to 0.001 g) Ultramicro (below 10-4 g) Trace analysis(100 to 10000 ppm ). Among all, the semi micro analysis is widely used.

10. METHODS OF ANALYSIS I INSTRUMENTAL NON-INSTRUMENTAL Electro Analytical Spectro Analytical Chromatography Other techniques Biological methods Chemical methods Electro -gravimetry Conducto -metry Coulometry Potentiometry Voltametry Spectrophotomet ry Spectrofluromtry IR Spectrophotometry Atomic emission spectroscopy Atomic absorption spectroscopy Flame emission spectroscopy Turbidimetry Nephelometry Colorimetry Ion pair extraction Colour development by chromogen GLC HPLC TLC/HPTLC RIA Flow injection ELISA Animal assay Microbiological Assay Titrimetry Gravinmetry Acid base Redox Precipitation Complexo etry Non aqueous

11. 1.CHEMICAL METHODS a) Titrimetric or Volumetric Method:- It involves reaction of substance to be determined with an appropriate reagent as a standard solution and volume of solution required to complete the reaction. There are Various types of Titrimetric methods are:- i )Acid-base titrations (Aqueous titrations /Neutralization reactions) ii)Non aqueous titrations iii) Redox Methods:- Iodimetric Titrations Iodometric Titrations iv) Precipitation titrations v)Oxidation reduction titrations vi) Complexometric titrations

12. b) Gravimetric methods:- In gravimetric analysis, a substance to be determined is converted into an insoluble precipitate in the purest form, which is then collected and weighed. Advance method:- Thermogravimetry Analysis (TGA):- records the change in weight. Differential Thermal Analysis (DTA):- records the difference in temperature between test substance and an inert reference material Differential Scanning Calorimetry (DSC):- records the energy needed to establish a zero temperature difference between a test substance and reference material.

13. c) Gasometric Analysis:- Gasometry involves measurement of the volume of gas evolved or absorbed in a chemical reaction. Some of the gases which are analysed by Gasometry are CO2 , N2O,cyclopropane, amyl nitrate, ethylene, N2, helium etc.

14. 2.ELECTRICAL METHODS Electrical methods of analysis involve the measurement of electric current, voltage or resistance in relation to the concentration of some species in the solution. Electrical methods of analysis include:- (a) Potentiometry :- It measures electrical potential of an electrode in equilibrium with an ion to be determined.example.PH meter. (b) Conductometry :- It measures electrical conductivity of an electrode with a reference electrode. (c) Voltametry :- It measures electrical current at a micro-electrode. example:- Polarography , Amperometry

15. 3.INSTRUMENTAL METHODS OF ANALYSIS Instrumental method involves measurement of some physical properties of the compound or a substance. These methods are employed for determination of minor or trace concentration of element in the sample. Instrumental methods are preferred due to their selectivity, high speed, accuracy and simplicity of analysis. Any change in the properties of the system are detected by measurement of absorbance, specific rotation, refractive index, migration difference, charge to mass ratio etc.

16. Spectroscopic methods of analysis depend upon measurement of the amount of radiant energy of a particular wavelength emitted by the sample. Methods which include absorption of radiation are ultra violet, visible, infra red, atomic absorption, nuclear magnetic resonance spectroscopy etc. Emission methods involve heating or electrical treatment of the sample so that the atoms are raised to the excited state to emit the energy and the intensity of this energy is measured. Emission methods include emission spectroscopy, flame photometry, flourimetry etc.

17. Chromatographic techniques and electrophoretic methods are separation methods for the mixure of compounds, but also applied for identification of compounds of mixures . Various chromatographic techniques are GC, HPLC, TLC, HPTLC, PC etc. Mass spectrometry involves vaporization of material using a high vaccum and the vapour is bombarded by a high energy electron beam. Vapour molecules undergo fragmentation to produce ions of varying size. These ions are differentiated by accelerating them in electrical field and then deflecting them in a magnetic field. Each kind of ion gives a peak in the mass spectrum.

18. 4. BIOLOGICAL AND MICROBIOLOGICAL METHODS Biological methods are used when potency of a drug or its derivative can not be properly determined by any physical or chemical methods. They are measured by bio-assays. Microbiological methods are used to observe potency of antibiotic or anti- microbial agents. In antimicrobial assay, inhibition of growth of bacteria of the sample is compared with that of the standard antibiotic. These methods include cup plate method and turbidimetric analysis.

19. APPLICATIONS:- Manufacturing industries require both qualitative and quantitative analysis to ensure that their raw materials meet certain specifications, and to check the quality of final product. Raw materials are to be checked to ensure that the essential components are present within the predetermined range of composition and there are not. Determination of radioactive compounds. Determination of natural phytoconstituents . Determination of moisture or water contain of sample by using Karl fischer titration. Quantitative estimation of Nitrogen by using Kjeldahls Mrthod .

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