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About The Book
The subject matter has been divided into two parts. Part-I covers phytochemical isolation, purification methods dealing with chromatography. Part-II deals with instrumental methods namely, UV, IR, NMR; CMR, CD/ORD, X-ray, Electrophoresis, Mass and finally dealing with characterization in structure elucidation of national products.
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Part-I : Phytochemical Method
1. Phytochemical Extraction Methods
1.01 Introduction
1.02 Extraction of plant material
1.03 Flow sheet showing extraction and purification methdos
1.04 Supercritical fluid extraction
1.05 Volatile oils extraction
2. Scale Up-pilot Plant Working
3. Isolation and Purification Techniques (Chromatography)
3.01 Introduction
3.02 Classification
3.03 General theoretical considerations
3.04 Liquid chromatography
4. Paper Chromatography (PC)
4.01 Mechanism
4.02 Apparatus
4.03 Radial / Circular
4.04 2-Dimensional
4.05 Paper
4.06 Sample application
4.07 Developing solvents
4.08 Drying of Chromatogram
4.09 Location of spots
4.10 Rf value
4.11 Preparative PC
4.12 Applications
4.13 Choice of method over TLC
5. Thin Layer Chromatography (TLC)
5.01 Introduction
5.02 Advantages
5.03 Requirements
5.04 Adsorbants as coating materials
5.05 Reverse phase partition TLC
5.06 Other spotted plate development methods
5.07 Unidimensional chromatography
5.08 Two dimensional TLC on square plants
5.09 Multiple development
5.10 Stepwise development
5.11 Preparative Chromatography on non-bound layers
5.12 Gradient TLC technique
5.13 Solvent systems (Mobile phases)
5.14 Detection of resolved substances
5.15 Detection (Location) reagents
5.16 Some specific general spray reagents for some categories
5.17 High performance thin layer chromatography (HPTLC)
5.18 GC-TLC Coupling
5.19 Application
6. Column Chromatography
6.01 Introduction
6.02 Apparatus
6.03 Adsorbents for column packing
6.04 Partition columns
6.05 Role of solvents
6.06 Techniques for chromatographic separations
6.07 Other forms of column chromatography
6.08 Columns for chromatography
6.09 Applications
7. Molecular Sieve Chromatography
7.01 Introduction
7.02 Materials
7.03 Column packing
7.04 Exclusion limit
7.05 Applications
8. Ion-exchange Chromatography
8.01 Introduction
8.02 Ion-exchangers
8.03 Ion exchange capacity
8.04 Some commercially available ion exchanges
8.05 ion exchange process
8.06 Applications
9. High Performance Liquid Chromatography (HPLC)
9.01 Introduction
9.02 Instrumentation
9.03 Special forms of HPLC
9.04 Applications
10. Gas Chromatography (GC)
10.01 Introduction
10.02 Gas liquid chromatography (GLC)
10.03 Instrumentation
10.04 Detectors
10.05 Temperature programming
10.06 Recorder device
10.07 Schematic representation
10.08 Resolution
10.09 Preparative gas chromatography
10.10 Applications
11. Counter Current Chromatography (CCC)
11.01 Introduction
11.02 High speed counter chromatography
11.03 Applications
12. Electrophoresis
12.01 Introduction
12.02 Factors affecting electrophoresis
12.03 Instrumentation technique
12.04 Capillary electrophoresis
12.05 Zone electrophoresis
12.06 Column electrophoresis
12.07 Applications
13. Multidimensional Chromatography
13.01 Introduction
13.02 Multi-Dimensional column separation
13.03 Liquid-Liquid Extraction
13.04 Multi-Dimensional TlC
13.05 Multi Dimensional GC
13.06 Multidimensional Electrophoresis (MDE)
13.07 Super critical fluid extraction (SFE) / super critical fluid chromatography (SFC)
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Part-II: Spectroscopy Method
14. Ultraviolet (UV) and Visible Spectroscopy
14.01 Introduction
14.02 Regions of electromagnetic spectrum
14.03 definition of terms and equatoins
14.04 UV and visible-spectroscopy
14.05 Instrumentation
14.06 Presentation of UV and visible absorption spectral data
14.07 Modes of Electronic Excitation (Designation of Various Transitions)
14.08 Chromophore
14.09 Auxochromes
14.10 Red shift or Bathochromic Shift
14.11 blue or hypsochromic shift
14.12 Isobestic point
14.13 Transiton probability
14.14 Effect of conjugation
14.15 Solvent effect
14.16 Lone pair in ketones
14.17 Measurement of UV spectrum
14.18 Spectral corelations
14.19 Woodward and Fieser and Fieser rules
14.20 Derivatives of >c=0 compounds
14.21 Effect of Substituents on Benzene
14.22 Miscellaneous conjugation extension
14.23 Model componds
14.24 Additivity of Chromophores
15. Infared (IR) Spectroscopy
15.01 Introduction
15.02 Theory
15.03 Calculation of vibrational frequencies
15.04 Hydrogen Bonding
15.05 Instrumentation
15.06 Sample Handling
15.07 Interpretation of IR spectrum
15.08 characteristics functional group frequencies of organic compounds
16. Nuclear Magnetic Resonance
16.01 Introduction
16.02 Instrumentation and sample handling
16.03 Peak intensities
16.04 Chemical shift
16.05 Factors influencing chemical shift
16.06 Spin spin coupling (J)
16.07 Splitting pattern rules
16.08 Classification of protons (Labelling of Proton)
16.09 AX system (Two Sets of Protons – Two Spin Systems)
16.10 AB system (Two Interacting Nucleii)
16.11 A2X spin system
16.12 A3X2 system
16.13 AB2 system
16.14 A2X2 or A2B2 system
16.15 Three Sets of Protons (Unsymmetrical Three Spin Systems)
16.16 ABX spectrum
16.17 ABC spin system
16.18 Chemical shift equivalence (Presence of Symmetry)
16.19 Four spin systems (Symmetrical)
16.20 Spin decoupling (Double Irradiation or Double Resonance)
16.21 Factors influencing ‘J’
16.22 Nuclear over houser effect (NOE)
16.23 NMR shift reagents
16.24 Two dimensional spectrometry (2D–NMR)
16.25 Cosy correlation spectroscopy (Cross-peak correlations)
16.26 Advantages of 2D-NMR
16.27 Multi dimensional NMR
17. 13C NMR Spectrometry (CMR)
17.01 Introduction
17.02 Characteristics of 13C Spectra
17.03 Sample Handling
17.04 Broad band hydrogen (proton) decoupling
17.05 Off resonance decoupling
17.06 Quaternary Carbon intensities
17.07 Deuterium Labelling
17.08 Chemical Shifts
17.09 Chemical Classes
17.10 Functional Groups Attached to carbon
17.11 ‘H NMR, 13C–H and Decoupled 13C NMR’
17.12 CMR Identification of Phenyal Butazone
18. Optical Potatory Dispersion (ORD)
18.01 Introduction
18.02 Cotton effect (CE)
18.03 Circularly bire fringent
18.04 Molecular elliptically
18.05 Chiroptical techniques
18.06 Types of curves in ORD/CD
18.07 Octant rule
18.08 Solvents
18.09 Vibrational circular dichroism (VCD)
18.10 Applications
19. X-ray Absorption, Fluorescence and Diffraction
19.01 Introduction
19.02 X-ray Absorption Methods
19.03 X-ray fluorescence methods
19.04 X-ray Diffraction Methods
19.05 Determination of Crystal Structure
19.06 Applications
20. Mass Spectrometry
20.01 Introduction
20.02 Instrumentation
20.03 Working
20.04 Decomposition and Rearrangement of Organic ions
20.05 Molecular ion peak (M+)
20.06 Ionisation techniques
20.07 Fragmentation
20.08 General Rules of Fragmentation
20.09 Mass spectra of classes of organic compounds
20.10 Rearrangements
20.11 Metastable Ions Decomposition
20.12 Identification of neutral fragments
20.13 Gas chromatography—Mass spectrometry (GC-MS)
20.14 High resolution mass spectrometry
20.15 Applications
Annexure
I. Common Fragment Ions
II. Common Fragment Ions Radicals or Molecules
III. Some Structure Discussions on Spectral Basis
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